Crystal structure of [3,10-bis(4-fluorophenethyl)-1,3,5,8,10,12-hexaazacyclotetradecane]nickel(II) diperchlorate
Kwak, Chee-Hun; Chang, Mee; Acta Crystallographica Section E 77 (2021) 148–152; doi:10.1107/S2056989020016795

data_2243732
_publ_section_title
;
 Crystal structure of
 [3,10-bis(4-fluorophenethyl)-1,3,5,8,10,12-hexaazacyclotetradecane]nickel(II)
 diperchlorate
;
_journal_coeditor_code           VM2242
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              148
_journal_page_last               152
_journal_paper_doi               10.1107/S2056989020016795
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ni (C24 H36 F2 N6)] (Cl O4)2'
_chemical_formula_moiety         'C24 H36 F2 N6 Ni, 2(Cl O4)'
_chemical_formula_sum            'C24 H36 Cl2 F2 N6 Ni O8'
_chemical_formula_weight         704.20
_chemical_name_systematic
;
[3,10-Bis(4-fluorophenethyl)-1,3,5,8,10,12-hexaazacyclotetradecane]nickel(II)
bis(perchlorate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 126.1890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9910(12)
_cell_length_b                   15.5187(11)
_cell_length_c                   13.8864(9)
_cell_measurement_reflns_used    3600
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.82
_cell_volume                     2955.1(4)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012), Mercury (Macrae <i>et al.</i>,
2020)
;
_computing_publication_material
;
WinGx (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker SMART 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  0.0827
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9357
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.982
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.629
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0449P)^2^+12.0119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                2737
_reflns_number_total             3400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2242sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243732
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.834
_shelx_hkl_checksum              3666
_shelx_res_checksum              48355
_cod_database_fobs_code 2243732