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_4316875
_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            'C30 H48 Cl2 Fe P2 Pt'
_chemical_formula_weight         792.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.259(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6457(15)
_cell_length_b                   16.942(2)
_cell_length_c                   17.134(2)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.57
_cell_volume                     3089.5(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41788
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    5.288
_exptl_absorpt_correction_T_max  0.7085
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         22742
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                20152
_reflns_number_total             22742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016164_si_002_05.cif
_cod_data_source_block           '[PtCl2(RiPrFL)]'
_cod_depositor_comments
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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        3089.4(7)
_cod_database_code               4316875