Synthesis and Structures of [{HC(CMeNAr)2}Ge(S)X] (Ar = 2,6-iPr2C6H3, X = F, Cl, Me): Structurally Characterized Examples with a Formal Double Bond between Group 14 and 16 Elements Bearing a Halide
Yuqiang Ding; Qingjun Ma; Isabel Usón; Herbert W. Roesky; Mathias Noltemeyer; Hans-Georg Schmidt; Journal of the American Chemical Society 124 (2002) 8542–8543; doi:10.1021/ja017645z

data_4114957
_publ_section_title
;
 Synthesis and Structures of [{HC(CMeNAr)2}Ge(S)X] (Ar = 2,6-iPr2C6H3, X =
 F, Cl, Me): Structurally Characterized Examples with a Formal Double Bond
 between Group 14 and 16 Elements Bearing a Halide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8542
_journal_page_last               8543
_journal_paper_doi               10.1021/ja017645z
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C29 H41 Cl Ge N2 S'
_chemical_formula_weight         557.74
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.880(3)
_cell_length_b                   13.044(3)
_cell_length_c                   13.801(3)
_cell_measurement_reflns_used    1013
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      55.283
_cell_measurement_theta_min      5.931
_cell_volume                     2880.5(12)
_computing_cell_refinement       'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_data_collection       'Siemens SMART (V.5.050, Siemens 1998)'
_computing_data_reduction        'Bruker AXS SAINT (V.5.00, Madison 1997)'
_computing_molecular_graphics    'Bruker AXS Shelxtl (Madison 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'STOE-Siemens-Huber four circle diffractometer'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42179
_diffrn_reflns_theta_full        27.82
_diffrn_reflns_theta_max         27.82
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25mm
_exptl_crystal_size_mid          0.13mm
_exptl_crystal_size_min          0.13mm
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6747
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.7290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                6090
_reflns_number_total             6747
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017645z_s1_2.cif
_cod_data_source_block           pub
_cod_original_cell_volume        2880.5(10)
_cod_original_formula_sum        'H41 C29 N2 S Cl Ge'
_cod_database_code               4114957