Temperature-Dependent Ordering of the Methyl Group in the Crystal Structure of 5-(2-Chlorophenyl)-7-ethyl-1H-thieno [2,3-E][1,4]diazepin-2(3H)-one
Dutkiewicz, Grzegorz; Kubicki, Maciej; Dayananda, Alaloor S.; Yathirajan, Hemmige S.; Ramesha, Andagar R.; Crystals 2 (2012) 1347–1356; doi:10.3390/cryst2031347

data_1508495
_publ_section_title
;
 Temperature-Dependent Ordering of the Methyl Group in the Crystal
 Structure of 5-(2-Chlorophenyl)-7-ethyl-1H-thieno
 [2,3-E][1,4]diazepin-2(3H)-one
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              1347
_journal_page_last               1356
_journal_paper_doi               10.3390/cryst2031347
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C15 H13 Cl N2 O S'
_chemical_formula_weight         304.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.726(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1766(19)
_cell_length_b                   11.2809(14)
_cell_length_c                   8.9334(14)
_cell_measurement_reflns_used    1160
_cell_measurement_temperature    380(1)
_cell_measurement_theta_max      28.8142
_cell_measurement_theta_min      2.9236
_cell_volume                     1511.7(4)
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_collection       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      380(1)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6031
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2942
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.3814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                1625
_reflns_number_total             2942
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file
C15H13ClN2OS_P21_c_08_230_d_crystals-02-01347-s001_DC227.cif
_cod_data_source_block           8_230_chateigner_1508495
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1508495