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_4307945
_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         'C90 H90 Mo4 N12 O14, 1.5(CH2Cl2)'
_chemical_formula_sum            'C91.5 H93 Cl3 Mo4 N12 O14'
_chemical_formula_weight         2074.89
_chemical_name_common            '[Mo2(DAniF)3]2(OH)2,1.5CH2Cl2'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.055(2)
_cell_angle_beta                 88.116(2)
_cell_angle_gamma                93.027(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8348(17)
_cell_length_b                   17.3985(19)
_cell_length_c                   17.809(2)
_cell_measurement_reflns_used    16810
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.530
_cell_measurement_theta_min      2.177
_cell_volume                     4585.0(9)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28833
_diffrn_reflns_theta_full        25.55
_diffrn_reflns_theta_max         25.55
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.8629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2114
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         16810
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0799P)^2^+9.6785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                12573
_reflns_number_total             16810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062443vsi20070207_040322_01.cif
_cod_data_source_block           xl1-1.5CH2Cl2-1
_cod_original_cell_volume        4585.1(9)
_cod_original_formula_sum        'C91.50 H93 Cl3 Mo4 N12 O14'
_cod_database_code               4307945