Crystal-to-Crystal Oxidative Deprotonation of a Di(μ-hydroxo) to a Di(μ-oxo) Dimer of Dimolybdenum Units
F. Albert Cotton; Zhong Li; Carlos A. Murillo; Xiaoping Wang; Rongmin Yu; Qinliang Zhao; Inorganic Chemistry 46 (2007) 3245–3250; doi:10.1021/ic062443v

data_4307954
_publ_section_title
;
Crystal-to-Crystal Oxidative Deprotonation of a Di(\m-hydroxo) to a
Di(\m-oxo) Dimer of Dimolybdenum Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3245
_journal_page_last               3250
_journal_paper_doi               10.1021/ic062443v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         C90H91Mo4N12O14,BF4
_chemical_formula_sum            'C90 H91 B F4 Mo4 N12 O14'
_chemical_formula_weight         2035.32
_chemical_name_common            '[Mo2(DAniF)3]2(OH)(O),BF4'
_chemical_name_systematic
; 
 ? 
;
_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                 109.503(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.683(3)
_cell_length_b                   14.1381(18)
_cell_length_c                   26.693(3)
_cell_measurement_reflns_used    9152
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.790
_cell_measurement_theta_min      2.531
_cell_volume                     8780.6(18)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       \w-scan
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28603
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         1.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.8620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10191
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+19.5515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                7415
_reflns_number_total             10191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062443vsi20070207_040322_10.cif
_cod_data_source_block           xl3
_cod_original_cell_volume        8780.6(19)
_cod_database_code               4307954