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_4076878
_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            'C17 H9 N O8 Os3 S'
_chemical_formula_weight         957.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-96
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6916(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1881(4)
_cell_length_b                   11.2807(4)
_cell_length_c                   11.8325(4)
_cell_measurement_reflns_used    'entire data set'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.21
_cell_volume                     2123.26(12)
_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      293(2)
_diffrn_measurement_device       'Bruker Nonius Kappa CCD area detector'
_diffrn_measurement_method
'COLLECT data collection software (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  0.1053
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23716
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    18.050
_exptl_absorpt_correction_T_max  0.371
_exptl_absorpt_correction_T_min  0.136
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.997
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.879
_refine_diff_density_min         -3.554
_refine_diff_density_rms         0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.994
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment
'The three bridging hydride s were located from difference calculated positions, but not refined. Other hydrogens were included in calculated positions, riding model''
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_obs         0.0980
_reflns_number_observed          3486
_reflns_number_total             4842
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om020174k.cif
_cod_data_source_block           compoud_C17H9N1O8OS3S1
_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_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^)+(0.0563P)^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^)+(0.0563P)^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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4076878