Synthesis and crystal structure of [2,7,12-trimethyl-3,7,11,17-tetraazabicyclo[11.3.1]heptadeca-1(17),13,15-triene-κ^4^<i>N</i>]copper(II) bis(perchlorate)
Hilvano, Edward Gabrielle V.; Yang, Guang; Emnacen, Inno A.; Rybak-Akimova, Elena V.; Billones, Junie B.; Carrillo, Maria Constancia O.; Noll, Bruce C.; Organo, Voltaire G.; Acta Crystallographica Section E 72 (2016) 1009–1012; doi:10.1107/S2056989016009701

data_2241731
_publ_section_title
;
 Synthesis and crystal structure of
 [2,7,12-trimethyl-3,7,11,17-tetraazabicyclo[11.3.1]heptadeca-1(17),13,15-triene-\k^4^<i>N</i>]copper(II)
 bis(perchlorate)
;
_journal_coeditor_code           ZL2666
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1009
_journal_page_last               1012
_journal_paper_doi               10.1107/S2056989016009701
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cu (C16 H28 N4)] (Cl O4)2'
_chemical_formula_moiety         'C16 H28 Cu N4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C16 H28 Cl2 Cu N4 O8'
_chemical_formula_weight         538.86
_chemical_name_systematic
;
[2,7,12-Trimethyl-3,7,11,17-tetraazabicyclo[11.3.1]heptadeca-\
1(17),13,15-triene-\k^4^<i>N</i>]copper(II) bis(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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.153(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6918(12)
_cell_length_b                   12.0588(16)
_cell_length_c                   20.068(3)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.64
_cell_measurement_theta_min      2.89
_cell_volume                     2103.4(5)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 and <i>Bruker Instrument Service</i> (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006) and OLEX2 (Dolomanov <i>et
al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 1.024
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36478
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.221
_diffrn_reflns_theta_min         2.889
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  0.4541
_exptl_absorpt_correction_T_min  0.4135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       'clear dark blue cube'
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                5054
_reflns_number_total             5284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2666sup1.cif
_cod_data_source_block           I
_cod_database_code               2241731
_cod_database_fobs_code          2241731
_shelx_hkl_checksum              48525
_shelx_res_checksum              89738