2-Methyl-2,4-di-4-pyridyl-2,3-dihydro-1<i>H</i>-1,5-benzodiazepine acetic acid solvate
Wang, Shi-Chao; Hou, Qiu-Fei; Jiang, Shi-Mei; Acta Crystallographica Section E 65 (2009) o3213–; doi:10.1107/S1600536809049836

data_2224178
_publ_section_title
;
 2-Methyl-2,4-di-4-pyridyl-2,3-dihydro-1<i>H</i>-1,5-benzodiazepine
 acetic acid solvate
;
_journal_coeditor_code           CV2662
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3213
_journal_paper_doi               10.1107/S1600536809049836
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C20 H18 N4, C2 H4 O2'
_chemical_formula_moiety         'C20 H18 N4, C2 H4 O2'
_chemical_formula_sum            'C22 H22 N4 O2'
_chemical_formula_weight         374.44
_chemical_name_systematic
;2-Methyl-2,4-di-4-pyridyl-2,3-dihydro-1<i>H</i>-1,5-benzodiazepine acetic
 acid
solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.56(3)
_cell_angle_beta                 75.41(3)
_cell_angle_gamma                88.52(3)
_cell_formula_units_Z            2
_cell_length_a                   8.925(6)
_cell_length_b                   10.172(8)
_cell_length_c                   12.283(9)
_cell_measurement_reflns_used    6051
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.08
_cell_volume                     1001.8(13)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9946
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_correction_T_min  0.9910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1067P)^2^+0.0338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.2105
_reflns_number_gt                2400
_reflns_number_total             4547
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv2662.cif
_cod_data_source_block           I
_cod_original_cell_volume        1001.8(12)
_cod_database_code               2224178
_cod_database_fobs_code          2224178