Click synthesis of symmetric bis-triazol ligands and full characterisation of their copper(ii)-complexes
Benkhellat, Zakia; Allali, Mustapha; Beley, Marc; Wenger, Emmanuel; Bernard, Maxime; Parizel, Nathalie; Selmeczi, Katalin; Joly, Jean-Pierre; New Journal of Chemistry 38 (2014) 419–; doi:10.1039/c3nj00570d

data_7053999
_publ_section_title
;
 Click synthesis of symmetric bis-triazol ligands and full
 characterisation of their copper(ii)-complexes
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              419
_journal_paper_doi               10.1039/c3nj00570d
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         'C25 H32 Cl Cu N8 O4, Cl O4'
_chemical_formula_sum            'C25 H32 Cl2 Cu N8 O8'
_chemical_formula_weight         707.04
_chemical_name_common            '[CuL6(ClO4)](ClO4)'
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-09-02 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8356(4)
_cell_length_b                   25.4907(6)
_cell_length_c                   8.1556(2)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.238
_cell_measurement_theta_min      1.588
_cell_volume                     3084.20(13)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Collect Bruker-Nonius'
_computing_data_reduction        HKL2000
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\w scans'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.238
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1460.0
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Flack x determined using 1871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.473(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4755
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0654P)^2^+10.6592P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                4401
_reflns_number_total             4755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00570d.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      Cmc21
_cod_database_code               7053999