Five closely related 4-chloro-6,11-dihydro-5<i>H</i>-benzo[<i>b</i>]pyrimido[5,4-<i>f</i>]azepines: similar molecular structures but different supramolecular assemblies
Acosta, Lina M.; Jurado, Jorge; Palma, Alirio; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615020811

data_2020295
_publ_section_title
;
 Five closely related
 4-chloro-6,11-dihydro-5<i>H</i>-benzo[<i>b</i>]pyrimido[5,4-<i>f</i>]azepines:
 similar molecular structures but different supramolecular assemblies
;
_journal_coeditor_code           YF3094
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615020811
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C14 H14 Cl N3 O'
_chemical_formula_moiety         'C14 H14 Cl N3 O'
_chemical_formula_sum            'C14 H14 Cl N3 O'
_chemical_formula_weight         275.73
_chemical_name_systematic
(6<i>RS</i>)-4-Chloro-8-hydroxy-6,11-dimethyl-6,11-dihydro-5<i>H</i>-benzo[<i>b</i>]pyrimido[5,4-<i>f</i>]azepine
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 116.216(6)
_cell_angle_gamma                90
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_cell_length_c                   8.0709(6)
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_cell_measurement_temperature    120(2)
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_computing_cell_refinement
;
DIRAX/LSQ (Duisenberg <i>et al.</i>,  2000)
;
_computing_data_collection
;
COLLECT (Nonius, 1999)
;
_computing_data_reduction
;
EVALCCD (Duisenberg <i>et al.</i>,  2003)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
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SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
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_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.390
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
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_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
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_exptl_crystal_size_max          0.320
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_exptl_crystal_size_min          0.160
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_refine_diff_density_min         -0.283
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2870
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0280P)^2^+1.1981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2154
_reflns_number_total             2870
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3094sup1.cif
_cod_data_source_block           II
_cod_database_code               2020295
_cod_database_fobs_code          2020295
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.954
_shelx_hkl_checksum              93037
_shelx_res_checksum              30715
_shelxl_version_number           2.014