Crystal structure of (glycinto-κ 2 O,N ′)-[5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ 4 N,N ′,N ″,N ‴]nickel(II) perchlorate monohydrate C18H42ClN5NiO7
Zhang, Zu-Jiao; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 645–647; doi:10.1515/ncrs-2023-0131

data_8107519
_publ_section_title
;
 Crystal structure of (glycinto-\k 2 O,N
 &#x2032;)-[5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k
 4 N,N &#x2032;,N &#x2033;,N &#x2034;]nickel(II) perchlorate monohydrate
 C18H42ClN5NiO7
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              645
_journal_page_last               647
_journal_paper_doi               10.1515/ncrs-2023-0131
_journal_volume                  238
_journal_year                    2023
_chemical_absolute_configuration adm
_chemical_formula_sum            'C18 H42 Cl N5 Ni O7'
_chemical_formula_weight         534.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.270(3)
_cell_length_b                   9.918(2)
_cell_length_c                   17.603(4)
_cell_measurement_reflns_used    4317
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.17
_cell_measurement_theta_min      2.50
_cell_volume                     2491.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12902
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.131
_diffrn_reflns_theta_min         2.053
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1428 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.919
_reflns_Friedel_fraction_max     0.896
_reflns_number_gt                3834
_reflns_number_total             5229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0131_suppl_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        2491.4(10)
_cod_database_code               8107519
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.873
_shelx_res_checksum              36068
_shelx_hkl_checksum              1128