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_4342830
_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_sum            'C53 H47 Cu F6 N9 O7 S2 V'
_chemical_formula_weight         1214.59
_chemical_name_common            XY05
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 113.311(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0595(7)
_cell_length_b                   15.3356(6)
_cell_length_c                   20.4359(8)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      32.3639
_cell_measurement_theta_min      2.4235
_cell_volume                     5197.8(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            90561
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.579
_refine_diff_density_min         -1.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         17326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+3.8048P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                14005
_reflns_number_total             17326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00370_si_002.cif
_cod_data_source_block           Cu
_cod_depositor_comments
'Adding full bibliography for 4342825--4342830.cif.'
_cod_database_code               4342830
_shelx_res_checksum              26280
_shelx_hkl_checksum              90418