Synthesis and structural characterisation of Fe(ii) and Cu(i) complexes of a new tetrafunctional N-donor ligand with dodecahedral or tetrahedral binding domains
Ameerunisha, Sardar; Schneider, Jörg; Meyer, Thomas; Henkel, Gerald; Zacharias, Panthapally S.; Bill, Eckhard; Chemical Communications  (2000) 2155–; doi:10.1039/b005671p

data_7111064
_publ_section_title
;
 Synthesis and structural characterisation of Fe(ii) and Cu(i) complexes
 of a new tetrafunctional N-donor ligand with dodecahedral or tetrahedral
 binding domains
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2155
_journal_paper_doi               10.1039/b005671p
_journal_year                    2000
_chemical_formula_sum            'C65 H65 Cl2 Cu2 N11 O11 S4'
_chemical_formula_weight         1502.50
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                89.54(2)
_cell_angle_beta                 84.40(2)
_cell_angle_gamma                87.11(2)
_cell_formula_units_Z            2
_cell_length_a                   11.188(3)
_cell_length_b                   16.587(4)
_cell_length_c                   17.538(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    150
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     3235.0(14)
_computing_cell_refinement       'P3 (Siemens, 1991)'
_computing_data_collection       'P3 (Siemens, 1991)'
_computing_data_reduction        'P3 (Siemens, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4RA'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14631
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_interval_count 99
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         14130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0402P)^2^+3.1977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                10639
_reflns_number_total             14130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005671psup1.cif
_cod_data_source_block           (2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111064