Phosph(on/in)ate-Bridged Vanadium(IV) Dimers: Synthesis and Characterization
Alexander E. Anderson; Michael P. Weberski; Craig C. McLauchlan; Inorganic Chemistry 51 (2012) 8719–8728; doi:10.1021/ic3002306

data_4330000
_publ_contact_author_address
; Department of Chemistry
  Illinois State University
  Campus Box 4160
  Normal, IL 61790-4160, USA
;
_publ_contact_author_email       mclauchlan@ilstu.edu
_publ_contact_author_fax         +(309)438-5538
_publ_contact_author_name        'Craig C. McLauchlan'
_publ_contact_author_phone       +(309)438-7019
_publ_section_title
;
 Phosph(on/in)ate-Bridged Vanadium(IV) Dimers: Synthesis and
 Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8719
_journal_page_last               8728
_journal_paper_doi               10.1021/ic3002306
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C46 H82 Co2 O24 P8 V2, 2 (H2 O1)'
_chemical_formula_sum            'C46 H86 Co2 O26 P8 V2'
_chemical_formula_weight         1522.65
_chemical_name_systematic
; 
 ? 
;
_chemical_temperature_decomposition 418(5)
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1414(6)
_cell_length_b                   15.3604(7)
_cell_length_c                   32.0801(14)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.915
_cell_measurement_theta_min      2.403
_cell_volume                     6475.6(5)
_computing_cell_refinement       'Apex2 v2008.2-4'
_computing_data_collection       'Apex2 v2008.2-4 (Bruker, 2008)'
_computing_data_reduction        'Apex2 v2008.2-4'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_structure_solution    'SHELXTL 6.14 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            36612
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-2 (Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       Block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0552P)^2^+21.4869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                6259
_reflns_number_total             7409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3002306_si_002_2.cif
_cod_data_source_block           4isu115
_cod_database_code               4330000