 

data_9911

 

_audit_creation_method            SHELXL

_chemical_name_systematic         Methyl 3-(2-methyl-acroylamido)-2-phenylacetylamino-acrylate

;

 Methyl 3-(2-methyl-acroylamido)-2-phenylacetylamino-acrylate



;

_chemical_name_common             ?

_chemical_formula_moiety          ?

_chemical_formula_structural      ?

_chemical_formula_analytical      ?

_chemical_formula_sum             'C15 H15 N2 O4'

_chemical_formula_weight          287.29

_chemical_melting_point           ?

_chemical_compound_source         ?

 

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'

 'N'  'N'   0.0061   0.0033

 '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    ?

 

loop_

 _symmetry_equiv_pos_as_xyz

 'x, y, z'

 '-x+1/2, y+1/2, -z+1/2'

 '-x, -y, -z'

 'x-1/2, -y-1/2, z-1/2'

 

_cell_length_a                    16.744

_cell_length_b                    4.719

_cell_length_c                    19.995

_cell_angle_alpha                 90.00

_cell_angle_beta                  102.70

_cell_angle_gamma                 90.00

_cell_volume                      1541.0

_cell_formula_units_Z             4

_cell_measurement_temperature     293(2)

_cell_measurement_reflns_used     ?

_cell_measurement_theta_min       ?

_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     1.238

_exptl_crystal_density_method     ?

_exptl_crystal_F_000              604

_exptl_absorpt_coefficient_mu     0.091

_exptl_absorpt_correction_type    ?

_exptl_absorpt_correction_T_min   ?

_exptl_absorpt_correction_T_max   ?

 

_exptl_special_details

;

 ?

;

 

_diffrn_ambient_temperature       293(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        ?

_diffrn_measurement_method        ?

_diffrn_standards_number          ?

_diffrn_standards_interval_count  ?

_diffrn_standards_interval_time   ?

_diffrn_standards_decay_%         ?

_diffrn_reflns_number             2812

_diffrn_reflns_av_R_equivalents   0.0089

_diffrn_reflns_av_sigmaI/netI     0.0166

_diffrn_reflns_limit_h_min        0

_diffrn_reflns_limit_h_max        15

_diffrn_reflns_limit_k_min        -1

_diffrn_reflns_limit_k_max        5

_diffrn_reflns_limit_l_min        -20

_diffrn_reflns_limit_l_max        20

_diffrn_reflns_theta_min          2.88

_diffrn_reflns_theta_max          25.44

_reflns_number_total              2539

_reflns_number_observed           1914

_reflns_observed_criterion        >2sigma(I)

 

_computing_data_collection        ?

_computing_cell_refinement        ?

_computing_data_reduction         ?

_computing_structure_solution     ?

_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'

_computing_molecular_graphics     ?

_computing_publication_material   ?

 

_refine_special_details

;

 Refinement on F² for ALL reflections except for 0 with very negative F²

 or flagged by the user for potential systematic errors.  Weighted R-factors

 wR and all goodnesses of fit S are based on F², conventional R-factors R

 are based on F, with F set to zero for negative F². The observed criterion

 of F² > 2sigma(F²) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1768P)^2^+1.7095P] where P=(Fo^2^+2Fc^2^)/3'

_atom_sites_solution_primary      direct

_atom_sites_solution_secondary    difmap

_atom_sites_solution_hydrogens    geom

_refine_ls_hydrogen_treatment     ?

_refine_ls_extinction_method      none

_refine_ls_extinction_coef        ?

_refine_ls_number_reflns          2539

_refine_ls_number_parameters      199

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.1097

_refine_ls_R_factor_obs           0.0911

_refine_ls_wR_factor_all          0.2921

_refine_ls_wR_factor_obs          0.2654

_refine_ls_goodness_of_fit_all    1.092

_refine_ls_goodness_of_fit_obs    1.151

_refine_ls_restrained_S_all       1.092

_refine_ls_restrained_S_obs       1.151

_refine_ls_shift/esd_max          0.041

_refine_ls_shift/esd_mean         0.008

 

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_thermal_displace_type

 _atom_site_occupancy

 _atom_site_calc_flag

 _atom_site_refinement_flags

 _atom_site_disorder_group

O15 O 0.6003(2) 1.2492(6) 0.80109(14) 0.0520(8) Uani 1 d . .

