Crystal structure of {tris((1H-benzo[d]imidazol-2-yl)methyl)amine-κ4 N,N′,N′′,N′′′}-(nitrito-κ2 O,O′)nickel(II) perchlorate – ethanol (1/1), C26H27ClN8NiO7
Li, Xin-Lun; Luo, Zhong-Ping; Zhang, Jun-Chao; Nie, Feng-Mei; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 767–769; doi:10.1515/ncrs-2019-0862

data_8105282
_publ_section_title
;
 Crystal structure of {tris((1H-benzo[d]imidazol-2-yl)methyl)amine-\k4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;}-(nitrito-\k2
 O,O&#x2032;)nickel(II) perchlorate -- ethanol (1/1), C26H27ClN8NiO7
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              767
_journal_page_last               769
_journal_paper_doi               10.1515/ncrs-2019-0862
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H21 N8 Ni O2, Cl O4, C2 H6 O'
_chemical_formula_sum            'C26 H27 Cl N8 Ni O7'
_chemical_formula_weight         657.71
_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     iterative
_cell_angle_alpha                78.77(3)
_cell_angle_beta                 70.52(3)
_cell_angle_gamma                83.40(3)
_cell_formula_units_Z            2
_cell_length_a                   9.893(2)
_cell_length_b                   11.503(2)
_cell_length_c                   13.295(3)
_cell_measurement_reflns_used    4659
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.2335
_cell_volume                     1397.0(6)
_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      153.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16933
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.761
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0414P)^2^+1.1833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6056
_reflns_number_total             6358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0862_suppl.cif
_cod_data_source_block           bww19113
_cod_database_code               8105282
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.828
_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 O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O7(H)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C25(HA,HB)
2.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), N7(H7), C2(H2), C3(H3A), C4(H4), C5(H5A), C12(H12), C13(H13),
 C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23)
2.d Idealised Me refined as rotating group:
 C26(HC,HD,HE)
;