Crystal structure of dichloro-bis-(1-butyl-1H-benzo[d]imidazole)-nickel(II), C22H28Cl2N4Ni
Li, Zhuang-yu; Liu, Xiao-jing; Liu, E.; Jian, Fang-fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 911–912; doi:10.1515/ncrs-2020-0098

data_8105328
_publ_section_title
;
 Crystal structure of
 dichloro-bis-(1-butyl-1H-benzo[d]imidazole)-nickel(II), C22H28Cl2N4Ni
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              911
_journal_page_last               912
_journal_paper_doi               10.1515/ncrs-2020-0098
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C22 H28 Cl2 N4 Ni'
_chemical_formula_sum            'C22 H28 Cl2 N4 Ni'
_chemical_formula_weight         478.09
_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'
_symmetry_Int_Tables_number      14
_cell_angle_alpha                90
_cell_angle_beta                 117.45(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7332(19)
_cell_length_b                   14.886(3)
_cell_length_c                   18.623(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      14
_cell_measurement_theta_min      4
_cell_volume                     2394.5(10)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRCVAX (Gabe et al., 1989)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23163
_diffrn_reflns_theta_full        27.4796
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.9157
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.3261
_exptl_crystal_description       block
_exptl_crystal_F_000             1002.8357
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.8005
_refine_diff_density_min         -0.4722
_refine_diff_density_rms         0.0762
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             6.7865
_refine_ls_goodness_of_fit_ref   0.9802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      0.9637
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3720
_reflns_number_total             5478
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2020-0098_suppl.cif
_cod_data_source_block           QJ0984
_cod_database_code               8105328
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C2A = C3-C2 = C2A-C1A = C2-C1
 1.54 with sigma of 0.01
 C13A-C12A
 1.54 with sigma of 0.01
 C14A-C13A = C14-C13 = C15-C14A = C15-C14 = C13-C12
 1.54 with sigma of 0.01
 C14-C12
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C12A \\sim C13 \\sim C13A
\\sim C14 \\sim C14A \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim
C20 \\sim C21 \\sim C22: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Ni1 \\sim N1 \\sim N3: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C13A)=Sof(H13c)=Sof(H13d)=Sof(C14A)=Sof(H14c)=Sof(H14d)=Sof(H15c)=
 Sof(H15d)=1-FVAR(1)
 Sof(C13)=Sof(H13a)=Sof(H13b)=Sof(C14)=Sof(H14a)=Sof(H14b)=Sof(H15a)=Sof(H15b)=
 FVAR(1)
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=Sof(H3bc)=
 Sof(H3bd)=1-FVAR(2)
 Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(H1c)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(H3aa)=
 Sof(H3ab)=FVAR(2)
 Sof(C12A)=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(3)
 Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(H12c)=FVAR(3)
5.a Riding coordinates:
 C12(H12a,H12b,H12c)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C2A(H2Aa,H2Ab), C3(H3aa,H3ab), C3(H3bc,H3bd), C4(H4a,H4b),
 C13(H13a,H13b), C13A(H13c,H13d), C14(H14a,H14b), C14A(H14c,H14d), C15(H15a,
 H15b), C15(H15c,H15d)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C1A(H1Aa,H1Ab,H1Ac), C12A(H12d,H12e,H12f)
;
_olex2_submission_special_instructions 'No special instructions were received'