Iron Thiobiurets: Single-Source Precursors for Iron Sulfide Thin Films
Karthik Ramasamy; Mohammad A. Malik; Madeline Helliwell; Floriana Tuna; Paul O'Brien; Inorganic Chemistry 49 (2010) 8495–8503; doi:10.1021/ic1011204

data_4316526
_publ_section_title
;
 Iron Thiobiurets: Single-Source Precursors for Iron Sulfide Thin Films
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8495
_journal_page_last               8503
_journal_paper_doi               10.1021/ic1011204
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C44 H87 Fe N10 O3 S3'
_chemical_formula_weight         956.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.144(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.341(3)
_cell_length_b                   15.224(3)
_cell_length_c                   25.725(5)
_cell_measurement_reflns_used    790
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.68
_cell_measurement_theta_min      2.94
_cell_volume                     5572.9(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_sigmaI/netI    0.1686
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31561
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.709
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         11281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.709
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                5685
_reflns_number_total             11281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011204_si_002.cif
_cod_data_source_block           s3000m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5572.9(18)
_cod_database_code               4316526