Synthesis, structural characterization, EPR spectroscopy and Hirshfeld surface analysis of a novel Cu^2+^-doped 3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane bis(perchlorate)
Moncol, Jan; Mazúr, Milan; Valko, Marian; Choi, Jong-Ha; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619005588

data_2021617
_publ_section_title
;
 Synthesis, structural characterization, EPR spectroscopy and Hirshfeld
 surface analysis of a novel Cu^2+^-doped
 3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane
 bis(perchlorate)
;
_journal_coeditor_code           YF3174
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619005588
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'{[Cu (C22 H44 N4)] (Cl O4)2}0.69, (C22 H46 N4 2+, 2Cl O4 -)0.31'
_chemical_formula_moiety         'C22 H44.62 Cu0.69 N4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C22 H44.62 Cl2 Cu0.69 N4 O8'
_chemical_formula_weight         607.98
_chemical_name_systematic
;[3,14-Diethyl-2,6,13,17-tetraazatricyclo[16.4.0.0^7,12^]docosane]copper(II)
bis(perchlorate)--3,14-diethyl-2,13-diaza-6,17-diazoniatricyclo[16.4.0.0^7,12^]docosane bis(perchlorate) (0.69/0.31)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.722(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2244(7)
_cell_length_b                   11.5540(8)
_cell_length_c                   12.8659(9)
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.51
_cell_measurement_theta_min      5.17
_cell_volume                     1358.80(17)
_computing_cell_refinement
;
<i>Recipe</i> in <i>X-AREA</i> (Stoe & Cie, 2018)
;
_computing_data_collection
;
<i>Pilatus3_SV</i> in <i>X-AREA</i> (Stoe & Cie, 2018)
;
_computing_data_reduction
;
<i>Integrate</i> and <i>LANA</i> in <i>X-AREA</i> (Stoe & Cie, 2018)
;
_computing_molecular_graphics
;
<i>DIAMOND-4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>X-AREA</i> (Stoe & Cie, 2018)
;
_computing_structure_refinement
;
<i>SHELXL2018</i> (Sheldrick, 2015b)
within <i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_solution
;
<i>SHELXT2018</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Pilatus3R 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari with Xenocs Genix3D Cu HF'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12575
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.635
_diffrn_reflns_theta_min         5.166
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.148
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>LANA</i>; Koziskova <i>et al.</i>,  2016)
;
_exptl_crystal_colour            'pinkish violet'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             645
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.466
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0765
_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^)+(0.1419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.2070
_reflns_number_gt                1653
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yf3174sup1.cif
_cod_data_source_block           global
_cod_database_code               2021617
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.704
_shelx_hkl_checksum              97648
_shelx_res_checksum              69622