Three transition-metal complexes with the macrocyclic ligand <i>meso</i>-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (<i>L</i>): [Cu(ClO~4~)~2~(<i>L</i>)], [Zn(NO~3~)~2~(<i>L</i>)] and [CuCl(<i>L</i>)(H~2~O)]Cl
Yasmin, Sabina; Suarez, Sebastián; Doctorovich, Fabio; Roy, Tapashi G.; Baggio, Ricardo; Acta Crystallographica Section C 69 (2013) 862–867; doi:10.1107/S0108270113018465

data_2019104
_publ_section_title
;
 Three transition-metal complexes with the macrocyclic ligand
 <i>meso</i>-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane
 (<i>L</i>): [Cu(ClO~4~)~2~(<i>L</i>)], [Zn(NO~3~)~2~(<i>L</i>)] and
 [CuCl(<i>L</i>)(H~2~O)]Cl
;
_journal_coeditor_code           SK3501
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              862
_journal_page_last               867
_journal_paper_doi               10.1107/S0108270113018465
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cu Cl (C18 H40 N4) (H2 O)] Cl'
_chemical_formula_moiety         'C16 H38 Cl Cu N4 O +, Cl -'
_chemical_formula_sum            'C16 H38 Cl2 Cu N4 O'
_chemical_formula_weight         436.94
_chemical_name_systematic
'Aquachlorido(<i>meso</i>-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)copper(II) chloride'
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.255(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0350(4)
_cell_length_b                   11.6288(2)
_cell_length_c                   13.8132(4)
_cell_measurement_temperature    295(2)
_cell_volume                     2101.10(10)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Oxford Gemini S Ultra CCD area-detector'
_diffrn_measurement_method       '\w scans, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45230
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            blue--violet
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5230
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.6364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                4195
_reflns_number_total             5230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3501.cif
_cod_data_source_block           III
_cod_original_cell_volume        2101.10(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019104
_cod_database_fobs_code          2019104