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_4330001
_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_sum            'C46 H82 Co2 O26 P8 V2'
_chemical_formula_weight         1518.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.684(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2986(12)
_cell_length_b                   25.4641(24)
_cell_length_c                   20.5721(20)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.372
_cell_measurement_theta_min      2.174
_cell_volume                     6410.9(11)
_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 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Giacovazzo et al, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48531
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.99
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-2 (Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             3142
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.528(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         28302
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0599P)^2^+14.0785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                22866
_reflns_number_total             28302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3002306_si_002_3.cif
_cod_data_source_block           5isu143
_cod_original_cell_volume        6411(1)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4330001