Reversible methyl group migration between osmium and tin in reactions of osmium trimethylstannyl complexes
Rickard, Clifton E. F.; Roper, Warren R.; Woodman, Timothy J.; James Wright, L.; Chemical Communications  (1999) 1101–; doi:10.1039/a902938i

data_7110557
_publ_section_title
;
 Reversible methyl group migration between osmium and tin in reactions of
 osmium trimethylstannyl complexes
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1101
_journal_paper_doi               10.1039/a902938i
_journal_year                    1999
_chemical_formula_moiety         'C45 H44 Cl N O Os P2 Sn, (C H2 Cl2)'
_chemical_formula_sum            'C46 H46 Cl3 N O Os P2 Sn'
_chemical_formula_weight         1106.02
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.708(1)
_cell_angle_beta                 97.968(1)
_cell_angle_gamma                107.02(1)
_cell_formula_units_Z            2
_cell_length_a                   9.6249(1)
_cell_length_b                   12.5510(2)
_cell_length_c                   19.6568(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.06
_cell_volume                     2217.39(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       multi-scan
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21704
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_T_max  0.4021
_exptl_absorpt_correction_T_min  0.3564
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.285
_refine_diff_density_min         -3.515
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         9612
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+12.6327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                9304
_reflns_number_total             9612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902938isup1.cif
_cod_data_source_block           (2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+12.6327P] 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^)+(0.0381P)^2^+12.6327P] 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        2217.36(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110557