Tetranuclear Complexes Containing Quadruply Bonded Dimolybdenum Units Joined by μ-Hydride Ions
F. Albert Cotton; Lee M. Daniels; Glenn T. Jordan; Chun Lin; Carlos A. Murillo; Journal of the American Chemical Society 120 (1998) 3398–3401; doi:10.1021/ja973947i

data_4116715
_publ_section_title
;
 Tetranuclear Complexes Containing Quadruply Bonded Dimolybdenum Units
 Joined by \m-Hydride Ions
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3398
_journal_page_last               3401
_journal_paper_doi               10.1021/ja973947i
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_sum            'C96 H106 Mo4 N12 O12'
_chemical_formula_weight         2003.69
_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
_cell_angle_alpha                110.28(1)
_cell_angle_beta                 94.90(1)
_cell_angle_gamma                108.55(1)
_cell_formula_units_Z            1
_cell_length_a                   13.487(2)
_cell_length_b                   13.665(2)
_cell_length_c                   14.354(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     2294.9(6)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5 (Sheldrick, 1990)'
_computing_publication_material  'SHELXTL V5 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14679
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   'empirical (Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.118
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7603
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.113
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+6.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1141
_refine_ls_wR_factor_obs         0.1061
_reflns_number_observed          6806
_reflns_number_total             7613
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973947i_2.cif
_cod_data_source_block           cmpd_2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+6.6000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+6.6000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116715