Syntheses, Crystal Structures, and Density Functional Theory Calculations of the closo-[1-M(CO)3(η4-E9)]4- (E = Sn, Pb; M = Mo, W) Cluster Anions and Solution NMR Spectroscopic Characterization of [1-M(CO)3(η4-Sn9)]4- (M = Cr, Mo, W)
Janette Campbell; Hélène P. A. Mercier; Holger Franke; David P. Santry; David A. Dixon; Gary J. Schrobilgen; Inorganic Chemistry 41 (2002) 86–107; doi:10.1021/ic010695k

data_4317396
_publ_section_title
;
 Syntheses, Crystal Structures, and Density Functional Theory Calculations
 of the closo-[1-M(CO)3(\h4-E9)]4- (E = Sn, Pb; M = Mo, W) Cluster Anions
 and Solution NMR Spectroscopic Characterization of [1-M(CO)3(\h4-Sn9)]4-
 (M = Cr, Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              86
_journal_page_last               107
_journal_paper_doi               10.1021/ic010695k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C87 H180 K4 Mo2 N17 O30 Pb9'
_chemical_formula_weight         4157.47
_chemical_name_systematic
;
  ?
;
_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                71.82(3)
_cell_angle_beta                 83.01(3)
_cell_angle_gamma                81.73(3)
_cell_formula_units_Z            2
_cell_length_a                   16.319(3)
_cell_length_b                   17.078(3)
_cell_length_c                   24.827(5)
_cell_measurement_temperature    140(2)
_cell_volume                     6484(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_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  0.1415
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            86717
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    12.022
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_F_000             3918
_refine_diff_density_max         5.444
_refine_diff_density_min         -4.394
_refine_diff_density_rms         0.391
_refine_ls_extinction_coef       0.00032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         31538
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_obs          0.0700
_refine_ls_shift/esd_max         0.775
_refine_ls_shift/esd_mean        0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+39.2163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1967
_refine_ls_wR_factor_obs         0.1781
_reflns_number_observed          24428
_reflns_number_total             31613
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010695k_4.cif
_cod_data_source_block           Pb9Mo(CO)34-
_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^)+(0.1030P)^2^+39.2163P] 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^)+(0.1030P)^2^+39.2163P] 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        6483.7(21)
_cod_database_code               4317396