Electrochemistry of 1,1'-Bis(2,4-dialkylphosphetanyl)ferrocene and 1,1'-Bis(2,5-dialkylphospholanyl)ferrocene Ligands: Free Phosphines, Metal Complexes, and Chalcogenides
Chelsea L. Mandell; Shannon S. Kleinbach; William G. Dougherty; W. Scott Kassel; Chip Nataro; Inorganic Chemistry 49 (2010) 9718–9727; doi:10.1021/ic1016164

data_4316874
_publ_section_title
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 Electrochemistry of 1,1'-Bis(2,4-dialkylphosphetanyl)ferrocene and
 1,1'-Bis(2,5-dialkylphospholanyl)ferrocene Ligands: Free Phosphines,
 Metal Complexes, and Chalcogenides
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9718
_journal_page_last               9727
_journal_paper_doi               10.1021/ic1016164
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_formula_sum            'C12 H18 Fe0.5 P S'
_chemical_formula_weight         253.22
_chemical_name_systematic
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 ? 
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_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7105(9)
_cell_length_b                   7.7105(9)
_cell_length_c                   41.386(5)
_cell_measurement_reflns_used    8740
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      2.69
_cell_volume                     2460.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            25456
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.29
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.8741
_exptl_absorpt_correction_T_min  0.8370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0388P)^2^+0.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                4438
_reflns_number_total             4733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016164_si_002_04.cif
_cod_data_source_block           '[SEtFTS2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_formula_sum        'C12 H18 Fe0.50 P S'
_cod_database_code               4316874