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_4307951
_publ_section_title
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Crystal-to-Crystal Oxidative Deprotonation of a Di(\m-hydroxo) to a
Di(\m-oxo) Dimer of Dimolybdenum Units
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_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'
_chemical_formula_sum            'C90 H90 Mo4 N12 O14'
_chemical_formula_weight         1947.50
_chemical_name_common            '[Mo2(DAniF)3]2O2'
_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                91.456(3)
_cell_angle_beta                 91.093(3)
_cell_angle_gamma                95.972(3)
_cell_formula_units_Z            2
_cell_length_a                   14.661(3)
_cell_length_b                   17.247(3)
_cell_length_c                   17.539(3)
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.22
_cell_volume                     4408.3(14)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23333
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.9401
_exptl_absorpt_correction_T_min  0.8747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         11405
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+6.5425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2343
_reflns_number_gt                6072
_reflns_number_total             11405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062443vsi20070207_040322_07.cif
_cod_data_source_block           xl1-7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value 'NOREF' changed to 'noref' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4307951