







      #     TITL of the paper:

      #     Calixcrowns Derived from p-Bridged Calix[4]arenes



      #     CCDC ELECTRONIC DATA DEPOSITION FORM (CIF, VERSION DEC95)





      #     This electronic data deposition form must be associated with CIF

      #     output and can be used :

      #     (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or

      #     (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC



      #     A comprehensive archive of CIF resources is maintained by the IUCr

      #     at its Chester office. This can be accessed

      #     by anonymous ftp to ftp.iucr.ac.uk

      #     or via the WWW at http://www.iucr.ac.uk/cif/home.html



      #     If data items in this form are not available or not applicable

      #     then ignore these items



      #     A few items specific to CCDC input are indicated by _ccdc_ 



      #     Submission and help information is provided at the end of this form



      #-------------------------------------------------------------------------

      #1    Data block identification for start of deposition



data_



      #-------------------------------------------------------------------------

      #2    Person making the deposition



_publ_contact_author               

;

E. F. Paulus

Hoechst Marion Roussel Deutschland GmbH, G864

D-65926 Frankfurt/Main, Germany

;

_publ_contact_author_email          e.paulus@em.uni-frankfurt.de



      #-------------------------------------------------------------------------

      #3    Publication details



      #     Provide these details if the structure has been published,

      #     accepted or submitted for publication



      #     The CCDC journal deposition number, eg. 182/357,

      #     should be included only if it has been assigned by the journal



loop_

_publ_author_name

;

H. Stephan

Institut fr Anorganische Chemie der Technischen Universitt,

Mommsenstr. 13, D-01062 Dresden, Germany

;

;

K. Gloe

Institut fr Anorganische Chemie der Technischen Universitt,

Mommsenstr. 13, D-01062 Dresden, Germany

;

;

E. F. Paulus

Hoechst Marion Roussel Deutschland GmbH, G864

D-65926 Frankfurt/Main, Germany

;

;

M. Saadioui

Johannes Gutenberg-Universitaet, Institut fuer Organische Chemie, 

J.-J.-Becher Weg 34, SB1, D-5099 Mainz, Germany

;

;

V. Boehmer

Johannes Gutenberg-Universitaet, Institut fuer Organische Chemie, 

J.-J.-Becher Weg 34, SB1, D-5099 Mainz, Germany

;

;

B. Botta

Dipartimento di Studi di Chimica e Tecnologia delle Sostanze Biologicamente 

Attive, Universita' "La Sapienza", P. le A. Moro 5, 00185 Roma, Italy

;

_journal_name_full                 ''

_journal_volume                    '?'

_journal_page_first                '?'

_journal_page_last                 '?'

_journal_year                      '?'

_ccdc_journal_depnumber            '?'



      #-------------------------------------------------------------------------

      #4    Chemical and physical data



      #     Note that the units for melting point are Kelvin

      #     The compound_id is the identifier for the compound in the published

      #       paper, eg. 4a, II, etc.

      #     Provide a brief description of any significant biological activity,

      #       eg. antimalarial activity

      #     If the compound exhibits polymorphism provide brief details,

      #       eg. monoclinic form, low-temperature phase, etc.

      #     For chemdiag include any ASCII file output by a chemical drawing

      #       package

      #       Against _type record, for example, ChemDraw

      #       Against _records supply the chemical connectivity records



_chemical_name_systematic          

;

5,17-Di-t-butyl-26,28-dihydroxy-11,23-pentano-25,27-(1,4,7,10,13-pentaoxo-

tredecano)-calix[4]arene

;

_chemical_name_common              '?'

_chemical_formula_moiety           'C49H62O7'

_chemical_formula_sum              'C49H62O7'

_chemical_formula_weight            '762.99'

_chemical_melting_point             ?



_ccdc_compound_id                  '?'

_ccdc_biological_activity          '?'

_ccdc_polymorph                    '?'

_ccdc_chemdiag_type                ''

_loop

;





$Version: 4 

$Endsketch: 

;





_exptl_crystal_density_diffrn       '1.192'

_exptl_crystal_colour              '?'



      #-------------------------------------------------------------------------

      #5    Other data relating to the structure determination and refinement



      #     Record the radiation type if not X-rays, eg. neutron

      #     Record the temperature of the data collection (Kelvin)

      #       if not room-temperature

      #     Record R_squared if this is the only reliability factor given by

      #       your refinement program

      #     Describe briefly any disorder, eg. t-Butyl C31-33 disordered over

      #       two sites with occupancies 0.6 and 0.4

      #     Under ccdc_comments record any other important information



_diffrn_radiation_type             'Mo-K-alpha'            

_diffrn_measurement_device         'SIEMENS four-circle-diffractometer scint. c.'

_ccdc_temp_data_collection          '193(2)'

_ccdc_ls_R_squared                  '0.1303'

_refine_ls_abs_structure_details   'centrosymmetric'

_ccdc_disorder                     'no disorder'

_ccdc_comments ''



      #-------------------------------------------------------------------------

      #6    Include your "standard" CIF file here

      #     It should contain the following data items:

      #       unit cell parameters and volume, z value, space group symbol,

      #       R-factor(s), atomic coordinates with standard deviations,

      #       occupancy factors, bond lengths and bond angles

      #     Other data items may be present but will not necessarily be

      #       included in the Cambridge Structural Database

      #     Do not include structure factors

 

 

data_l378 

 

_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

 ? 

; 

_chemical_name_common             ? 

_chemical_melting_point           ? 

_chemical_formula_moiety          ? 

_chemical_formula_sum 

 'C49 H62 O7' 

_chemical_formula_weight          762.99 

 

loop_ 

 _atom_type_symbol 

 _atom_type_description 

 _atom_type_scat_dispersion_real 

 _atom_type_scat_dispersion_imag 

 _atom_type_scat_source 

 'C'  'C'   0.0033   0.0016 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 'H'  'H'   0.0000   0.0000 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 'O'  'O'   0.0106   0.0060 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 

_symmetry_cell_setting            ? 

