Crystal structure of catena-poly[(5,5,7,12,12,14-hexamethyl -1,4,8,11-tetraazacyclotetradecane- κ 4 N,N′,Nʺ,N‴)nickel(II)-(μ2-perchlorato-κ 2 O:O′)] 3,5-dicarboxybenzoate – methanol (1/2), C27H49ClN4NiO12
Wang, Qiong; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 745–747; doi:10.1515/ncrs-2022-0206

data_8107204
_publ_section_title
;
 Crystal structure of catena-poly[(5,5,7,12,12,14-hexamethyl
 -1,4,8,11-tetraazacyclotetradecane- \k 4
 N,N&#x2032;,N&#x02BA;,N&#x2034;)nickel(II)-(\m2-perchlorato-\k 2
 O:O&#x2032;)] 3,5-dicarboxybenzoate -- methanol (1/2), C27H49ClN4NiO12
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              745
_journal_page_last               747
_journal_paper_doi               10.1515/ncrs-2022-0206
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C16 H36 Cl N4 Ni O4, C9 H5 O6, 2(C H4 O)'
_chemical_formula_sum            'C27 H49 Cl N4 Ni O12'
_chemical_formula_weight         715.86
_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
_cell_angle_alpha                98.263(2)
_cell_angle_beta                 97.524(2)
_cell_angle_gamma                99.470(2)
_cell_formula_units_Z            2
_cell_length_a                   11.180(2)
_cell_length_b                   12.320(3)
_cell_length_c                   12.754(3)
_cell_measurement_reflns_used    7067
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.28
_cell_volume                     1693.1(6)
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19175
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.398
_diffrn_reflns_theta_min         1.634
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0675P)^2^+0.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6179
_reflns_number_total             7498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0206_suppl.cif
_cod_data_source_block           1
_cod_database_code               8107204
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H11 of O11, H12 of O12, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H4A of O4, H1A of O1
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C15(H15), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,
 H21B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O4(H4A)
;
_shelx_res_checksum              6960
_shelx_hkl_checksum              57447
_olex2_submission_special_instructions 'No special instructions were received'