Crystal structure of bis(benzene-1 carboxylato-O 3,5-carboxyl-κ 1O)-[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ 4 N,N′,N′′,N′′′)nickel(II) ─ benzene-1,3,5-tricarboxylic acid ─ water (1/2/4), C52H66N4NiO28
Chen, Xiao-Ming; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1189–1191; doi:10.1515/ncrs-2023-0389

data_8107698
_publ_section_title
;
 Crystal structure of bis(benzene-1 carboxylato-O 3,5-carboxyl-\k
 1O)-[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k 4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;)nickel(II)
 &#x2500; benzene-1,3,5-tricarboxylic acid &#x2500; water (1/2/4),
 C52H66N4NiO28
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1189
_journal_page_last               1191
_journal_paper_doi               10.1515/ncrs-2023-0389
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C34 H46 N4 Ni O12, 4(H2 O), 2(C9 H6 O6)'
_chemical_formula_sum            'C52 H66 N4 Ni O28'
_chemical_formula_weight         1253.79
_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                81.872(6)
_cell_angle_beta                 67.036(5)
_cell_angle_gamma                75.624(6)
_cell_formula_units_Z            1
_cell_length_a                   11.292(6)
_cell_length_b                   11.670(6)
_cell_length_c                   12.165(6)
_cell_measurement_reflns_used    4686
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.15
_cell_volume                     1428.0(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.367
_diffrn_reflns_theta_min         1.804
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_correction_T_min  0.8287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.92
_exptl_transmission_factor_min   0.83
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6262
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5008
_reflns_number_total             6262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0389_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        1428.1(12)
_cod_database_code               8107698
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.829
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H1WA-H1WB = H2WB-H2WA
 1.39 with sigma of 0.01
 O1W-H1WA = O1W-H1WB = O2W-H2WB = O2W-H2WA
 0.86 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C21(H21), N1(H1), N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C14(H14), C16(H16), C18(H18)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5A), O8(H8), O10(H10), O11(H11)
;
_shelx_res_checksum              60551
_shelx_hkl_checksum              35662
_olex2_submission_special_instructions 'No special instructions were received'