meso-(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradec-4,11-diene) copper(II) perchlorate; an unexpected preparation and structure determination
Neil F. Curtis; Jan Wikaira; Inorganica Chimica Acta 396 (2013) 14–16; doi:10.1016/j.ica.2012.11.027

data_1512962
_publ_section_title
;
 meso-(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradec-4,11-diene)
 copper(II) perchlorate; an unexpected preparation and structure
 determination
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              14
_journal_page_last               16
_journal_paper_doi               10.1016/j.ica.2012.11.027
_journal_volume                  396
_journal_year                    2013
_chemical_formula_moiety         'C16 H32 N4 Cu, 2(Cl O4)'
_chemical_formula_sum            'C16 H32 Cl2 Cu N4 O8'
_chemical_formula_weight         542.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.179(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2477(3)
_cell_length_b                   10.4920(2)
_cell_length_c                   10.9152(3)
_cell_measurement_reflns_used    2463
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      73.3308
_cell_measurement_theta_min      4.2102
_cell_volume                     1094.32(5)
_computing_data_collection
; CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'ORTEP3.2 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3474
_diffrn_reflns_theta_full        65.49
_diffrn_reflns_theta_max         65.49
_diffrn_reflns_theta_min         4.63
_exptl_absorpt_coefficient_mu    4.118
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.9409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                1759
_reflns_number_total             1876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-14-16.cif
_cod_data_source_block           nfc4-9-4
_cod_database_code               1512962