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_4346523
_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 P3 Fe1 V1, 0.5(C7 H8)'
_chemical_formula_sum            'C42.5 H64 Fe N4 P3 V'
_chemical_formula_weight         830.68
_chemical_name_common            2_FeVL
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.92
_cell_angle_beta                 80.58
_cell_angle_gamma                82.81
_cell_formula_units_Z            2
_cell_length_a                   11.2034(4)
_cell_length_b                   14.1739(6)
_cell_length_c                   14.3424(6)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.435
_cell_measurement_theta_min      2.232
_cell_volume                     2117.09(15)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24610
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.8013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.8453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                7371
_reflns_number_total             9574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01631_si_002.cif
_cod_data_source_block           13002_0m_compound_2
_cod_original_cell_volume        2117.12(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C42.50 H64 Fe N4 P3 V'
_cod_database_code               4346523