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_7111063
_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            'C124 H116 Cl8 Fe4 N20 O13 S8'
_chemical_formula_weight         2857.85
_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                 100.66(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.760(4)
_cell_length_b                   21.356(5)
_cell_length_c                   25.690(8)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    150
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     6341(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14494
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_count 99
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         13833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0560P)^2^+12.2383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                9226
_reflns_number_total             13833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005671psup1.cif
_cod_data_source_block           (1)
_cod_original_sg_symbol_H-M      'P21 /c'
_cod_database_code               7111063