Syntheses, structures and properties of [{HC(CMeNAr)2}Ge(E)X] (Ar = 2,6-iPr2C6H3; E = S, Se; X = F, Cl)
Ding, Yuqiang; Ma, Qingjun; Roesky, Herbert W.; Usón, Isabel; Noltemeyer, Mathias; Schmidt, Hans-Georg; Dalton Transactions  (2003) 1094–; doi:10.1039/b211617k

data_7012525
_publ_section_title
;
 Syntheses, structures and properties of [{HC(CMeNAr)2}Ge(E)X] (Ar =
 2,6-iPr2C6H3; E = S, Se; X = F, Cl)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1094
_journal_paper_doi               10.1039/b211617k
_journal_year                    2003
_chemical_formula_sum            'C35 H54 Cl0 Ge N2 Se'
_chemical_formula_weight         654.35
_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                 99.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.714(3)
_cell_length_b                   10.213(2)
_cell_length_c                   18.801(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3169.8(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5791
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '90 min'
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  0.4814
_exptl_absorpt_correction_T_min  0.2234
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.575
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5569
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0600P)^2^+3.0300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                4844
_reflns_number_total             5569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211617k.txt
_cod_data_source_block           r1015x
_cod_original_cell_volume        3170.1(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012525