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_4330004
_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         'C111 H207 Co6 O98 P27 V12, 6(K), 6(H2 O)'
_chemical_formula_sum            'C111 H219 Co6 K6 O104 P27 V12'
_chemical_formula_weight         5219.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                109.582(2)
_cell_angle_beta                 90.397(2)
_cell_angle_gamma                118.739(2)
_cell_formula_units_Z            1
_cell_length_a                   17.116(2)
_cell_length_b                   17.308(2)
_cell_length_c                   23.670(3)
_cell_measurement_reflns_used    8493
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.524
_cell_measurement_theta_min      3.325
_cell_volume                     5671.6(12)
_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, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0919
_diffrn_reflns_av_sigmaI/netI    0.2092
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            64789
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-2 (Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.281
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1221
_refine_ls_number_reflns         32949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.2996
_refine_ls_R_factor_gt           0.1338
_refine_ls_shift/su_max          2.200
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1983P)^2^+22.9571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3621
_refine_ls_wR_factor_ref         0.4558
_reflns_number_gt                10413
_reflns_number_total             32949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3002306_si_002_6.cif
_cod_data_source_block           8bisu127
_cod_original_cell_volume        5671.4(13)
_cod_database_code               4330004