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_7049953
_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         'C37 H21 Cl F12 Ge N5, Cl3 Ge'
_chemical_formula_sum            'C37 H21 Cl4 F12 Ge2 N5'
_chemical_formula_weight         1050.57
_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     dual
_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                73.936(3)
_cell_angle_beta                 80.147(3)
_cell_angle_gamma                75.525(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9182(8)
_cell_length_b                   14.4073(13)
_cell_length_c                   16.3208(14)
_cell_measurement_reflns_used    9231
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.183
_cell_measurement_theta_min      3.071
_cell_volume                     1939.4(3)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88406
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.225
_diffrn_reflns_theta_min         2.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0892 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.7356. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10430
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+14.8977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9187
_reflns_number_total             10430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00995g2.cif
_cod_data_source_block           as890_test
_cod_depositor_comments
'Adding full bibliography for 7049950--7049959.cif.'
_cod_database_code               7049953
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F4'-F6' \\sim F4'-F5' \\sim F6'-F5' \\sim F5-F4 \\sim F5-F6 \\sim F4-F6
 with sigma of 0.04
 C35-C25 \\sim C35-F4' \\sim C35-F6' \\sim C35-F5' \\sim C35-F5 \\sim C35-F4
\\sim C35-F6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C35, F4', F6', F5'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, F5, F4, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5)=Sof(F4)=Sof(F6)=1-FVAR(1)
 Sof(F4')=Sof(F6')=Sof(F5')=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C9(H9), C18(H18), C2(H2), C11(H11), C5(H5), C15(H15),
 C4(H4), C16(H16), C26(H26), C29(H29), C22(H22), C3(H3), C31(H31), C33(H33),
 C24(H24)
;
_shelx_res_checksum              12541
_shelx_hkl_checksum              34142
_olex2_submission_special_instructions 'No special instructions were received'