Role of Anions on the Crystal Structures of Copper(II) and Zinc(II) Complexes of a Tunable Butterfly Cyclophane Macrocycle
Martin Chadim; Pilar Díaz; Enrique García-España; Jana Hodačová; Julio Latorre; Malva Liu-González; Santiago V. Luis; José M. Llinares; Jiří Závada; Inorganic Chemistry 44 (2005) 7503–7510; doi:10.1021/ic051099j

data_4309778
_publ_section_title
;
Role of Anions on the Crystal Structures of Copper(II) and Zinc(II)
Complexes of a Tunable Butterfly Cyclophane Macrocycle
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7503
_journal_page_last               7510
_journal_paper_doi               10.1021/ic051099j
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C13 H25 Cl F3 N4 O3.3 S Zn'
_chemical_formula_sum            'C13 H25 Cl F3 N4 O3.3 S Zn'
_chemical_formula_weight         480.05
_chemical_name_common            'Compound jm1_3'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-04-05T17:37:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                84.262(5)
_cell_angle_beta                 77.490(5)
_cell_angle_gamma                73.558(5)
_cell_formula_units_Z            2
_cell_length_a                   8.472(5)
_cell_length_b                   9.310(5)
_cell_length_c                   13.745(5)
_cell_measurement_reflns_used    5606
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     1014.2(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maXus(Mackay et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0066993
_diffrn_orient_matrix_UB_12      -0.0337443
_diffrn_orient_matrix_UB_13      -0.0637593
_diffrn_orient_matrix_UB_21      -0.1095945
_diffrn_orient_matrix_UB_22      -0.0272287
_diffrn_orient_matrix_UB_23      -0.0145582
_diffrn_orient_matrix_UB_31      -0.0279761
_diffrn_orient_matrix_UB_32      0.060686
_diffrn_orient_matrix_UB_33      -0.0113742
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.1616
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6373
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             495
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   32.865
_refine_ls_goodness_of_fit_gt    35.529
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.2171
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          1.817
_refine_ls_shift/su_mean         0.165
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1301P)^2^+1.7880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         99.99
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2783
_reflns_number_gt                1715
_reflns_number_total             4164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051099jsi20050701_104326.cif
_cod_data_source_block           jm1
_cod_database_code               4309778