_symmetry_space_group_name_H-M    P1- 

 

loop_ 

 _symmetry_equiv_pos_as_xyz 

 'x, y, z' 

 '-x, -y, -z' 

 

_cell_length_a                    11.1790(10) 

_cell_length_b                    13.411(2) 

_cell_length_c                    14.3820(10) 

_cell_angle_alpha                 84.260(10) 

_cell_angle_beta                  83.38(2) 

_cell_angle_gamma                 85.510(10) 

_cell_volume                      2126.2(4) 

_cell_formula_units_Z             2 

_cell_measurement_temperature     193(2) 

_cell_measurement_reflns_used     25 

_cell_measurement_theta_min       10 

_cell_measurement_theta_max       ? 

 

_exptl_crystal_description        ? 

_exptl_crystal_colour             ? 

_exptl_crystal_size_max           ? 

_exptl_crystal_size_mid           ? 

_exptl_crystal_size_min           ? 

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     1.192 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              824 

_exptl_absorpt_coefficient_mu     0.078 

_exptl_absorpt_correction_type    ? 

_exptl_absorpt_correction_T_min   ? 

_exptl_absorpt_correction_T_max   ? 

_exptl_absorpt_process_details    ? 

 

_exptl_special_details 

; 

 ? 

; 

 

_diffrn_ambient_temperature       193(2) 

_diffrn_radiation_wavelength      0.71073 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device_type   ? 

_diffrn_measurement_method        ? 

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          ? 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   ? 

_diffrn_standards_decay_%         ? 

_diffrn_reflns_number             6629 

_diffrn_reflns_av_R_equivalents   0.0373 

_diffrn_reflns_av_sigmaI/netI     0.1287 

_diffrn_reflns_limit_h_min        -12 

_diffrn_reflns_limit_h_max        0 

_diffrn_reflns_limit_k_min        -15 

_diffrn_reflns_limit_k_max        14 

_diffrn_reflns_limit_l_min        -16 

_diffrn_reflns_limit_l_max        16 

_diffrn_reflns_theta_min          2.00 

_diffrn_reflns_theta_max          23.55 

_reflns_number_total              6327 

_reflns_number_gt                 2991 

_reflns_threshold_expression      >2sigma(I) 

 

_computing_data_collection        ? 

_computing_cell_refinement        ? 

_computing_data_reduction         ? 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     ? 

_computing_publication_material   ? 

 

_refine_special_details 

; 

 Refinement of F² against ALL reflections.  The weighted R-factor wR and 

 goodness of fit S are based on F², conventional R-factors R are based 

 on F, with F set to zero for negative F². The threshold expression of 

 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 

 not relevant to the choice of reflections for refinement.  R-factors based 

 on F² are statistically about twice as large as those based on F, and R- 

 factors based on ALL data will be even larger. 

; 

 

_refine_ls_structure_factor_coef  Fsqd  

_refine_ls_matrix_type            full 

_refine_ls_weighting_scheme       calc  

_refine_ls_weighting_details 

 'calc w=1/[σ²(Fo²)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3' 

_atom_sites_solution_primary      direct 

_atom_sites_solution_secondary    difmap 

_atom_sites_solution_hydrogens    geom 

_refine_ls_hydrogen_treatment     mixed 

_refine_ls_extinction_method      SHELXL 

_refine_ls_extinction_coef        0.0050(7) 

_refine_ls_extinction_expression 

 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 

_refine_ls_number_reflns          6327 

_refine_ls_number_parameters      506 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.1416 

_refine_ls_R_factor_gt            0.0546 

_refine_ls_wR_factor_ref          0.1303 

_refine_ls_wR_factor_gt           0.1050 

_refine_ls_goodness_of_fit_ref    0.867 

_refine_ls_restrained_S_all       0.867 

_refine_ls_shift/su_max           0.000 

_refine_ls_shift/su_mean          0.000 

 

loop_ 

 _atom_site_label 

 _atom_site_type_symbol 

 _atom_site_fract_x 

 _atom_site_fract_y 

 _atom_site_fract_z 

 _atom_site_U_iso_or_equiv 

 _atom_site_adp_type 

 _atom_site_occupancy 

 _atom_site_symetry_multiplicity 

 _atom_site_calc_flag 

 _atom_site_refinement_flags 

 _atom_site_disorder_assembly 

 _atom_site_disorder_group 

C01 C 1.0517(3) 0.4210(3) 0.2245(3) 0.0310(10) Uani 1 1 d . . . 

C02 C 1.0372(3) 0.3407(3) 0.2929(3) 0.0327(10) Uani 1 1 d . . . 

H02A H 1.0821 0.2780 0.2831 0.080 Uiso 1 1 d R . . 

C03 C 0.9570(3) 0.3465(3) 0.3734(2) 0.0258(9) Uani 1 1 d . . . 

C04 C 0.9354(3) 0.2545(3) 0.4423(2) 0.0327(10) Uani 1 1 d . . . 

H04A H 0.8690 0.2708 0.4880 0.080 Uiso 1 1 d R . . 

H04B H 1.0055 0.2360 0.4746 0.080 Uiso 1 1 d R . . 

C05 C 0.9049(3) 0.1685(3) 0.3907(2) 0.0277(9) Uani 1 1 d . . . 

C06 C 0.9923(3) 0.0953(3) 0.3617(3) 0.0328(10) Uani 1 1 d . . . 

H06A H 1.0710 0.0930 0.3828 0.080 Uiso 1 1 d R . . 

C07 C 0.9707(4) 0.0248(3) 0.3017(3) 0.0349(10) Uani 1 1 d . . . 

C08 C 0.8560(3) 0.0305(3) 0.2729(3) 0.0338(10) Uani 1 1 d . . . 

H08A H 0.8392 -0.0172 0.2314 0.080 Uiso 1 1 d R . . 

C09 C 0.7649(3) 0.1004(3) 0.3016(2) 0.0276(9) Uani 1 1 d . . . 

C10 C 0.6432(3) 0.1086(3) 0.2616(2) 0.0320(10) Uani 1 1 d . . . 

H10A H 0.5799 0.1141 0.3124 0.080 Uiso 1 1 d R . . 

H10B H 0.6333 0.0502 0.2306 0.080 Uiso 1 1 d R . . 

C11 C 0.6357(3) 0.2015(3) 0.1919(3) 0.0288(9) Uani 1 1 d . . . 

