Chemical Bond Characterization of a Mixed-Valence Tri-Cobalt Complex, Co3(μ-admtrz)4(μ-OH)2(CN)6.2H2O
Lai-Chin Wu; Tsu-Chien Weng; I-Jui Hsu; Yi-Hung Liu; Gene-Hsiang Lee; Jyh-Fu, Lee; Yu Wang; Inorganic Chemistry 52 (2013) 11023–11033; doi:10.1021/ic401147b

data_4336165
_publ_section_title
;
 Chemical Bond Characterization of a Mixed-Valence Tri-Cobalt Complex,
 Co3(\m-admtrz)4(\m-OH)2(CN)6.2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11023
_journal_page_last               11033
_journal_paper_doi               10.1021/ic401147b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H42 Co3 N22 O6'
_chemical_formula_weight         887.57
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 103.0260(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.82740(10)
_cell_length_b                   9.82110(8)
_cell_length_c                   17.73730(2)
_cell_measurement_reflns_used    583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     1837.60(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford CCD diffractometer'
_diffrn_measurement_method       'Omega scan+phi scan'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            153502
_diffrn_reflns_theta_full        48.67
_diffrn_reflns_theta_max         48.67
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.8515
_exptl_absorpt_correction_T_min  0.7224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
A combination of a face-indexed absorption and a multi-scan 
correction (in SADABS) was applied.
The crystal faces were indexed, and distances measured using the CrystAlis
software.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         18076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                12653
_reflns_number_total             18076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401147b_si_002.cif
_cod_data_source_block           ic13189
_cod_database_code               4336165