Synthesis of Unsupported d(1)-d(x) Oxido-Bridged Heterobimetallic Complexes Containing V(IV): A New Direction for Metal-to-Metal Charge Transfer.
Wu, Xinyuan; Huang, Tao; Lekich, Travis T.; Sommer, Roger D.; Weare, Walter W.; Inorganic chemistry 54 (2015) 5322–5328; doi:10.1021/acs.inorgchem.5b00370

data_4342829
_publ_section_title
;
 Synthesis of Unsupported d(1)-d(x) Oxido-Bridged Heterobimetallic
 Complexes Containing V(IV): A New Direction for Metal-to-Metal Charge
 Transfer.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5322
_journal_page_last               5328
_journal_paper_doi               10.1021/acs.inorgchem.5b00370
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C51 H47 Ni N9 O V, 2(C F3 O3 S), H2 O'
_chemical_formula_sum            'C53 H49 F6 N9 Ni O8 S2 V'
_chemical_formula_weight         1227.78
_chemical_name_common            XW-VONi
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 113.556(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3482(6)
_cell_length_b                   15.7837(4)
_cell_length_c                   19.1046(6)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      25.6301
_cell_measurement_theta_min      2.3258
_cell_volume                     5071.7(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60975
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.432
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         9624
_refine_ls_number_restraints     754
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0327P)^2^+5.5072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                7407
_reflns_number_total             9624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00370_si_002.cif
_cod_data_source_block           Ni
_cod_depositor_comments
'Adding full bibliography for 4342825--4342830.cif.'
_cod_database_code               4342829
_shelx_res_checksum              38539
_shelx_hkl_checksum              33761