Heterobimetallic Complexes That Bond Vanadium to Iron, Cobalt, and Nickel.
Clouston, Laura J.; Bernales, Varinia; Cammarota, Ryan C.; Carlson, Rebecca K.; Bill, Eckhard; Gagliardi, Laura; Lu, Connie C.; Inorganic chemistry 54 (2015) 11669–11679; doi:10.1021/acs.inorgchem.5b01631

data_4346526
_publ_section_title
;
 Heterobimetallic Complexes That Bond Vanadium to Iron, Cobalt, and
 Nickel.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11669
_journal_page_last               11679
_journal_paper_doi               10.1021/acs.inorgchem.5b01631
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C39 H60 Co N4 P3 V, C24 H20 B, 2(C4 H8 O)'
_chemical_formula_sum            'C71 H96 B Co N4 O2 P3 V'
_chemical_formula_weight         1251.11
_chemical_name_common            3ox_[CoVL][BPh4]
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 100.6311(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3813(5)
_cell_length_b                   14.3313(4)
_cell_length_c                   26.5204(7)
_cell_measurement_reflns_used    8178
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      66.67
_cell_measurement_theta_min      3.39
_cell_volume                     6492.8(3)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'normal parabolic mirrors'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48756
_diffrn_reflns_theta_full        66.79
_diffrn_reflns_theta_max         66.79
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    4.271
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.4148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+19.3546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                7994
_reflns_number_total             11373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01631_si_002.cif
_cod_data_source_block           13282z_compound_3ox
_cod_original_cell_volume        6492.7(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4346526