2,6-Bis(benzimidazol-2-yl)pyridine complexes of group 14 elements.
Swidan, Ala'aeddeen; St Onge, P Blake J; Binder, Justin F.; Suter, Riccardo; Burford, Neil; Macdonald, Charles L. B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7835–7843; doi:10.1039/c9dt00995g

data_7049950
_publ_section_title
;
 2,6-Bis(benzimidazol-2-yl)pyridine complexes of group 14 elements.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7835
_journal_page_last               7843
_journal_paper_doi               10.1039/c9dt00995g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '4(C33 H25 Cl Ge N5), 4(Cl3 Ge), C H2 Cl2'
_chemical_formula_sum            'C133 H102 Cl18 Ge8 N20'
_chemical_formula_weight         3199.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-04 deposited with the CCDC.    2019-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                86.094(2)
_cell_angle_beta                 74.051(2)
_cell_angle_gamma                76.567(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1393(9)
_cell_length_b                   15.1768(9)
_cell_length_c                   16.3072(11)
_cell_measurement_reflns_used    9114
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.390
_cell_measurement_theta_min      2.937
_cell_volume                     3272.6(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            224637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.593
_diffrn_reflns_theta_min         2.936
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.238
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0750 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8520. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       prism
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.135
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         20073
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+3.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15518
_reflns_number_total             20073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00995g2.cif
_cod_data_source_block           as660_p-1
_cod_depositor_comments
'Adding full bibliography for 7049950--7049959.cif.'
_cod_database_code               7049950
_shelx_shelxl_version_number     2016/6
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl9-C67 = Cl10-C67
 1.771 with sigma of 0.01
 Cl9-Cl10
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl9 \\sim Cl10 \\sim C67: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl9, Cl10, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl9(0.5) Cl10(0.5) C67(0.5) H67A(0.5) H67B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C20(H20A,H20B), C27(H27A,H27B), C60(H60A,H60B), C67(H67A,H67B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C38(H38), C4(H4), C5(H5), C35(H35), C36(H36), C42(H42),
 C43(H43), C44(H44), C59(H59), C9(H9), C11(H11), C48(H48), C15(H15), C37(H37),
 C51(H51), C50(H50), C49(H49), C66(H66), C58(H58), C55(H55), C57(H57), C26(H26),
  C22(H22), C56(H56), C16(H16), C62(H62), C18(H18), C17(H17), C65(H65),
 C64(H64), C63(H63), C29(H29), C33(H33), C24(H24), C25(H25), C23(H23), C10(H10),
  C32(H32), C30(H30), C31(H31)
;
_shelx_res_checksum              58943
_shelx_hkl_checksum              84569
_olex2_submission_special_instructions 'No special instructions were received'