(11<i>R</i>,11a<i>S</i>-<i>trans</i>)-11-Ethylthio-2,3,5,10,11,11a-hexahydro-1<i>H</i>-pyrrolo[2,1-<i>c</i>][1,4]benzodiazepin-5-one
Kubicki, Maciej; Szkaradzińska, Maria B.; Codding, Penelope W.; Acta Crystallographica Section C 53 (1997) 1288–1290; doi:10.1107/S0108270197005581

data_2006538
_publ_section_title
(11<i>R</i>,11a<i>S</i>-<i>trans</i>)-11-Ethylthio-2,3,5,10,11,11a-hexahydro-1<i>H</i>-pyrrolo[2,1-<i>c</i>][1,4]benzodiazepin-5-one
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1288
_journal_page_last               1290
_journal_paper_doi               10.1107/S0108270197005581
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C14 H18 N2 O S'
_chemical_formula_sum            'C14 H18 N2 O S'
_chemical_formula_weight         262.36
_chemical_name_systematic
;
(11R-trans)-11-ethylthio-1,2,3,10,11,11a-hexahydro--5H-pyrrolo[2,1-c][1,4]
benzodiazepin-5-one
;
_space_group_IT_number           78
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9850(8)
_cell_length_b                   8.9850(8)
_cell_length_c                   17.1652(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39
_cell_measurement_theta_min      14
_cell_volume                     1385.75(19)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'ENPROC (Rettig, 1978)'
_computing_molecular_graphics    'Stereochemical Workstation (Siemens, 1989)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4F diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3162
_diffrn_reflns_theta_max         74.73
_diffrn_reflns_theta_min         4.92
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  33
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.236
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.06(5)
_refine_ls_extinction_coef       0.0041(16)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         1472
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.240
_refine_ls_restrained_S_obs      1.283
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_obs          .0529
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.3355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1476
_refine_ls_wR_factor_obs         .1443
_reflns_number_gt                1347
_reflns_number_total             1472
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1103.cif
_cod_data_source_block           brm1
_cod_original_cell_volume        1385.8(2)
_cod_original_sg_symbol_H-M      P4~3~
_cod_database_code               2006538