C12 C 0.7095(3) 0.2046(3) 0.1070(3) 0.0317(10) Uani 1 1 d . . . 

H12A H 0.7562 0.1448 0.0898 0.080 Uiso 1 1 d R . . 

C13 C 0.7159(3) 0.2910(3) 0.0460(2) 0.0299(9) Uani 1 1 d . . . 

C14 C 0.6442(3) 0.3748(3) 0.0703(3) 0.0314(10) Uani 1 1 d . . . 

H14A H 0.6484 0.4355 0.0289 0.080 Uiso 1 1 d R . . 

C15 C 0.5653(3) 0.3758(2) 0.1532(2) 0.0244(9) Uani 1 1 d . . . 

C16 C 0.4912(3) 0.4711(3) 0.1774(3) 0.0315(10) Uani 1 1 d . . . 

H16A H 0.4439 0.4580 0.2368 0.080 Uiso 1 1 d R . . 

H16B H 0.4367 0.4890 0.1305 0.080 Uiso 1 1 d R . . 

C17 C 0.5679(3) 0.5575(3) 0.1825(2) 0.0273(9) Uani 1 1 d . . . 

C18 C 0.5624(3) 0.6443(3) 0.1211(2) 0.0277(9) Uani 1 1 d . . . 

H18A H 0.5084 0.6498 0.0733 0.080 Uiso 1 1 d R . . 

C19 C 0.6340(3) 0.7241(3) 0.1253(2) 0.0282(9) Uani 1 1 d . . . 

C20 C 0.7172(3) 0.7115(3) 0.1911(2) 0.0284(9) Uani 1 1 d . . . 

H20A H 0.7701 0.7640 0.1936 0.080 Uiso 1 1 d R . . 

C21 C 0.7253(3) 0.6246(3) 0.2547(2) 0.0297(9) Uani 1 1 d . . . 

C22 C 0.8174(3) 0.6148(3) 0.3256(3) 0.0359(10) Uani 1 1 d . . . 

H22A H 0.7750 0.6120 0.3876 0.080 Uiso 1 1 d R . . 

H22B H 0.8644 0.6726 0.3168 0.080 Uiso 1 1 d R . . 

C23 C 0.9006(3) 0.5203(3) 0.3173(3) 0.0303(10) Uani 1 1 d . . . 

C24 C 0.9828(3) 0.5092(3) 0.2383(3) 0.0338(10) Uani 1 1 d . . . 

H24A H 0.9899 0.5643 0.1904 0.080 Uiso 1 1 d R . . 

C25 C 1.1344(3) 0.4082(3) 0.1346(3) 0.0398(11) Uani 1 1 d . . . 

H25A H 1.2147 0.3888 0.1500 0.080 Uiso 1 1 d R . . 

H25B H 1.1364 0.4717 0.0973 0.080 Uiso 1 1 d R . . 

C26 C 1.0942(4) 0.3326(3) 0.0735(3) 0.0503(12) Uani 1 1 d . . . 

H26A H 1.0980 0.2678 0.1086 0.080 Uiso 1 1 d R . . 

H26B H 1.1475 0.3288 0.0164 0.080 Uiso 1 1 d R . . 

C27 C 0.9679(4) 0.3524(3) 0.0480(3) 0.0440(11) Uani 1 1 d . . . 

H27A H 0.9618 0.4189 0.0166 0.080 Uiso 1 1 d R . . 

H27B H 0.9126 0.3502 0.1044 0.080 Uiso 1 1 d R . . 

C28 C 0.9348(4) 0.2757(3) -0.0169(3) 0.0455(11) Uani 1 1 d . . . 

H28A H 0.9434 0.2093 0.0146 0.080 Uiso 1 1 d R . . 

H28B H 0.9904 0.2787 -0.0731 0.080 Uiso 1 1 d R . . 

C29 C 0.8060(3) 0.2947(3) -0.0409(3) 0.0403(11) Uani 1 1 d . . . 

H29A H 0.7984 0.3600 -0.0745 0.080 Uiso 1 1 d R . . 

H29B H 0.7884 0.2461 -0.0812 0.080 Uiso 1 1 d R . . 

C30 C 0.8365(4) 0.4700(3) 0.5451(3) 0.0440(11) Uani 1 1 d . . . 

H30A H 0.8950 0.4199 0.5678 0.080 Uiso 1 1 d R . . 

H30B H 0.8725 0.5334 0.5341 0.080 Uiso 1 1 d R . . 

C31 C 0.7295(4) 0.4707(4) 0.6179(3) 0.0591(14) Uani 1 1 d . . . 

H31A H 0.6677 0.5146 0.5913 0.080 Uiso 1 1 d R . . 

H31B H 0.7485 0.4976 0.6734 0.080 Uiso 1 1 d R . . 

C32 C 0.5889(4) 0.3556(3) 0.5896(3) 0.0467(11) Uani 1 1 d . . . 

H32A H 0.5207 0.4023 0.6021 0.080 Uiso 1 1 d R . . 

H32B H 0.6137 0.3603 0.5232 0.080 Uiso 1 1 d R . . 

C33 C 0.5550(4) 0.2517(3) 0.6227(3) 0.0594(13) Uani 1 1 d . . . 

H33A H 0.5326 0.2470 0.6894 0.080 Uiso 1 1 d R . . 

H33B H 0.6230 0.2052 0.6091 0.080 Uiso 1 1 d R . . 

C34 C 0.4309(5) 0.1294(3) 0.5868(3) 0.0723(16) Uani 1 1 d . . . 

H34A H 0.5006 0.0901 0.5619 0.080 Uiso 1 1 d R . . 

H34B H 0.4129 0.1076 0.6523 0.080 Uiso 1 1 d R . . 

C35 C 0.3315(5) 0.1117(4) 0.5304(3) 0.0705(16) Uani 1 1 d . . . 

H35A H 0.2650 0.1568 0.5511 0.080 Uiso 1 1 d R . . 

H35B H 0.3064 0.0444 0.5420 0.080 Uiso 1 1 d R . . 

C36 C 0.3211(4) 0.2323(3) 0.3993(3) 0.0452(11) Uani 1 1 d . . . 

H36A H 0.2345 0.2386 0.4048 0.080 Uiso 1 1 d R . . 

