Crystal structure of diaqua[bis(benzimidazol-2-yl-methyl)amine-κ3 N,N′,N″]-phthalato-κ1 O-nickel(II)-methanol (1/2), C26H31N5NiO8
Chen, Yu-Xiao; Luo, Zhong-Ping; Zhang, He; Nie, Feng-Mei; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 373–375; doi:10.1515/ncrs-2020-0502

data_8104835
_publ_section_title
;
 Crystal structure of diaqua[bis(benzimidazol-2-yl-methyl)amine-\k3
 N,N&#x2032;,N&#x2033;]-phthalato-\k1 O-nickel(II)-methanol (1/2),
 C26H31N5NiO8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              373
_journal_page_last               375
_journal_paper_doi               10.1515/ncrs-2020-0502
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C24 H23 N5 Ni O6, 2(C H4 O)'
_chemical_formula_sum            'C26 H31 N5 Ni O8'
_chemical_formula_weight         600.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 107.844(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.554(3)
_cell_length_b                   12.401(3)
_cell_length_c                   18.718(5)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.124
_cell_measurement_theta_min      2.001
_cell_volume                     2773.9(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  AFC10/Saturn724+
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30130
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.815
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0638P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5655
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0502_suppl.cif
_cod_data_source_block           bo1575
_cod_original_cell_volume        2774.0(12)
_cod_database_code               8104835
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.824
_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) groups, All N(H) groups,
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H5A-H5B = H6A-H6B
 1.38 with sigma of 0.01
 O5-H5A = O5-H5B = O6-H6A = O6-H6B
 0.84 with sigma of 0.01
3.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A), O8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C4(H4), C5(H5C), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
  C15(H15), C19(H19), C20(H20), C21(H21), C22(H22)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;