The first structural characterization of the protonated azacyclam ligand in <i>catena</i>-poly[[[(perchlorato)copper(II)]-μ-3-(3-carboxypropyl)-1,5,8,12-tetraaza-3-azoniacyclotetradecane] bis(perchlorate)]
Tsymbal, Liudmyla V.; Arion, Vladimir B.; Lampeka, Yaroslaw D.; Acta Crystallographica Section E 75 (2019) 1700–1704; doi:10.1107/S205698901901377X

data_2243138
_publ_section_title
;
 The first structural characterization of the protonated azacyclam ligand
 in
 <i>catena</i>-poly[[[(perchlorato)copper(II)]-\m-3-(3-carboxypropyl)-1,5,8,12-tetraaza-3-azoniacyclotetradecane]
 bis(perchlorate)]
;
_journal_coeditor_code           HB7857
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1700
_journal_page_last               1704
_journal_paper_doi               10.1107/S205698901901377X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Cu (C13 H30 N5 O2) (Cl O4)] (Cl O4)2'
_chemical_formula_moiety         'C13 H30 Cl Cu N5 O6 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C13 H30 Cl3 Cu N5 O14'
_chemical_formula_weight         650.31
_chemical_name_systematic
'<i>catena</i>-Poly[[[(perchlorato-\k<i>\kO</i>)copper(II)]-\m-\m-3-(3-carboxypropyl)-1,5,8,12-tetraaza-3-azoniacyclotetradecane-\k^4^<i>N</i>^1^,<i>N</i>^2^,<i>N</i>^4^,<i>N</i>^5^] bis(perchlorate)]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.990(4)
_cell_length_b                   9.3640(19)
_cell_length_c                   13.636(3)
_cell_measurement_reflns_used    4345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.480
_cell_measurement_theta_min      2.140
_cell_volume                     2424.8(9)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.418
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.445
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.50(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1002P)^2^+10.5107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.2151
_reflns_number_gt                2787
_reflns_number_total             4458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7857sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2424.9(8)
_cod_database_code               2243138
_shelx_estimated_absorpt_t_min   0.799
_shelx_estimated_absorpt_t_max   0.859
_shelx_hkl_checksum              79075
_shelx_res_checksum              29814
_shelxl_version_number           2.014
_cod_database_fobs_code 2243138