Syntheses, X-ray Structural Characterizations, and Thermal Stabilities of Two Nonclassical Trinuclear Vanadium(IV) Complexes, (V3(μ3-O)O2)(μ2-O2P(CH2C6H5)2)6(H2O) and (V3(μ3-O)O2)(μ2-O2P(CH2C6H5)2)6(py), and Polymeric Complexes of Stoichiometry (VO(O2PR2)2)\ιnfty, R2 = Ph2 and o-(CH2)2(C6H4)
John S. Maass; Zhichao Chen; Matthias Zeller; Floriana Tuna; Richard E. P. Winpenny; Rudy L. Luck; Inorganic Chemistry 51 (2012) 2766–2776; doi:10.1021/ic201259u

data_4328478
_publ_contact_author_address
;
Department of Chemistry
Michigan Technological University
1400 Townsend Drive
Houghton, MI USA 49931
;
_publ_contact_author_email       rluck@mtu.edu
_publ_contact_author_fax         '(906)487 2061'
_publ_contact_author_name        'Luck, Rudy L.'
_publ_contact_author_phone       '(906)487 2309'
_publ_section_title
;
 Syntheses, X-ray Structural Characterizations, and Thermal Stabilities of
 Two Nonclassical Trinuclear Vanadium(IV) Complexes,
 (V3(\m3-O)O2)(\m2-O2P(CH2C6H5)2)6(H2O) and
 (V3(\m3-O)O2)(\m2-O2P(CH2C6H5)2)6(py), and Polymeric Complexes of
 Stoichiometry (VO(O2PR2)2)\\infty, R2 = Ph2 and o-(CH2)2(C6H4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2766
_journal_page_last               2776
_journal_paper_doi               10.1021/ic201259u
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C84 H86 O16 P6 V3), 7.0(C H2 Cl2)'
_chemical_formula_sum            'C175 H186 Cl14 O32 P12 V6'
_chemical_formula_weight         3974.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-05-18T16:08:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.804(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.630(10)
_cell_length_b                   20.903(8)
_cell_length_c                   16.779(7)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4198
_cell_measurement_theta_min      2.4254
_cell_measurement_wavelength     0.71073
_cell_volume                     9339(6)
_computing_cell_refinement       'SAINT V7.66A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.579162E-1
_diffrn_orient_matrix_UB_12      0.105985E-1
_diffrn_orient_matrix_UB_13      0.359792E-2
_diffrn_orient_matrix_UB_21      -0.55322E-2
_diffrn_orient_matrix_UB_22      0.182157E-2
_diffrn_orient_matrix_UB_23      0.373167E-1
_diffrn_orient_matrix_UB_31      0.129517E-1
_diffrn_orient_matrix_UB_32      -0.466152E-1
_diffrn_orient_matrix_UB_33      0.227624E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66641
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         0.76
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       plate
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00070(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         25531
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+15.7040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2125
_reflns_number_gt                15719
_reflns_number_total             25531
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201259u_si_002_2.cif
_cod_data_source_block           new
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328478