Crystal structure of (4-aminobenzoato-κ2 O,O′)-[5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4 N,N′,N′′,N′′′]nickel(II) perchlorate monohydrate, C23H44ClN5NiO7
Ou, Guang-Chuan; Zhou, Qiang; Wang, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1095–1097; doi:10.1515/ncrs-2020-0184

data_8105388
_publ_section_title
;
 Crystal structure of (4-aminobenzoato-\k2
 O,O&#x2032;)-[5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k4
 N,N&#x2032;,N&#x2032;&#x2032;,N&#x2032;&#x2032;&#x2032;]nickel(II)
 perchlorate monohydrate, C23H44ClN5NiO7
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1095
_journal_page_last               1097
_journal_paper_doi               10.1515/ncrs-2020-0184
_journal_volume                  235
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C23 H44 Cl N5 Ni O7'
_chemical_formula_weight         596.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4994(16)
_cell_length_b                   19.799(2)
_cell_length_c                   20.040(2)
_cell_measurement_reflns_used    7957
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.29
_cell_volume                     5753.0(10)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40380
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.080
_diffrn_reflns_theta_min         1.446
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.8411
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.220
_exptl_transmission_factor_max   0.84
_exptl_transmission_factor_min   0.70
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
; 
 Flack x determined using 3917 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12576
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0552P)^2^+1.2037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                10129
_reflns_number_total             12576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0184_suppl.cif
_cod_data_source_block           L806285m
_cod_original_cell_volume        5752.9(11)
_cod_database_code               8105388
_shelx_estimated_absorpt_t_min   0.700
_shelx_estimated_absorpt_t_max   0.841