H36B H 0.3487 0.2805 0.4357 0.080 Uiso 1 1 d R . . 

C37 C 0.3740(3) 0.2547(3) 0.2991(3) 0.0444(11) Uani 1 1 d . . . 

H37A H 0.3273 0.3069 0.2660 0.080 Uiso 1 1 d R . . 

H37B H 0.3757 0.1943 0.2683 0.080 Uiso 1 1 d R . . 

C38 C 0.5637(3) 0.2871(3) 0.2124(2) 0.0253(9) Uani 1 1 d . . . 

C39 C 0.6469(3) 0.5512(3) 0.2516(2) 0.0290(9) Uani 1 1 d . . . 

C40 C 0.8903(3) 0.4379(3) 0.3848(3) 0.0293(9) Uani 1 1 d . . . 

C41 C 0.7902(3) 0.1690(3) 0.3623(2) 0.0268(9) Uani 1 1 d . . . 

C42 C 1.0694(4) -0.0500(3) 0.2637(3) 0.0431(11) Uani 1 1 d . . . 

C43 C 1.1828(5) -0.0534(4) 0.3124(5) 0.117(3) Uani 1 1 d . . . 

H43A H 1.2159 0.0112 0.3056 0.080 Uiso 1 1 d R . . 

H43B H 1.1595 -0.0725 0.3777 0.080 Uiso 1 1 d R . . 

H43C H 1.2424 -0.1023 0.2878 0.080 Uiso 1 1 d R . . 

C44 C 1.1019(5) -0.0241(4) 0.1606(4) 0.102(2) Uani 1 1 d . . . 

H44A H 1.1318 0.0417 0.1504 0.080 Uiso 1 1 d R . . 

H44B H 1.1625 -0.0721 0.1361 0.080 Uiso 1 1 d R . . 

H44C H 1.0308 -0.0248 0.1292 0.080 Uiso 1 1 d R . . 

C45 C 1.0276(5) -0.1559(3) 0.2767(3) 0.0737(16) Uani 1 1 d . . . 

H45A H 0.9576 -0.1563 0.2437 0.080 Uiso 1 1 d R . . 

H45B H 1.0891 -0.2035 0.2526 0.080 Uiso 1 1 d R . . 

H45C H 1.0062 -0.1737 0.3425 0.080 Uiso 1 1 d R . . 

C46 C 0.6129(3) 0.8227(3) 0.0649(3) 0.0299(9) Uani 1 1 d . . . 

C47 C 0.7135(4) 0.8934(3) 0.0654(3) 0.0484(12) Uani 1 1 d . . . 

H47A H 0.7879 0.8604 0.0405 0.080 Uiso 1 1 d R . . 

H47B H 0.6984 0.9556 0.0281 0.080 Uiso 1 1 d R . . 

H47C H 0.7189 0.9065 0.1291 0.080 Uiso 1 1 d R . . 

C48 C 0.4934(4) 0.8756(3) 0.1045(3) 0.0507(12) Uani 1 1 d . . . 

H48A H 0.4975 0.8871 0.1688 0.080 Uiso 1 1 d R . . 

H48B H 0.4789 0.9386 0.0683 0.080 Uiso 1 1 d R . . 

H48C H 0.4288 0.8334 0.1011 0.080 Uiso 1 1 d R . . 

C49 C 0.6033(4) 0.8059(3) -0.0376(2) 0.0406(11) Uani 1 1 d . . . 

H49A H 0.6778 0.7736 -0.0633 0.080 Uiso 1 1 d R . . 

H49B H 0.5384 0.7639 -0.0405 0.080 Uiso 1 1 d R . . 

H49C H 0.5884 0.8692 -0.0733 0.080 Uiso 1 1 d R . . 

O1 O 0.7986(2) 0.44418(18) 0.45899(16) 0.0333(7) Uani 1 1 d . . . 

O2 O 0.6852(3) 0.3746(2) 0.64155(19) 0.0596(9) Uani 1 1 d . . . 

O3 O 0.4547(3) 0.2317(2) 0.57534(19) 0.0522(8) Uani 1 1 d . . . 

O4 O 0.3635(3) 0.1349(2) 0.43211(19) 0.0562(9) Uani 1 1 d . . . 

O5 O 0.4944(2) 0.28468(18) 0.30029(16) 0.0309(6) Uani 1 1 d . . . 

O6 O 0.6387(2) 0.46755(18) 0.31465(17) 0.0384(7) Uani 1 1 d . . . 

H6A H 0.6908 0.4688 0.3531 0.080 Uiso 1 1 d R . . 

O7 O 0.7067(2) 0.24103(18) 0.39557(16) 0.0373(7) Uani 1 1 d . . . 

H7A H 0.6484 0.2461 0.3620 0.080 Uiso 1 1 d R . . 

 


 

_geom_special_details 

; 

 All esds (except the esd in the dihedral angle between two l.s. planes) 

 are estimated using the full covariance matrix.  The cell esds are taken 

 into account individually in the estimation of esds in distances, angles 

 and torsion angles; correlations between esds in cell parameters are only 

 used when they are defined by crystal symmetry.  An approximate (isotropic) 

 treatment of cell esds is used for estimating esds involving l.s. planes. 

; 

 

loop_ 

 _geom_bond_atom_site_label_1 

 _geom_bond_atom_site_label_2 

 _geom_bond_distance 

 _geom_bond_site_symmetry_2 

 _geom_bond_publ_flag 

C01 C24 1.379(5) . ? 

C01 C02 1.390(5) . ? 

C01 C25 1.516(5) . ? 

C02 C03 1.385(5) . ? 

C02 H02A 0.9600 . ? 

C03 C40 1.398(5) . ? 

C03 C04 1.520(5) . ? 

C04 C05 1.513(5) . ? 

C04 H04A 0.9600 . ? 

C04 H04B 0.9600 . ? 

C05 C41 1.389(5) . ? 

C05 C06 1.390(5) . ? 

C06 C07 1.394(5) . ? 

C06 H06A 0.9601 . ? 

C07 C08 1.386(5) . ? 

C07 C42 1.523(5) . ? 

C08 C09 1.386(5) . ? 

C08 H08A 0.9600 . ? 

C09 C41 1.396(5) . ? 

