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_4116714
_publ_section_title
;
 Tetranuclear Complexes Containing Quadruply Bonded Dimolybdenum Units
 Joined by \m-Hydride Ions
;
_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_moiety         'C90 H92 Mo4 N12, C6 H14'
_chemical_formula_sum            'C96 H106 Mo4 N12'
_chemical_formula_weight         1811.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 115.97(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.051(3)
_cell_length_b                   17.430(4)
_cell_length_c                   17.284(2)
_cell_measurement_reflns_used    178
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.1
_cell_volume                     4347.3(14)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5.0 (Siemens, 1990)'
_computing_publication_material  'SHELXTL V5.0 (Siemens, 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  0.0738
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       17
_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            16075
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'golden orange'
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5471
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_obs          0.0577
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+29.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1578
_refine_ls_wR_factor_obs         0.1306
_reflns_number_observed          4004
_reflns_number_total             5485
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973947i_1.cif
_cod_data_source_block           cmpd_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+29.0000P] 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^)+(0.0500P)^2^+29.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4347(1)
_cod_database_code               4116714