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_7049959
_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
'2(Cl3 Sn), C66 H50 N10 Ni, 0.5(C4 H8 O), C4 H5 O'
_chemical_formula_sum            'C72 H59 Cl6 N10 Ni O1.5 Sn2'
_chemical_formula_weight         1597.08
_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             2019-01-16
_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                82.180(2)
_cell_angle_beta                 76.134(2)
_cell_angle_gamma                63.862(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7350(7)
_cell_length_b                   14.0932(8)
_cell_length_c                   19.9403(12)
_cell_measurement_reflns_used    9076
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      32.138
_cell_measurement_theta_min      2.783
_cell_volume                     3362.1(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            223779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.783
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0696 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.8889. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       prsim
_exptl_crystal_F_000             1606
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.089
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         20496
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+6.5244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16036
_reflns_number_total             20496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00995g2.cif
_cod_data_source_block           as720_p-1_new
_cod_depositor_comments
'Adding full bibliography for 7049950--7049959.cif.'
_cod_original_formula_sum        'C72 H59 Cl6 N10 Ni O1.50 Sn2'
_cod_database_code               7049959
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.808
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1E-C1F \\sim C1F-C1G \\sim C1G-C1H
 with sigma of 0.02
 O1-C1E \\sim O1-C1H
 with sigma of 0.02
 O1-C1F \\sim O1-C1G
 with sigma of 0.04
 C1F-C1H \\sim C1E-C1G
 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O2-C1A \\sim O2-C1D
 with sigma of 0.02
 O2-C1B \\sim O2-C1C
 with sigma of 0.04
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 O2-C1A \\sim O2-C0AA
 with sigma of 0.02
 O2-C1D \\sim O2-C3AA
 with sigma of 0.02
 C1C-C1D \\sim C2AA-C3AA
 with sigma of 0.02
 O2-C1B \\sim O2-C1AA
 with sigma of 0.04
 O2-C1C \\sim O2-C2AA
 with sigma of 0.04
 C1A-C1B \\sim C0AA-C1AA
 with sigma of 0.04
 C1A-C1C \\sim C0AA-C2AA
 with sigma of 0.04
 C1A-C1D \\sim C0AA-C3AA
 with sigma of 0.04
 C1B-C1C \\sim C1AA-C2AA
 with sigma of 0.04
 C1B-C1D \\sim C1AA-C3AA
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C1E, C1F, C1G, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C0AA, C1AA, C2AA, C3AA
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=
 Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=FVAR(1)
 Fixed Sof: O1(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) C1F(0.5) H1FA(0.5) H1FB(0.5)
 C1G(0.5) H1GA(0.5) H1GB(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C60(H60A,H60B), C27(H27A,H27B), C53(H53A,H53B), C1E(H1EA,
 H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB), C1D(H1DA,H1DB),
 C3AA(H3AA,H3AB)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C10(H10), C2(H2), C43(H43), C51(H51), C42(H42), C50(H50),
 C5(H5), C36(H36), C44(H44), C3(H3), C26(H26), C48(H48), C49(H49), C66(H66),
 C18(H18), C22(H22), C35(H35), C38(H38), C33(H33), C62(H62), C59(H59), C37(H37),
  C15(H15), C17(H17), C23(H23), C65(H65), C4(H4), C32(H32), C25(H25), C64(H64),
 C16(H16), C63(H63), C24(H24), C58(H58), C31(H31), C55(H55), C29(H29), C57(H57),
  C30(H30), C56(H56), C1A(H1A), C1B(H1B), C1C(H1C), C0AA(H0AA), C1AA(H1AA),
 C2AA(H2AA)
;
_shelx_res_checksum              23328
_shelx_hkl_checksum              72031
_olex2_submission_special_instructions 'No special instructions were received'