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_4114958
_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            'C36 H49 F Ge N2 S'
_chemical_formula_weight         633.42
_chemical_name_systematic        ?
_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                 92.783(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.467(2)
_cell_length_b                   16.804(3)
_cell_length_c                   15.668(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3541.5(11)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9893
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.7015
_exptl_absorpt_correction_T_min  0.4488
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0800P)^2^+2.2444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                5424
_reflns_number_total             6266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017645z_s1_3.cif
_cod_data_source_block           r1000
_cod_original_formula_sum        'C36 H49 F Ge N2 S incl. toluene'
_cod_database_code               4114958
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C36 H49 F Ge N2 S cl e en in lu to' to 'C36 H49 F Ge N2 S'.

 Antanas Vaitkus,
 2017-01-04
;