Synthesis, Structural Characterization, and Magnetic Studies of Polynuclear Iron Complexes with a New Disubstituted Pyridine Ligand
Hayley A. Burkill; Neil Robertson; Ramón Vilar; Andrew J. P. White; David J. Williams; Inorganic Chemistry 44 (2005) 3337–3346; doi:10.1021/ic048620e

data_4308837
_publ_section_title
;
Synthesis, Structural Characterization, and Magnetic Studies of Polynuclear
Iron Complexes with a New Disubstituted Pyridine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3337
_journal_page_last               3346
_journal_paper_doi               10.1021/ic048620e
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H66 Cl4 Fe6 N10 O17'
_chemical_formula_weight         1435.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.052(8)
_cell_length_b                   21.790(6)
_cell_length_c                   10.205(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      4.06
_cell_volume                     6392(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.1643
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4424
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         2.54
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.736
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.2660
_exptl_absorpt_correction_type   'Lamina [1 0 0]'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.227
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.194
_refine_ls_restrained_S_obs      1.205
_refine_ls_R_factor_all          0.2135
_refine_ls_R_factor_obs          0.0871
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2978
_refine_ls_wR_factor_obs         0.1886
_reflns_number_observed          1787
_reflns_number_total             4327
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic048620esi20041004_064432_3.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0985P)^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^)+(0.0985P)^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        6391.3(27)
_cod_original_formula_sum        'C40 H66 N10 O17 Cl4 Fe6'
_cod_database_code               4308837