O11 O 0.6436(2) 1.1386(7) 1.01374(14) 0.0600(9) Uani 1 d . .

O8 O 0.8473(2) 0.5255(8) 0.9847(2) 0.0722(11) Uani 1 d . .

N13 N 0.5787(2) 0.8233(7) 0.8461(2) 0.0444(9) Uani 1 d . .

O10 O 0.5314(2) 1.2198(8) 0.9320(2) 0.0710(10) Uani 1 d . .

N3 N 0.7313(2) 0.5417(7) 0.9019(2) 0.0433(8) Uani 1 d . .

C2 C 0.6988(2) 0.7481(8) 0.9364(2) 0.0424(9) Uani 1 d . .

C17 C 0.4361(2) 1.1390(8) 0.7113(2) 0.0425(9) Uani 1 d . .

C1 C 0.6276(2) 0.8831(8) 0.9116(2) 0.0433(10) Uani 1 d . .

C5 C 0.8448(3) 0.2284(9) 0.8893(2) 0.0528(11) Uani 1 d . .

C16 C 0.5069(3) 0.9333(9) 0.7301(2) 0.0523(11) Uani 1 d . .

C9 C 0.5948(3) 1.0967(9) 0.9523(2) 0.0470(10) Uani 1 d . .

C4 C 0.8090(2) 0.4413(9) 0.9301(2) 0.0466(10) Uani 1 d . .

C14 C 0.5659(2) 1.0164(7) 0.7953(2) 0.0414(9) Uani 1 d . .

C22 C 0.3983(3) 1.2580(9) 0.7601(2) 0.0520(11) Uani 1 d . .

C18 C 0.4073(3) 1.2093(10) 0.6424(2) 0.0585(12) Uani 1 d . .

C6 C 0.8075(3) 0.1633(13) 0.8231(3) 0.0737(15) Uani 1 d . .

C21 C 0.3338(3) 1.4427(11) 0.7418(3) 0.0639(13) Uani 1 d . .

C20 C 0.3056(3) 1.5157(12) 0.6726(3) 0.0717(14) Uani 1 d . .

C12 C 0.6145(4) 1.3343(11) 1.0592(2) 0.0709(15) Uani 1 d . .

C7 C 0.9238(4) 0.1122(15) 0.9246(3) 0.087(2) Uani 1 d . .

C19 C 0.3421(3) 1.3982(13) 0.6242(3) 0.075(2) Uani 1 d . .

 

loop_

 _atom_site_aniso_label

 _atom_site_aniso_U_11

 _atom_site_aniso_U_22

 _atom_site_aniso_U_33

 _atom_site_aniso_U_23

 _atom_site_aniso_U_13

 _atom_site_aniso_U_12

O15 0.060(2) 0.0326(14) 0.056(2) -0.0020(12) -0.0036(13) -0.0056(12)

O11 0.069(2) 0.059(2) 0.047(2) -0.0156(14) 0.0038(14) 0.014(2)

O8 0.065(2) 0.087(3) 0.054(2) -0.009(2) -0.010(2) 0.014(2)

N13 0.049(2) 0.033(2) 0.048(2) -0.0042(13) 0.0026(14) 0.0008(13)

O10 0.062(2) 0.076(2) 0.070(2) -0.019(2) 0.005(2) 0.023(2)

N3 0.047(2) 0.037(2) 0.043(2) -0.0007(13) 0.0040(14) 0.0044(14)

C2 0.046(2) 0.035(2) 0.045(2) -0.001(2) 0.008(2) -0.002(2)

C17 0.045(2) 0.035(2) 0.044(2) -0.003(2) 0.003(2) -0.006(2)