C09 C10 1.529(5) . ? 

C10 C11 1.522(5) . ? 

C10 H10A 0.9600 . ? 

C10 H10B 0.9600 . ? 

C11 C38 1.386(5) . ? 

C11 C12 1.391(5) . ? 

C12 C13 1.383(5) . ? 

C12 H12A 0.9600 . ? 

C13 C14 1.380(5) . ? 

C13 C29 1.512(5) . ? 

C14 C15 1.399(5) . ? 

C14 H14A 0.9600 . ? 

C15 C38 1.391(5) . ? 

C15 C16 1.516(5) . ? 

C16 C17 1.506(4) . ? 

C16 H16A 0.9600 . ? 

C16 H16B 0.9599 . ? 

C17 C18 1.391(5) . ? 

C17 C39 1.396(5) . ? 

C18 C19 1.396(4) . ? 

C18 H18A 0.9601 . ? 

C19 C20 1.392(5) . ? 

C19 C46 1.525(5) . ? 

C20 C21 1.411(5) . ? 

C20 H20A 0.9599 . ? 

C21 C39 1.376(5) . ? 

C21 C22 1.520(5) . ? 

C22 C23 1.518(5) . ? 

C22 H22A 0.9600 . ? 

C22 H22B 0.9600 . ? 

C23 C24 1.388(5) . ? 

C23 C40 1.399(5) . ? 

C24 H24A 0.9601 . ? 

C25 C26 1.531(5) . ? 

C25 H25A 0.9600 . ? 

C25 H25B 0.9600 . ? 

C26 C27 1.497(5) . ? 

C26 H26A 0.9600 . ? 

C26 H26B 0.9600 . ? 

C27 C28 1.549(5) . ? 

C27 H27A 0.9600 . ? 

C27 H27B 0.9600 . ? 

C28 C29 1.515(5) . ? 

C28 H28A 0.9600 . ? 

C28 H28B 0.9600 . ? 

C29 H29A 0.9600 . ? 

C29 H29B 0.9599 . ? 

C30 O1 1.437(4) . ? 

C30 C31 1.496(5) . ? 

C30 H30A 0.9600 . ? 

C30 H30B 0.9600 . ? 

C31 O2 1.413(5) . ? 

C31 H31A 0.9600 . ? 

C31 H31B 0.9600 . ? 

C32 O2 1.431(4) . ? 

C32 C33 1.491(5) . ? 

C32 H32A 0.9601 . ? 

C32 H32B 0.9600 . ? 

C33 O3 1.433(5) . ? 

C33 H33A 0.9600 . ? 

C33 H33B 0.9600 . ? 

C34 O3 1.408(5) . ? 

C34 C35 1.496(6) . ? 

C34 H34A 0.9600 . ? 

C34 H34B 0.9601 . ? 

C35 O4 1.427(5) . ? 

C35 H35A 0.9601 . ? 

C35 H35B 0.9600 . ? 

C36 O4 1.409(4) . ? 

C36 C37 1.505(5) . ? 

C36 H36A 0.9600 . ? 

C36 H36B 0.9600 . ? 

C37 O5 1.436(4) . ? 

C37 H37A 0.9599 . ? 

C37 H37B 0.9600 . ? 

C38 O5 1.404(4) . ? 

C39 O6 1.372(4) . ? 

C40 O1 1.395(4) . ? 

C41 O7 1.372(4) . ? 

C42 C44 1.498(6) . ? 

C42 C43 1.512(6) . ? 

C42 C45 1.517(5) . ? 

C43 H43A 0.9600 . ? 

C43 H43B 0.9600 . ? 

C43 H43C 0.9600 . ? 

C44 H44A 0.9600 . ? 

C44 H44B 0.9600 . ? 

C44 H44C 0.9600 . ? 

C45 H45A 0.9600 . ? 

C45 H45B 0.9600 . ? 

C45 H45C 0.9600 . ? 

C46 C47 1.527(5) . ? 

C46 C49 1.530(5) . ? 

C46 C48 1.540(5) . ? 

C47 H47A 0.9600 . ? 

C47 H47B 0.9600 . ? 

C47 H47C 0.9600 . ? 

C48 H48A 0.9600 . ? 

C48 H48B 0.9600 . ? 

C48 H48C 0.9599 . ? 

C49 H49A 0.9600 . ? 

C49 H49B 0.9600 . ? 

C49 H49C 0.9600 . ? 

O6 H6A 0.8501 . ? 

O7 H7A 0.8500 . ? 

 

loop_ 

 _geom_angle_atom_site_label_1 

 _geom_angle_atom_site_label_2 

 _geom_angle_atom_site_label_3 

 _geom_angle 

 _geom_angle_site_symmetry_1 

 _geom_angle_site_symmetry_3 

 _geom_angle_publ_flag 

C24 C01 C02 117.9(4) . . ? 

C24 C01 C25 121.6(3) . . ? 

C02 C01 C25 120.3(4) . . ? 

C03 C02 C01 122.5(4) . . ? 

C03 C02 H02A 118.4 . . ? 

C01 C02 H02A 119.0 . . ? 

C02 C03 C40 117.4(3) . . ? 

C02 C03 C04 121.0(3) . . ? 

C40 C03 C04 121.5(3) . . ? 

C05 C04 C03 109.9(3) . . ? 

C05 C04 H04A 109.2 . . ? 

C03 C04 H04A 108.6 . . ? 

C05 C04 H04B 110.5 . . ? 

C03 C04 H04B 110.1 . . ? 

H04A C04 H04B 108.4 . . ? 

C41 C05 C06 119.0(3) . . ? 

C41 C05 C04 119.1(3) . . ? 

C06 C05 C04 121.6(3) . . ? 

C05 C06 C07 122.4(4) . . ? 

C05 C06 H06A 119.5 . . ? 

C07 C06 H06A 118.2 . . ? 

C08 C07 C06 116.4(4) . . ? 

C08 C07 C42 121.1(4) . . ? 

C06 C07 C42 122.3(4) . . ? 

C09 C08 C07 123.4(4) . . ? 

C09 C08 H08A 118.7 . . ? 

C07 C08 H08A 117.9 . . ? 

C08 C09 C41 118.2(3) . . ? 

