Crystal structure of (perchlorato-κ<i>O</i>)(1,4,7,10-tetraazacyclododecane-κ^4^<i>N</i>)copper(II) perchlorate
Gray, Jessica L.; Gerlach, Deidra L.; Papish, Elizabeth T.; Acta Crystallographica Section E 73 (2017) 31–34; doi:10.1107/S2056989016019563

data_2241979
_publ_section_title
;
 Crystal structure of
 (perchlorato-\k<i>O</i>)(1,4,7,10-tetraazacyclododecane-\k^4^<i>N</i>)copper(II)
 perchlorate
;
_journal_coeditor_code           ZL2687
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              31
_journal_page_last               34
_journal_paper_doi               10.1107/S2056989016019563
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Cu (Cl O4) (C8 H20 N4)] Cl1 O4'
_chemical_formula_moiety         'C8 H20 Cl1 Cu N4 O4 +, Cl1 O4 -'
_chemical_formula_sum            'C8 H20 Cl2 Cu N4 O8'
_chemical_formula_weight         434.72
_chemical_name_common            '[Cu cyclen](ClO4)2'
_chemical_name_systematic
;
(Perchlorato-\k<i>O</i>)(1,4,7,10-tetraazacyclododecane-\k^4^<i>N</i>)copper(II)
perchlorate
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.9490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9387(2)
_cell_length_b                   15.0607(4)
_cell_length_c                   11.9235(3)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.8550
_cell_measurement_theta_min      2.2815
_cell_volume                     1603.05(7)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2013)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43306
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.160
_diffrn_reflns_theta_min         2.180
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.438
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         7519
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                6655
_reflns_number_total             7519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2687sup1.cif
_cod_data_source_block           I
_cod_database_code               2241979
_cod_database_fobs_code          2241979
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.745
_shelx_hkl_checksum              50979
_shelx_res_checksum              65629