The reaction of [Os3(μ-H)(CO)10(μ-CO)]− with Ph2SbCl: a cluster with a six-membered Os4Sb2 ring and another with fluxional metal–metal bonds †
Leong, Weng Kee; Chen, Guizhu; Journal of the Chemical Society, Dalton Transactions  (2000) 4442–; doi:10.1039/b006669i

data_7010179
_publ_section_title
;
 The reaction of [Os3(\m-H)(CO)10(\m-CO)]&#x2212; with Ph2SbCl: a
 cluster with a six-membered Os4Sb2 ring and another with fluxional
 metal--metal bonds&#x200A;&#x2020;
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4442
_journal_paper_doi               10.1039/b006669i
_journal_year                    2000
_chemical_formula_sum            'C53 H43 O20 Os6 Sb2'
_chemical_formula_weight         2384.57
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 101.5870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8356(4)
_cell_length_b                   11.8116(3)
_cell_length_c                   19.4734(4)
_cell_measurement_reflns_used    5792
_cell_measurement_temperature    293(2)
_cell_volume                     3342.83(14)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19021
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    12.213
_exptl_absorpt_correction_T_max  0.262266
_exptl_absorpt_correction_T_min  0.155817
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_meas      ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2158
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.189
_refine_ls_goodness_of_fit_obs   1.164
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     8
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_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_obs          0.0323
_refine_ls_shift/esd_max         0.367
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+7.0127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0808
_refine_ls_wR_factor_obs         0.0704
_reflns_number_observed          5717
_reflns_number_total             7128
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006669i.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured ' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+7.0127P] 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^)+(0.0274P)^2^+7.0127P] 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        3342.82(14)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7010179