Synthesis and Crystal Structures of Dinuclear Cobalt(III) Complexes with 1,3-Bis(5-nitrosalicylideneamino)-2-propanol and 1,3-Bis(3-nitrosalicylideneamino)-2-propanol
MIKURIYA, Masahiro; NAKA, Yuko; YOSHIOKA, Daisuke; HANDA, Makoto; X-ray Structure Analysis Online 32 (2016) 55–; doi:10.2116/xraystruct.32.55

data_1551616
_publ_section_title
;
 Synthesis and Crystal Structures of Dinuclear Cobalt(III) Complexes with
 1,3-Bis(5-nitrosalicylideneamino)-2-propanol and
 1,3-Bis(3-nitrosalicylideneamino)-2-propanol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              55
_journal_paper_doi               10.2116/xraystruct.32.55
_journal_volume                  32
_journal_year                    2016
_chemical_formula_sum            'C39 H37.5 Co2 N10 O15.75'
_chemical_formula_weight         1016.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 124.334(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.560(19)
_cell_length_b                   17.013(10)
_cell_length_c                   18.888(12)
_cell_measurement_reflns_used    26270
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.814
_cell_measurement_theta_min      1.563
_cell_volume                     8375(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.814
_diffrn_reflns_theta_min         1.563
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             4172
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6263
_reflns_number_total             10031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_55_1.txt
_cod_data_source_block           COYN253
_cod_original_formula_sum        'C39 H37.50 Co2 N10 O15.75'
_cod_database_code               1551616
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.668
_shelx_estimated_absorpt_t_max   0.810
_shelx_res_checksum              37059
_shelx_hkl_checksum              86674