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_7110558
_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         'C42 H42 O3 Os P2 Sn, (C H2 Cl2)'
_chemical_formula_sum            'C43 H44 Cl2 O3 Os P2 Sn'
_chemical_formula_weight         1050.51
_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-97
_cell_angle_alpha                95.559(1)
_cell_angle_beta                 101.214(1)
_cell_angle_gamma                103.598(1)
_cell_formula_units_Z            2
_cell_length_a                   9.8497(1)
_cell_length_b                   11.9753(2)
_cell_length_c                   18.5656(3)
_cell_measurement_reflns_used    6181
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.13
_cell_volume                     2064.37(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19303
_diffrn_reflns_theta_full        27.40
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    3.924
_exptl_absorpt_correction_T_max  0.8279
_exptl_absorpt_correction_T_min  0.2395
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8834
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.148
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.5675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                7401
_reflns_number_total             8834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902938isup1.cif
_cod_data_source_block           (3)
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.5675P] 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^)+(0.0000P)^2^+8.5675P] 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        2064.36(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110558