Synthesis and characterization of iron(III) complexes of a new ligand containing a potentially bridging carboxylate; structural characterization of a helical tetranuclear iron complex
Trukhan, Vladimir M.; Shteinman, Albert A.; Pierpont, Cortlandt G.; Jensen, Kenneth B.; Nordlander, Ebbe; Chemical Communications  (1999) 1193–; doi:10.1039/a809888c

data_7110446
_publ_section_title
;
 Synthesis and characterization of iron(III) complexes of a new ligand
 containing a potentially bridging carboxylate; structural
 characterization of a helical tetranuclear iron complex
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1193
_journal_paper_doi               10.1039/a809888c
_journal_year                    1999
_chemical_formula_sum            'C168 H160 Cl16 Fe8 N24 O73.5'
_chemical_formula_weight         4705.20
_space_group_IT_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_creation_method           SHELXL
_cell_angle_alpha                77.5210(10)
_cell_angle_beta                 89.2450(10)
_cell_angle_gamma                86.4320(10)
_cell_formula_units_Z            2
_cell_length_a                   16.4575(3)
_cell_length_b                   17.8346(2)
_cell_length_c                   19.3790(3)
_cell_measurement_reflns_used    3861
_cell_measurement_temperature    293(2)
_cell_volume                     5542.84(15)
_computing_cell_refinement       'Siemens CCD'
_computing_data_collection       'Siemens CCD'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXP
_computing_publication_material  SHELXCIF
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD/Rigaku gen.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_av_sigmaI/netI    0.6577
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45710
_diffrn_reflns_theta_max         31.76
_diffrn_reflns_theta_min         1.08
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.854
_refine_ls_goodness_of_fit_obs   1.327
_refine_ls_hydrogen_treatment    'fixed, riding '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         31848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_restrained_S_obs      1.327
_refine_ls_R_factor_all          0.4759
_refine_ls_R_factor_obs          0.0973
_refine_ls_shift/esd_max         0.121
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3538
_refine_ls_wR_factor_obs         0.2047
_reflns_number_observed          5166
_reflns_number_total             31848
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809888csup1.cif
_cod_data_source_block           minka
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5542.85(15)
_cod_original_formula_sum        'C168 H160 Cl16 Fe8 N24 O73.50'
_cod_database_code               7110446