Reaction of Os3(CO)9(μ3-η2-C7H3(2-CH3)NS)(μ-H) with Diazomethane. The First Example of a Trimetallic Cluster Containing a μ-Methylidene and a σ-Methyl
Kabir, Shariff E.; Malik, K. M. Abdul; Mandal, Himadri S.; Mottalib, Md. Abdul; Abedin, Md. Joynal; Rosenberg, Edward; Organometallics 21 (2002) 2593–; doi:10.1021/om020174k

data_4076877
_publ_section_title
;
 Reaction of Os3(CO)9(\m3-\h2-C7H3(2-CH3)NS)(\m-H) with Diazomethane. The
 First Example of a Trimetallic Cluster Containing a \m-Methylidene and a
 \s-Methyl
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2593
_journal_paper_doi               10.1021/om020174k
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C19 H11 N O9 Os3 S'
_chemical_formula_weight         999.95
_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-96
_cell_angle_alpha                97.974(3)
_cell_angle_beta                 105.797(3)
_cell_angle_gamma                112.489(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2852(4)
_cell_length_b                   10.3219(4)
_cell_length_c                   13.4911(5)
_cell_measurement_reflns_used    'Entire data set'
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.63
_cell_volume                     1105.83(8)
_computing_cell_refinement       'COLLECT (Bruker Nonius, 1998)'
_computing_data_collection       'COLLECT (Bruker Nonius, 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Bruker Nonius kappa CCD area detector'
_diffrn_measurement_method       'COLLECT (Bruker Nonius, 1998)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16260
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    17.339
_exptl_absorpt_correction_T_max  0.135
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.003
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.514
_refine_diff_density_min         -3.247
_refine_diff_density_rms         0.344
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    'Calculated positions, riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0991
_refine_ls_wR_factor_obs         0.0931
_reflns_number_observed          4178
_reflns_number_total             5053
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om020174k.cif
_cod_data_source_block           C19H11N1O9Os3S1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] 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^)+(0.0513P)^2^+0.0000P] 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        1105.82(8)
_cod_original_sg_symbol_H-M      'P-1 (No. 2)'
_cod_database_code               4076877