C1 0.051(2) 0.033(2) 0.042(2) 0.000(2) 0.002(2) -0.002(2)

C5 0.052(3) 0.044(2) 0.065(3) 0.011(2) 0.018(2) 0.005(2)

C16 0.055(3) 0.038(2) 0.054(2) -0.010(2) -0.010(2) 0.005(2)

C9 0.047(3) 0.043(2) 0.050(2) -0.001(2) 0.009(2) 0.001(2)

C4 0.047(2) 0.048(2) 0.043(2) 0.009(2) 0.004(2) 0.000(2)

C14 0.045(2) 0.029(2) 0.048(2) -0.004(2) 0.005(2) 0.005(2)

C22 0.053(3) 0.051(2) 0.051(2) 0.000(2) 0.010(2) 0.000(2)

C18 0.055(3) 0.065(3) 0.048(2) 0.001(2) -0.004(2) 0.004(2)

C6 0.071(3) 0.078(4) 0.074(3) -0.021(3) 0.021(3) 0.003(3)

C21 0.056(3) 0.064(3) 0.073(3) -0.001(2) 0.016(2) 0.006(2)

C20 0.058(3) 0.072(3) 0.077(3) 0.001(3) -0.001(2) 0.009(3)

C12 0.095(4) 0.066(3) 0.055(3) -0.022(2) 0.024(3) 0.008(3)

C7 0.073(4) 0.099(4) 0.089(4) 0.025(3) 0.020(3) 0.035(3)

C19 0.074(3) 0.082(4) 0.061(3) 0.009(3) -0.005(2) 0.020(3)

 

_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

O15 C14 1.234(5) . ?

O11 C9 1.331(5) . ?

O11 C12 1.452(5) . ?

O8 C4 1.205(5) . ?

N13 C14 1.345(5) . ?

N13 C1 1.412(5) . ?

O10 C9 1.201(5) . ?

N3 C2 1.373(5) . ?

N3 C4 1.384(5) . ?

C2 C1 1.346(6) . ?

C17 C22 1.392(6) . ?

C17 C18 1.395(6) . ?

C17 C16 1.514(6) . ?

C1 C9 1.476(6) . ?

C5 C6 1.367(7) . ?

C5 C7 1.462(7) . ?

C5 C4 1.500(6) . ?

C16 C14 1.505(5) . ?

C22 C21 1.372(6) . ?

C18 C19 1.394(7) . ?

C21 C20 1.403(7) . ?

C20 C19 1.372(7) . ?

 

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

C9 O11 C12 116.7(4) . . ?

C14 N13 C1 121.9(3) . . ?

C2 N3 C4 118.6(3) . . ?

C1 C2 N3 124.5(4) . . ?

C22 C17 C18 118.9(4) . . ?

C22 C17 C16 122.4(4) . . ?

C18 C17 C16 118.6(4) . . ?

C2 C1 N13 122.2(4) . . ?

C2 C1 C9 121.8(3) . . ?

N13 C1 C9 116.0(3) . . ?

C6 C5 C7 123.8(5) . . ?

C6 C5 C4 121.6(4) . . ?

C7 C5 C4 114.5(4) . . ?

C14 C16 C17 112.2(3) . . ?

O10 C9 O11 123.9(4) . . ?

O10 C9 C1 123.6(4) . . ?

O11 C9 C1 112.6(3) . . ?

O8 C4 N3 121.4(4) . . ?

O8 C4 C5 121.2(4) . . ?

N3 C4 C5 117.4(3) . . ?

O15 C14 N13 122.6(3) . . ?

O15 C14 C16 121.1(3) . . ?

N13 C14 C16 116.3(3) . . ?

C21 C22 C17 121.5(4) . . ?

C19 C18 C17 119.4(4) . . ?

C22 C21 C20 119.5(5) . . ?

C19 C20 C21 119.4(5) . . ?

C20 C19 C18 121.3(4) . . ?

 

_refine_diff_density_max    0.630

_refine_diff_density_min   -0.332

_refine_diff_density_rms    0.090



#===END