Insertion of SO2 into a Sulfide-Bridged M-Ge Bond: Synthesis, Characterization, and Reactivity of the O-Germyl-S-sulfoxylate
Zuzanna T. Cygan; Jeff W. Kampf; Mark M. Banaszak Holl; Inorganic Chemistry 43 (2004) 2057–2063; doi:10.1021/ic0353155

data_4310746
_publ_section_title
;
 Insertion of SO2 into a Sulfide-Bridged M-Ge Bond: Synthesis,
 Characterization, and Reactivity of the O-Germyl-S-sulfoxylate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2057
_journal_page_last               2063
_journal_paper_doi               10.1021/ic0353155
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24 H66 Ge N2 O2 P2 Pd S2 Si4'
_chemical_formula_weight         832.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.026(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.8961(13)
_cell_length_b                   38.098(5)
_cell_length_c                   21.789(3)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.98
_cell_volume                     8134.5(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76431
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00079(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         16655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0286P)^2^+25.5318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                11279
_reflns_number_total             16655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0353155si20031113_034100_1.cif
_cod_data_source_block           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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4310746