C08 C09 C10 121.2(3) . . ? 

C41 C09 C10 120.4(3) . . ? 

C11 C10 C09 109.4(3) . . ? 

C11 C10 H10A 109.7 . . ? 

C09 C10 H10A 108.8 . . ? 

C11 C10 H10B 109.4 . . ? 

C09 C10 H10B 110.8 . . ? 

H10A C10 H10B 108.7 . . ? 

C38 C11 C12 117.9(3) . . ? 

C38 C11 C10 122.3(3) . . ? 

C12 C11 C10 119.7(3) . . ? 

C13 C12 C11 121.9(4) . . ? 

C13 C12 H12A 119.1 . . ? 

C11 C12 H12A 119.0 . . ? 

C14 C13 C12 118.1(4) . . ? 

C14 C13 C29 121.4(3) . . ? 

C12 C13 C29 120.4(4) . . ? 

C13 C14 C15 122.9(3) . . ? 

C13 C14 H14A 118.9 . . ? 

C15 C14 H14A 118.2 . . ? 

C38 C15 C14 116.4(3) . . ? 

C38 C15 C16 123.0(3) . . ? 

C14 C15 C16 120.5(3) . . ? 

C17 C16 C15 112.7(3) . . ? 

C17 C16 H16A 109.2 . . ? 

C15 C16 H16A 108.7 . . ? 

C17 C16 H16B 109.4 . . ? 

C15 C16 H16B 108.5 . . ? 

H16A C16 H16B 108.1 . . ? 

C18 C17 C39 118.4(3) . . ? 

C18 C17 C16 122.3(3) . . ? 

C39 C17 C16 119.3(3) . . ? 

C17 C18 C19 122.5(3) . . ? 

C17 C18 H18A 119.4 . . ? 

C19 C18 H18A 118.1 . . ? 

C20 C19 C18 117.0(3) . . ? 

C20 C19 C46 122.6(3) . . ? 

C18 C19 C46 120.2(3) . . ? 

C19 C20 C21 122.1(3) . . ? 

C19 C20 H20A 118.7 . . ? 

C21 C20 H20A 119.2 . . ? 

C39 C21 C20 118.4(3) . . ? 

C39 C21 C22 121.7(3) . . ? 

C20 C21 C22 120.0(3) . . ? 

C23 C22 C21 111.9(3) . . ? 

C23 C22 H22A 108.6 . . ? 

C21 C22 H22A 108.5 . . ? 

C23 C22 H22B 109.6 . . ? 

C21 C22 H22B 109.8 . . ? 

H22A C22 H22B 108.4 . . ? 

C24 C23 C40 117.4(4) . . ? 

C24 C23 C22 121.0(3) . . ? 

C40 C23 C22 121.3(4) . . ? 

C01 C24 C23 122.6(4) . . ? 

C01 C24 H24A 118.6 . . ? 

C23 C24 H24A 118.8 . . ? 

C01 C25 C26 114.0(3) . . ? 

C01 C25 H25A 109.1 . . ? 

C26 C25 H25A 109.8 . . ? 

C01 C25 H25B 108.8 . . ? 

C26 C25 H25B 107.0 . . ? 

H25A C25 H25B 107.9 . . ? 

C27 C26 C25 114.9(4) . . ? 

C27 C26 H26A 106.8 . . ? 

C25 C26 H26A 107.5 . . ? 

C27 C26 H26B 108.1 . . ? 

C25 C26 H26B 111.1 . . ? 

H26A C26 H26B 108.1 . . ? 

C26 C27 C28 112.2(3) . . ? 

C26 C27 H27A 107.4 . . ? 

C28 C27 H27A 109.7 . . ? 

C26 C27 H27B 109.3 . . ? 

C28 C27 H27B 109.5 . . ? 

H27A C27 H27B 108.6 . . ? 

C29 C28 C27 112.1(3) . . ? 

C29 C28 H28A 108.3 . . ? 

C27 C28 H28A 108.9 . . ? 

C29 C28 H28B 110.5 . . ? 

C27 C28 H28B 108.8 . . ? 

H28A C28 H28B 108.2 . . ? 

C13 C29 C28 112.0(3) . . ? 

C13 C29 H29A 109.1 . . ? 

C28 C29 H29A 108.2 . . ? 

C13 C29 H29B 109.3 . . ? 

C28 C29 H29B 110.1 . . ? 

H29A C29 H29B 108.1 . . ? 

O1 C30 C31 108.4(3) . . ? 

O1 C30 H30A 110.4 . . ? 

C31 C30 H30A 107.0 . . ? 

O1 C30 H30B 109.3 . . ? 

C31 C30 H30B 112.9 . . ? 

H30A C30 H30B 108.7 . . ? 

O2 C31 C30 112.6(4) . . ? 

O2 C31 H31A 108.8 . . ? 

C30 C31 H31A 106.5 . . ? 

O2 C31 H31B 109.9 . . ? 

C30 C31 H31B 110.6 . . ? 

H31A C31 H31B 108.3 . . ? 

O2 C32 C33 106.3(3) . . ? 

O2 C32 H32A 110.5 . . ? 

C33 C32 H32A 109.5 . . ? 

O2 C32 H32B 111.5 . . ? 

C33 C32 H32B 109.8 . . ? 

H32A C32 H32B 109.2 . . ? 

O3 C33 C32 107.9(3) . . ? 

O3 C33 H33A 110.1 . . ? 

C32 C33 H33A 109.4 . . ? 

O3 C33 H33B 111.3 . . ? 

C32 C33 H33B 109.2 . . ? 

H33A C33 H33B 109.0 . . ? 

O3 C34 C35 110.0(4) . . ? 

O3 C34 H34A 109.4 . . ? 

C35 C34 H34A 106.0 . . ? 

O3 C34 H34B 110.4 . . ? 

C35 C34 H34B 112.2 . . ? 

H34A C34 H34B 108.7 . . ? 

O4 C35 C34 111.9(4) . . ? 

O4 C35 H35A 108.9 . . ? 

C34 C35 H35A 105.3 . . ? 

O4 C35 H35B 109.8 . . ? 

C34 C35 H35B 112.4 . . ? 

H35A C35 H35B 108.3 . . ? 

O4 C36 C37 108.9(3) . . ? 

