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_1551615
_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            'C38.5 H35.75 Co2 N9.75 O15.25'
_chemical_formula_weight         996.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                109.245(3)
_cell_angle_beta                 95.243(4)
_cell_angle_gamma                92.303(3)
_cell_formula_units_Z            2
_cell_length_a                   10.816(2)
_cell_length_b                   12.803(2)
_cell_length_c                   15.812(3)
_cell_measurement_reflns_used    12050
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.135
_cell_measurement_theta_min      2.444
_cell_volume                     2052.8(6)
_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 0.985
_diffrn_measured_fraction_theta_max 0.872
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12050
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.135
_diffrn_reflns_theta_min         2.444
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             1022
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         8755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5270
_reflns_number_total             8755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_55_2.txt
_cod_data_source_block           COYN316
_cod_original_cell_volume        2052.8(7)
_cod_original_formula_sum        'C38.50 H35.75 Co2 N9.75 O15.25'
_cod_database_code               1551615
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.863
_shelx_res_checksum              80679
_shelx_hkl_checksum              23948