Bis[2,2'-ethylenedioxydibenzaldehyde bis(thiocarbohydrazide)] tris(pyridine) solvate
Chantrapromma, Suchada; Razak, Ibrahim Abdul; Fun, Hoong-Kun; Karalai, Chatchanok; Zhang, Hao; Xie, Fu-Xin; Tian, Yu-Peng; Ma, Wen; Zhang, Yin-Han; Ni, Shi-Sheng; Acta Crystallographica Section C 57 (2001) 289–290; doi:10.1107/S0108270100017972

data_2011823
_publ_section_title
;
 Bis[2,2'-ethylenedioxydibenzaldehyde bis(thiocarbohydrazide)]
 tris(pyridine) solvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              289
_journal_page_last               290
_journal_paper_doi               10.1107/S0108270100017972
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C34 H32 N8 O4 S2, 3C5 H5 N'
_chemical_formula_sum            'C49 H47 N11 O4 S2'
_chemical_formula_weight         918.10
_chemical_name_systematic
;
Bis[2,2'-ethylenedioxydibenzaldehyde bis(thiocarbohydrazide)] tripyridine
;
_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'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 117.1680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1752(2)
_cell_length_b                   22.20290(10)
_cell_length_c                   19.8479(4)
_cell_measurement_reflns_used    5918
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.11
_cell_measurement_theta_min      2.77
_cell_volume                     4773.42(13)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PLATON (Spek, 1990)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .995
_diffrn_measured_fraction_theta_max .995
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .043
_diffrn_reflns_av_sigmaI/netI    .060
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30445
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .168
_exptl_absorpt_correction_T_max  .955
_exptl_absorpt_correction_T_min  .941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          .37
_exptl_crystal_size_mid          .33
_exptl_crystal_size_min          .28
_refine_diff_density_max         .46
_refine_diff_density_min         -.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         10907
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          .135
_refine_ls_R_factor_gt           .068
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0460P)^2^+2.8579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .166
_reflns_number_gt                5918
_reflns_number_total             10907
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1435.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2011823
_cod_database_fobs_code          2011823