O4 C36 H36A 111.0 . . ? 

C37 C36 H36A 111.2 . . ? 

O4 C36 H36B 109.5 . . ? 

C37 C36 H36B 107.4 . . ? 

H36A C36 H36B 108.7 . . ? 

O5 C37 C36 107.8(3) . . ? 

O5 C37 H37A 109.7 . . ? 

C36 C37 H37A 112.2 . . ? 

O5 C37 H37B 110.4 . . ? 

C36 C37 H37B 107.7 . . ? 

H37A C37 H37B 108.9 . . ? 

C11 C38 C15 122.8(3) . . ? 

C11 C38 O5 117.3(3) . . ? 

C15 C38 O5 119.7(3) . . ? 

O6 C39 C21 123.9(3) . . ? 

O6 C39 C17 114.7(3) . . ? 

C21 C39 C17 121.4(3) . . ? 

O1 C40 C03 119.5(3) . . ? 

O1 C40 C23 117.8(3) . . ? 

C03 C40 C23 122.1(4) . . ? 

O7 C41 C05 116.3(3) . . ? 

O7 C41 C09 123.1(3) . . ? 

C05 C41 C09 120.6(3) . . ? 

C44 C42 C43 108.4(4) . . ? 

C44 C42 C45 107.6(4) . . ? 

C43 C42 C45 106.4(4) . . ? 

C44 C42 C07 110.0(4) . . ? 

C43 C42 C07 113.0(4) . . ? 

C45 C42 C07 111.1(4) . . ? 

C42 C43 H43A 111.1 . . ? 

C42 C43 H43B 106.4 . . ? 

H43A C43 H43B 109.5 . . ? 

C42 C43 H43C 110.9 . . ? 

H43A C43 H43C 109.5 . . ? 

H43B C43 H43C 109.5 . . ? 

C42 C44 H44A 109.5 . . ? 

C42 C44 H44B 110.3 . . ? 

H44A C44 H44B 109.5 . . ? 

C42 C44 H44C 108.6 . . ? 

H44A C44 H44C 109.5 . . ? 

H44B C44 H44C 109.5 . . ? 

C42 C45 H45A 107.9 . . ? 

C42 C45 H45B 111.7 . . ? 

H45A C45 H45B 109.5 . . ? 

C42 C45 H45C 108.7 . . ? 

H45A C45 H45C 109.5 . . ? 

H45B C45 H45C 109.5 . . ? 

C19 C46 C47 112.4(3) . . ? 

C19 C46 C49 112.1(3) . . ? 

C47 C46 C49 107.5(3) . . ? 

C19 C46 C48 108.3(3) . . ? 

C47 C46 C48 108.2(3) . . ? 

C49 C46 C48 108.2(3) . . ? 

C46 C47 H47A 108.2 . . ? 

C46 C47 H47B 111.6 . . ? 

H47A C47 H47B 109.5 . . ? 

C46 C47 H47C 108.7 . . ? 

H47A C47 H47C 109.5 . . ? 

H47B C47 H47C 109.5 . . ? 

C46 C48 H48A 109.6 . . ? 

C46 C48 H48B 109.9 . . ? 

H48A C48 H48B 109.5 . . ? 

C46 C48 H48C 108.9 . . ? 

H48A C48 H48C 109.5 . . ? 

H48B C48 H48C 109.5 . . ? 

C46 C49 H49A 109.0 . . ? 

C46 C49 H49B 109.5 . . ? 

H49A C49 H49B 109.5 . . ? 

C46 C49 H49C 109.9 . . ? 

H49A C49 H49C 109.5 . . ? 

H49B C49 H49C 109.5 . . ? 

C40 O1 C30 114.9(3) . . ? 

C31 O2 C32 113.7(3) . . ? 

C34 O3 C33 112.4(3) . . ? 

C36 O4 C35 113.0(3) . . ? 

C38 O5 C37 113.9(3) . . ? 

C39 O6 H6A 108.7 . . ? 

C41 O7 H7A 108.1 . . ? 

 

loop_ 

 _geom_torsion_atom_site_label_1 

 _geom_torsion_atom_site_label_2 

 _geom_torsion_atom_site_label_3 

 _geom_torsion_atom_site_label_4 

 _geom_torsion 

 _geom_torsion_site_symmetry_1 

 _geom_torsion_site_symmetry_2 

 _geom_torsion_site_symmetry_3 

 _geom_torsion_site_symmetry_4 

 _geom_torsion_publ_flag 

C24 C01 C02 C03 0.0(5) . . . . ? 

C25 C01 C02 C03 -175.7(3) . . . . ? 

C01 C02 C03 C40 -0.8(5) . . . . ? 

C01 C02 C03 C04 174.4(3) . . . . ? 

C02 C03 C04 C05 -52.0(4) . . . . ? 

C40 C03 C04 C05 123.0(4) . . . . ? 

C03 C04 C05 C41 -76.2(4) . . . . ? 

C03 C04 C05 C06 96.3(4) . . . . ? 

C41 C05 C06 C07 2.9(5) . . . . ? 

C04 C05 C06 C07 -169.7(3) . . . . ? 

C05 C06 C07 C08 -0.8(5) . . . . ? 

C05 C06 C07 C42 175.0(4) . . . . ? 

C06 C07 C08 C09 -0.8(5) . . . . ? 

C42 C07 C08 C09 -176.7(3) . . . . ? 

C07 C08 C09 C41 0.4(5) . . . . ? 

C07 C08 C09 C10 175.1(3) . . . . ? 

C08 C09 C10 C11 -105.0(4) . . . . ? 

C41 C09 C10 C11 69.7(4) . . . . ? 

C09 C10 C11 C38 -106.9(4) . . . . ? 

C09 C10 C11 C12 68.3(4) . . . . ? 

C38 C11 C12 C13 2.7(5) . . . . ? 

C10 C11 C12 C13 -172.7(3) . . . . ? 

C11 C12 C13 C14 -1.6(5) . . . . ? 

C11 C12 C13 C29 174.0(3) . . . . ? 

C12 C13 C14 C15 -0.4(5) . . . . ? 

C29 C13 C14 C15 -175.9(3) . . . . ? 

C13 C14 C15 C38 1.1(5) . . . . ? 

