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_4308835
_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            'C17 H25 N5 O4'
_chemical_formula_weight         363.42
_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                 97.854(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.0740(10)
_cell_length_b                   9.7147(3)
_cell_length_c                   33.303(2)
_cell_measurement_reflns_used    69
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      10.63
_cell_volume                     7715.6(6)
_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      293(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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            5882
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         2.68
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00014(5)
_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   1.045
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.312
_refine_ls_restrained_S_obs      1.429
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_obs          0.0630
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+2.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1962
_refine_ls_wR_factor_obs         0.1693
_reflns_number_observed          4097
_reflns_number_total             5725
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic048620esi20041004_064432_1.cif
_cod_data_source_block           Compound_H2L
_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^)+(0.1116P)^2^+2.8862P] 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^)+(0.1116P)^2^+2.8862P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4308835