Crystal structure of (pyridine-2-carboxamide-κ2 N,O)-[tris((1H-benzo[d]imidazol-2-yl)methyl)amine-κ4 N,N′,N′′,N′′′]nickel(II) diperchlorate — methanol (1/3), C33H39Cl2N9NiO12
Zhang, Jun-Chao; Chen, Jiang-Li; Nie, Feng-Mei; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 607–609; doi:10.1515/ncrs-2019-0847

data_8105234
_publ_section_title
;
 Crystal structure of (pyridine-2-carboxamide-\k2
 N,O)-[tris((1H-benzo[d]imidazol-2-yl)methyl)amine-\k4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;]nickel(II)
 diperchlorate --- methanol (1/3), C33H39Cl2N9NiO12
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              607
_journal_page_last               609
_journal_paper_doi               10.1515/ncrs-2019-0847
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C30 H27 N9 Ni O, 2(Cl O4), 3(C H4 O)'
_chemical_formula_sum            'C33 H39 Cl2 N9 Ni O12'
_chemical_formula_weight         883.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.767(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7478(4)
_cell_length_b                   20.6247(7)
_cell_length_c                   19.0897(11)
_cell_measurement_reflns_used    5406
_cell_measurement_temperature    108.4(2)
_cell_measurement_theta_max      25.3920
_cell_measurement_theta_min      3.6170
_cell_volume                     3833.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      108.4(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -36.00    6.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.1085  -37.0000  -30.0000 42

  2 omega   27.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4210  -99.0000 -120.0000 26

  3 omega  -39.00    8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4210  -19.0000 -150.0000 47

  4 omega    0.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4210   37.0000 -150.0000 81

  5 omega   42.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4210   57.0000  -60.0000 43

  6 omega  -23.00    4.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.1085   57.0000 -150.0000 27

  7 omega  -40.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.1085   77.0000    0.0000 66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24869
_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         26.000
_diffrn_reflns_theta_min         2.910
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0322P)^2^+3.5203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5606
_reflns_number_total             7508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0847_suppl.cif
_cod_data_source_block           exp_5916
_cod_database_code               8105234
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H12)=Sof(C33')=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(H12A)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9C,H9D), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), N7(H7), C5(H5A), C6(H6), C7(H7A), C8(H8), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28)
3.c Tetrahedral OH refined with riding coordinates:
 O12(H12A), O12(H12)
3.d X=CH2 refined with riding coordinates:
 N9(H9A,H9B)
3.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C33'(H33D,H33E,
 H33F)
3.f Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'