Reaction of Trihydridostannyl Complexes with SO2: Preparation of [Re2{Sn2(μ-S)(μ-SO3)2}(CO)4L2{PPh(OEt)2}4] (L = PPh(OEt)2, (CH3)3CNC)
Albertin, Gabriele; Antoniutti, Stefano; Castro, Jesús; Zanardo, Gianluigi; Organometallics 28 (2009) 1270–; doi:10.1021/om801013s

data_4068658
_publ_section_title
;
 Reaction of Trihydridostannyl Complexes with SO2: Preparation of
 [Re2{Sn2(\m-S)(\m-SO3)2}(CO)4L2{PPh(OEt)2}4] (L = PPh(OEt)2, (CH3)3CNC)
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1270
_journal_paper_doi               10.1021/om801013s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C54 H78 N2 O18 P4 Re2 S3 Sn2'
_chemical_formula_weight         1873.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.489(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.347(7)
_cell_length_b                   16.615(7)
_cell_length_c                   31.222(14)
_cell_measurement_reflns_used    5089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.28
_cell_volume                     7947(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            25074
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    3.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
A. L. Spek, Acta Crystallogr. 1990, A46, C34
;
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                5643
_reflns_number_total             9289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801013s_si_001.cif
_cod_data_source_block           GN470_2
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7946(6)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4068658