4-Substituted 1-Methyl-1<i>H</i>-2,3-benzodiazepine Compounds
Blake, A. J.; Harding, M.; Sharp, J. T.; Acta Crystallographica Section C 51 (1995) 1621–1627; doi:10.1107/S0108270195001120

data_2003781
_publ_section_title
;
 4-Substituted 1-Methyl-1<i>H</i>-2,3-benzodiazepine Compounds
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1621
_journal_page_last               1627
_journal_paper_doi               10.1107/S0108270195001120
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C18 H18 N2 O'
_chemical_formula_sum            'C18 H18 N2 O'
_chemical_formula_weight         278.34
_chemical_name_systematic
;
 1-methyl-4(1'-methoxy-benzyl)-1H-2,3-benzodiazepine
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   6.350(5)
_cell_length_b                   10.954(8)
_cell_length_c                   21.118(18)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1469(2)
_computing_cell_refinement       'STADI4 version 1.04 (Stoe & Cie, 1995a)'
_computing_data_collection       'STADI4 version 1.04 (Stoe & Cie, 1995a)'
_computing_data_reduction        'X-DATRED version 1.02 (Stoe & Cie, 1995b)'
_computing_molecular_graphics    'SHELXTL/PC version 4.3 (Sheldrick, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer'
_diffrn_measurement_method
;
\w-2\q scans with \w width given by (1.2 + 0.35tan\q)^o^
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1529
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Lath
_exptl_crystal_F_000             592
_exptl_crystal_size_max          1.14
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.412
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   1(4)
_refine_ls_extinction_coef       0.002(5)
_refine_ls_extinction_method
'F~c~^*^ = kF~c~[1 + 0.001xF~c~^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_obs          0.0552
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^) + (0.1064P)^2^ + 0.2300P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1591
_refine_ls_wR_factor_obs         0.1379
_reflns_number_observed          1283
_reflns_number_total             1529
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1139.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1469.(2)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2003781