[<i>N</i>'-(3-Methoxy-2-oxidobenzylidene-κ<i>O</i>^2^)benzohydrazidato-κ^2^<i>N</i>',<i>O</i>]tris(pyridine-κ<i>N</i>)cobalt(III) perchlorate
Yu, Gui-Miao; Yang, Xiu-Yun; Wang, Yuan; Xiao, Ya-Juan; Li, Yun-Hui; Acta Crystallographica Section E 67 (2011) m329–; doi:10.1107/S1600536811004715

data_2229455
_publ_section_title
;
 [<i>N</i>'-(3-Methoxy-2-oxidobenzylidene-\k<i>O</i>^2^)benzohydrazidato-\k^2^<i>N</i>',<i>O</i>]tris(pyridine-\k<i>N</i>)cobalt(III)
 perchlorate
;
_journal_coeditor_code           MW2001
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m329
_journal_paper_doi               10.1107/S1600536811004715
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C15 H12 N2 O3) (C5 H5 N)3] Cl O4'
_chemical_formula_moiety         'C30 H27 Co N5 O3 +, Cl O4 -'
_chemical_formula_sum            'C30 H27 Cl Co N5 O7'
_chemical_formula_weight         663.95
_chemical_name_systematic
;
[<i>N</i>'-(3-Methoxy-2-oxidobenzylidene-\k<i>O</i>^2^)benzohydrazidato-
\k^2^<i>N</i>',<i>O</i>]tris(pyridine-\k<i>N</i>)cobalt(III) perchlorate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7591(5)
_cell_length_b                   13.2318(6)
_cell_length_c                   21.0558(10)
_cell_measurement_reflns_used    4029
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      50.067
_cell_measurement_theta_min      4.890
_cell_volume                     2987.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 1999)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7543
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_correction_T_min  0.8694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.291
_refine_ls_abs_structure_details 'Flack (1983), 2332 Friedel pairs'
_refine_ls_abs_structure_Flack   0.011(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4991
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                4431
_reflns_number_total             4991
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mw2001.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2229455
_cod_database_fobs_code          2229455