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_4346527
_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 N4 Ni P3 V, C6 H6'
_chemical_formula_sum            'C45 H66 N4 Ni P3 V'
_chemical_formula_weight         865.61
_chemical_name_common            4_NiVL
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.875(3)
_cell_length_b                   10.875(3)
_cell_length_c                   21.431(6)
_cell_measurement_reflns_used    2595
_cell_measurement_temperature    173(2)
_cell_volume                     2195.0(11)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10182
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagons
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.216
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0633P)^2^+3.3046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                2455
_reflns_number_total             3270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01631_si_002.cif
_cod_data_source_block           13150_0m_compound_4
_cod_original_cell_volume        2194.9(11)
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               4346527