Crystal structure of diazido-bis(μ2-pyridin-2-ylmethanolato-κ2 N:O)-bis(pyridin-2-ylmethanolato-κ2 N,O)dicobalt(III) – methanol (1/3), C27H35Co2N10O7
Youzhu, Yu; Yanhong, Shen; Yongsheng, Niu; Xiaoming, Zheng; Xi, Han; Songyang, Chang; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 611–613; doi:10.1515/ncrs-2017-0368

data_8106233
_publ_section_title
;
 Crystal structure of diazido-bis(\m2-pyridin-2-ylmethanolato-\k2
 N:O)-bis(pyridin-2-ylmethanolato-\k2 N,O)dicobalt(III) -- methanol (1/3),
 C27H35Co2N10O7
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              611
_journal_page_last               613
_journal_paper_doi               10.1515/ncrs-2017-0368
_journal_volume                  233
_journal_year                    2018
_chemical_formula_sum            'C27 H35 Co2 N10 O7'
_chemical_formula_weight         729.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.6280(13)
_cell_length_b                   7.5784(3)
_cell_length_c                   14.3600(7)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.77
_cell_volume                     3224.3(2)
_computing_cell_refinement       'Bruker SAINT [16]'
_computing_data_collection       'Bruker APEX2 [15]'
_computing_data_reduction        'Bruker SAINT [16]'
_computing_molecular_graphics    'SHELXL-2013 [18]'
_computing_publication_material  'SHELXL-2013 [18]'
_computing_structure_refinement  'SHELXL-2013 [17]'
_computing_structure_solution    'SHELXS-2013 [17]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41911
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.291
_diffrn_reflns_theta_min         2.837
_exptl_absorpt_coefficient_mu    1.089
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 3083 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.036(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0614P)^2^+0.6083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                7048
_reflns_number_total             7954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0368_suppl.cif
_cod_data_source_block           1
_cod_database_code               8106233
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.845