Bridgehead Hydrogen Atoms Are Important: Unusual Electrochemistry and Proton Reduction at Iron Dimers with Ferrocenyl-Substituted Phosphido Bridges
Gimbert-Suriñach, Carolina; Bhadbhade, Mohan; Colbran, Stephen B.; Organometallics 31 (2012) 3480–; doi:10.1021/om201126w

data_4078204
_publ_section_title
;
 Bridgehead Hydrogen Atoms Are Important: Unusual Electrochemistry and
 Proton Reduction at Iron Dimers with Ferrocenyl-Substituted Phosphido
 Bridges
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3480
_journal_paper_doi               10.1021/om201126w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C28 H24 Fe4 O6 P2'
_chemical_formula_weight         741.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   7.7966(4)
_cell_length_b                   31.8493(15)
_cell_length_c                   11.5616(5)
_cell_measurement_reflns_used    3551
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      25.061
_cell_measurement_theta_min      2.689
_cell_volume                     2870.9(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2007)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>SAINT</i>  '
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      155(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD Diffractometer'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17933
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    2.133
_exptl_absorpt_correction_T_max  0.9195
_exptl_absorpt_correction_T_min  0.6924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2001)'
_exptl_crystal_colour            'Orange yellow'
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0243P)^2^+2.9944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                3418
_reflns_number_total             4462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201126w_si_003.cif
_cod_data_source_block           inpna21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4078204