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_4316873
_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_formula_sum            'C24 H36 Cl2 Fe P2 Pt'
_chemical_formula_weight         708.31
_chemical_name_systematic
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 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   11.2156(14)
_cell_length_b                   13.7145(17)
_cell_length_c                   16.728(2)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      2.35
_cell_volume                     2573.0(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 0.993
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27265
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.30
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    6.337
_exptl_absorpt_correction_T_max  0.4122
_exptl_absorpt_correction_T_min  0.3496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         9783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                9405
_reflns_number_total             9783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016164_si_002_03.cif
_cod_data_source_block           '[PtCl2(REtFT)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        2573.1(5)
_cod_database_code               4316873