Molecular Conformation and Crystallization: The Case of Ethenzamide
Back, Kevin R.; Davey, Roger J.; Grecu, Tudor; Hunter, Christopher A.; Taylor, Lynne S.; Crystal Growth & Design 12 (2012) 6110–; doi:10.1021/cg301244x

data_4517046
_publ_section_title
;
 Molecular Conformation and Crystallization: The Case of Ethenzamide
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6110
_journal_paper_doi               10.1021/cg301244x
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C9 H11 N O2'
_chemical_formula_sum            'C9 H11 N O2'
_chemical_formula_weight         165.19
_chemical_melting_point          402
_chemical_name_systematic        2-ethoxybenzamide
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-06
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_audit_update_record
;
2012-07-08 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.774(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.0512(8)
_cell_length_b                   12.027(3)
_cell_length_c                   14.251(3)
_cell_measurement_reflns_used    905
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.2192
_cell_measurement_theta_min      3.3275
_cell_volume                     859.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details
;
  1 omega -111.00  -49.00   1.0000  380.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2308  179.0000 -180.0000 62

  2 omega   -8.00  105.00   1.0000  380.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7933   77.0000   90.0000 113

  3 omega  -55.00    5.00   1.0000  380.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7933  -37.0000    0.0000 60
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0262538622
_diffrn_orient_matrix_UB_12      0.0502732887
_diffrn_orient_matrix_UB_13      0.0100179710
_diffrn_orient_matrix_UB_21      -0.0426589614
_diffrn_orient_matrix_UB_22      0.0307071545
_diffrn_orient_matrix_UB_23      -0.0166804616
_diffrn_orient_matrix_UB_31      -0.0009222728
_diffrn_orient_matrix_UB_32      0.0000035909
_diffrn_orient_matrix_UB_33      0.1402560780
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.1544
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3309
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             352
_exptl_crystal_preparation       'Aldrich as supplied'
_exptl_crystal_recrystallization_method 'MeCN cooling crystallisation'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.2530
_refine_ls_R_factor_gt           0.1378
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+3.0551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2961
_refine_ls_wR_factor_ref         0.3519
_reflns_number_gt                854
_reflns_number_total             1898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301244x_si_002.cif
_cod_data_source_block           ord68
_cod_database_code               4517046
_chemical_oxdiff_formula         C9N1O2H11
_reflns_odcompleteness_completeness 98.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32