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)∞, 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_4328477
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C89 H89 N1 O15 P6 V3'
_chemical_formula_sum            'C89 H89 N O15 P6 V3'
_chemical_formula_weight         1751.25
_chemical_name_systematic
;aa
 ?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
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_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-08-06T20:21:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.300(10)
_cell_angle_beta                 103.970(10)
_cell_angle_gamma                110.889(2)
_cell_formula_units_Z            1
_cell_length_a                   13.248(2)
_cell_length_b                   13.779(2)
_cell_length_c                   14.0500(10)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9125
_cell_measurement_theta_min      2.4328
_cell_measurement_wavelength     0.71073
_cell_volume                     2086.7(5)
_computing_cell_refinement       'SAINT V7.66A integration software'
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_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.862
_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'
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_diffrn_orient_matrix_UB_12      0.264659E-1
_diffrn_orient_matrix_UB_13      0.606201E-2
_diffrn_orient_matrix_UB_21      0.557276E-1
_diffrn_orient_matrix_UB_22      0.48512E-1
_diffrn_orient_matrix_UB_23      0.811436E-1
_diffrn_orient_matrix_UB_31      0.450528E-1
_diffrn_orient_matrix_UB_32      0.698246E-1
_diffrn_orient_matrix_UB_33      -0.771239E-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  0.0242
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_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_theta_max         31.43
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.51
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            green
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_exptl_crystal_description       block
_exptl_crystal_F_000             909
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.08
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         21017
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.099
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                17633
_reflns_number_total             21017
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201259u_si_002_1.cif
_cod_data_source_block           new
_cod_database_code               4328477