Crystal structure of {tris((1H-benzo[d]imidazol-2- yl)methyl)amine-κ 4 N,N′,N′′,N′′′}-(succinato-κ 2 O,O′)nickel(II) – methanol (1/4), C32H41N7NiO8
Qiao, Tian-Xu; Chen, Yu-Xiao; An, Jing-Yi; Nie, Feng-Mei; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 459–461; doi:10.1515/ncrs-2020-0608

data_8104859
_publ_section_title
;
 Crystal structure of {tris((1H-benzo[d]imidazol-2- yl)methyl)amine-\k 4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;}-(succinato-\k 2
 O,O&#x2032;)nickel(II) -- methanol (1/4), C32H41N7NiO8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              459
_journal_page_last               461
_journal_paper_doi               10.1515/ncrs-2020-0608
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C28 H25 N7 Ni O4, 4(C H4 O)'
_chemical_formula_sum            'C32 H41 N7 Ni O8'
_chemical_formula_weight         710.43
_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
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 108.532(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0076(5)
_cell_length_b                   18.6516(10)
_cell_length_c                   19.0893(18)
_cell_measurement_reflns_used    3018
_cell_measurement_temperature    111.90(10)
_cell_measurement_theta_max      25.8850
_cell_measurement_theta_min      3.5470
_cell_volume                     3378.4(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111.90(10)
_diffrn_detector                 'CCD plate'
_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  -28.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2647   77.0000   30.0000 71

  2 omega   23.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   77.0000  120.0000 60

  3 omega   42.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   77.0000  -90.0000 41

  4 omega    0.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5772   77.0000 -120.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0571413000
_diffrn_orient_matrix_UB_12      -0.0231086000
_diffrn_orient_matrix_UB_13      -0.0107660000
_diffrn_orient_matrix_UB_21      0.0326078000
_diffrn_orient_matrix_UB_22      -0.0168715000
_diffrn_orient_matrix_UB_23      -0.0259376000
_diffrn_orient_matrix_UB_31      0.0305740000
_diffrn_orient_matrix_UB_32      -0.0251145000
_diffrn_orient_matrix_UB_33      0.0272849000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0778
_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       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16175
_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         2.933
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95145
_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_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0364P)^2^+4.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4640
_reflns_number_total             6632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0608_suppl.cif
_cod_data_source_block           exp_6649
_cod_database_code               8104859
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.813
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(C28) = Uanis(C28')
Uanis(C27) = Uanis(C27')
3. Others
 Sof(C28')=Sof(H28C)=Sof(H28D)=Sof(C27')=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B), C17(H17A,H17B), C27(H27A,H27B), C28(H28A,H28B),
 C28'(H28C,H28D), C27'(H27C,H27D)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C8(H8), N7(H7), C21(H21), C16(H16), C5(H5A), C15(H15),
 C23(H23), C24(H24), C22(H22), C14(H14), C7(H7A), C13(H13), C6(H6)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C30(H30A,H30B,
 H30C)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5B), O7(H7B), O8(H8A), O6(H6A)
;