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_4330003
_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         '(K)4, C74 H162 Co4 O66 P18 V8'
_chemical_formula_sum            'C74 H162 Co4 K4 O66 P18 V8'
_chemical_formula_weight         3465.14
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 97.814(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.677(4)
_cell_length_b                   19.465(3)
_cell_length_c                   26.336(4)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4660
_cell_measurement_theta_min      2.2335
_cell_volume                     14056(4)
_computing_cell_refinement       'SAINT+ 6.45 (Bruker, 2003)'
_computing_data_collection       'SMART 5.630 (Bruker, 1997-2002)'
_computing_data_reduction        'SAINT+ 6.45'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21342
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SAINT+
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       rod
_exptl_crystal_F_000             7088
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
As noted above, there is a disordered region of electron density on a special
position.  The sturcture is of marginal quality, so the region of electron
density was removed using SQUEEZE.  Prior to removal, the molecular
structure and size of the q peaks were consistent with a DMF molecule.
;
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         21342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0726P)^2^+84.1669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1738
_reflns_number_gt                14559
_reflns_number_total             21342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3002306_si_002_5.cif
_cod_data_source_block           8aisu135
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4330003