New Metal−Organic Polygons Involving MM Quadruple Bonds: M8(O2CtBu)4(μ-SC4H2-3,4-{CO2}2)6(M = Mo, W)
Byrnes, Matthew J.; Chisholm, Malcolm H.; Patmore, Nathan J.; Inorganic Chemistry 44 (2005) 9347–9352; doi:10.1021/ic051516s

data_4331765
_publ_section_title
;
 New Metal&#x2212;Organic Polygons Involving MM Quadruple Bonds:&#x00A0;
 M8(O2CtBu)4(\m-SC4H2-3,4-{CO2}2)6(M = Mo, W)
;
_journal_issue                   25
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9347
_journal_page_last               9352
_journal_paper_doi               10.1021/ic051516s
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C56 H48 Mo8 O32 S6'
_chemical_formula_sum            'C56 H48 Mo8 O32 S6'
_chemical_formula_weight         2192.82
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.315(2)
_cell_length_b                   15.315(2)
_cell_length_c                   39.624(7)
_cell_measurement_temperature    150(2)
_cell_volume                     9294(2)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'XCAD (P.McArdle, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Phi and Omega 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  0.046
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            43988
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Irregular block'
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5336
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+1.3572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                3930
_reflns_number_total             5336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051516ssup1.cif
_cod_data_source_block           Mo8(O2CtBu)4(SC4H2-3,4-(CO2)2)6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4331765