C13 C14 C15 C16 178.3(3) . . . . ? 

C38 C15 C16 C17 119.4(4) . . . . ? 

C14 C15 C16 C17 -57.6(4) . . . . ? 

C15 C16 C17 C18 116.2(4) . . . . ? 

C15 C16 C17 C39 -64.4(4) . . . . ? 

C39 C17 C18 C19 1.0(5) . . . . ? 

C16 C17 C18 C19 -179.5(3) . . . . ? 

C17 C18 C19 C20 3.3(5) . . . . ? 

C17 C18 C19 C46 -172.1(3) . . . . ? 

C18 C19 C20 C21 -3.4(5) . . . . ? 

C46 C19 C20 C21 171.9(3) . . . . ? 

C19 C20 C21 C39 -0.8(5) . . . . ? 

C19 C20 C21 C22 -179.7(3) . . . . ? 

C39 C21 C22 C23 57.5(5) . . . . ? 

C20 C21 C22 C23 -123.6(4) . . . . ? 

C21 C22 C23 C24 67.4(4) . . . . ? 

C21 C22 C23 C40 -107.0(4) . . . . ? 

C02 C01 C24 C23 0.0(5) . . . . ? 

C25 C01 C24 C23 175.7(3) . . . . ? 

C40 C23 C24 C01 0.8(5) . . . . ? 

C22 C23 C24 C01 -173.8(3) . . . . ? 

C24 C01 C25 C26 -112.0(4) . . . . ? 

C02 C01 C25 C26 63.6(5) . . . . ? 

C01 C25 C26 C27 54.7(5) . . . . ? 

C25 C26 C27 C28 177.7(3) . . . . ? 

C26 C27 C28 C29 178.8(3) . . . . ? 

C14 C13 C29 C28 115.6(4) . . . . ? 

C12 C13 C29 C28 -59.8(5) . . . . ? 

C27 C28 C29 C13 -58.2(4) . . . . ? 

O1 C30 C31 O2 65.4(5) . . . . ? 

O2 C32 C33 O3 177.3(3) . . . . ? 

O3 C34 C35 O4 62.5(5) . . . . ? 

O4 C36 C37 O5 -80.8(4) . . . . ? 

C12 C11 C38 C15 -1.9(5) . . . . ? 

C10 C11 C38 C15 173.3(3) . . . . ? 

C12 C11 C38 O5 -176.8(3) . . . . ? 

C10 C11 C38 O5 -1.5(5) . . . . ? 

C14 C15 C38 C11 0.1(5) . . . . ? 

C16 C15 C38 C11 -177.1(3) . . . . ? 

C14 C15 C38 O5 174.8(3) . . . . ? 

C16 C15 C38 O5 -2.3(5) . . . . ? 

C20 C21 C39 O6 -174.2(3) . . . . ? 

C22 C21 C39 O6 4.6(6) . . . . ? 

C20 C21 C39 C17 5.4(5) . . . . ? 

C22 C21 C39 C17 -175.7(3) . . . . ? 

C18 C17 C39 O6 174.1(3) . . . . ? 

C16 C17 C39 O6 -5.3(5) . . . . ? 

C18 C17 C39 C21 -5.5(5) . . . . ? 

C16 C17 C39 C21 175.0(3) . . . . ? 

C02 C03 C40 O1 172.7(3) . . . . ? 

C04 C03 C40 O1 -2.5(5) . . . . ? 

C02 C03 C40 C23 1.6(5) . . . . ? 

C04 C03 C40 C23 -173.6(3) . . . . ? 

C24 C23 C40 O1 -172.8(3) . . . . ? 

C22 C23 C40 O1 1.7(5) . . . . ? 

C24 C23 C40 C03 -1.6(5) . . . . ? 

C22 C23 C40 C03 173.0(3) . . . . ? 

C06 C05 C41 O7 178.0(3) . . . . ? 

C04 C05 C41 O7 -9.3(5) . . . . ? 

C06 C05 C41 C09 -3.3(5) . . . . ? 

C04 C05 C41 C09 169.4(3) . . . . ? 

C08 C09 C41 O7 -179.6(3) . . . . ? 

C10 C09 C41 O7 5.5(5) . . . . ? 

C08 C09 C41 C05 1.7(5) . . . . ? 

C10 C09 C41 C05 -173.1(3) . . . . ? 

C08 C07 C42 C44 65.7(5) . . . . ? 

C06 C07 C42 C44 -109.9(5) . . . . ? 

C08 C07 C42 C43 -172.9(4) . . . . ? 

C06 C07 C42 C43 11.5(6) . . . . ? 

C08 C07 C42 C45 -53.4(5) . . . . ? 

C06 C07 C42 C45 131.0(4) . . . . ? 

C20 C19 C46 C47 15.4(5) . . . . ? 

C18 C19 C46 C47 -169.6(3) . . . . ? 

C20 C19 C46 C49 136.6(4) . . . . ? 

C18 C19 C46 C49 -48.3(5) . . . . ? 

C20 C19 C46 C48 -104.1(4) . . . . ? 

C18 C19 C46 C48 71.0(4) . . . . ? 

C03 C40 O1 C30 89.1(4) . . . . ? 

C23 C40 O1 C30 -99.5(4) . . . . ? 

C31 C30 O1 C40 -178.4(3) . . . . ? 

C30 C31 O2 C32 -94.5(4) . . . . ? 

C33 C32 O2 C31 179.5(3) . . . . ? 

C35 C34 O3 C33 -176.0(4) . . . . ? 

C32 C33 O3 C34 168.0(4) . . . . ? 

C37 C36 O4 C35 172.0(3) . . . . ? 

C34 C35 O4 C36 -96.3(5) . . . . ? 

C11 C38 O5 C37 -93.3(4) . . . . ? 

C15 C38 O5 C37 91.7(4) . . . . ? 

C36 C37 O5 C38 167.0(3) . . . . ? 

 

_diffrn_measured_fraction_theta_max    0.999 

_diffrn_reflns_theta_full              23.55 

_diffrn_measured_fraction_theta_full   0.999 

_refine_diff_density_max    0.291 

_refine_diff_density_min   -0.223 

_refine_diff_density_rms    0.046 

