The crystal structure of aqua{N,N,N′,N′-tetrakis[(1H-benzimidazol-κN 3) methyl]cyclohexane-1,2-diamine}lead(II) diacetate–methanol (1/2), C44H54N10O7Pb
Li, Ji; Miao, Ming-Zhi; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1417–1420; doi:10.1515/ncrs-2020-0343

data_8105482
_publ_section_title
;
 The crystal structure of
 aqua{N,N,N&#x2032;,N&#x2032;-tetrakis[(1H-benzimidazol-\kN 3)
 methyl]cyclohexane-1,2-diamine}lead(II) diacetate--methanol (1/2),
 C44H54N10O7Pb
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1417
_journal_page_last               1420
_journal_paper_doi               10.1515/ncrs-2020-0343
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C38 H40 N10 O Pb, 2(C2 H3 O2), 2(C H4 O)'
_chemical_formula_sum            'C44 H54 N10 O7 Pb'
_chemical_formula_weight         1042.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                101.163(2)
_cell_angle_beta                 110.634(2)
_cell_angle_gamma                100.698(2)
_cell_formula_units_Z            2
_cell_length_a                   12.096(2)
_cell_length_b                   12.9160(2)
_cell_length_c                   16.5904(7)
_cell_measurement_reflns_used    3344
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.90
_cell_measurement_theta_min      2.38
_cell_volume                     2287.0(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2003) [1]'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2003)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2006)[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[5]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [2-3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2015) [2-3]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7966
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.820
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.748
_exptl_absorpt_correction_T_max  0.7056
_exptl_absorpt_correction_T_min  0.5854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick, 2008)[6]'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.813
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0689P)^2^+0.0406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1409
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7079
_reflns_number_total             7966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0343_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105482
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.585
_exptl_absorpt_special_details   'SADABS, (Sheldrick, 2008)[6]'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.748(4)
 0.252(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Restrained distances
 C43-O6 = C44-O7
 1.42 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C44) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Riding coordinates:
 O1(H1A,H1B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C6(H6)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C15(H15A,
 H15B), C23(H23A,H23B), C31(H31A,H31B)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20),
 C21(H21), C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
  C37(H37), N4(H4), N6(H6A), N8(H8), N10(H10A)
5.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
5.f Idealised tetrahedral OH refined as rotating group:
 O6(H6B), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'