Structural and Redox Properties of Novel Spirocyclic 1-Sila-3-ferracyclobutanes, [(η5-C5H4)Fe(L2)CH2SiMe2], L2= P−P (diphosphine)
Kumar, Mukesh; Cervantes-Lee, Francisco; Sharma, Hemant K.; Pannell, Keith H.; Organometallics 26 (2007) 3005–; doi:10.1021/om061141y

data_4072930
_publ_section_title
;
 Structural and Redox Properties of Novel Spirocyclic
 1-Sila-3-ferracyclobutanes, [(\h5-C5H4)Fe(L2)CH2SiMe2], L2= P&#x2212;P
 (diphosphine)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3005
_journal_paper_doi               10.1021/om061141y
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C34 H36 Fe P2 Si'
_chemical_formula_weight         590.51
_chemical_name_systematic
; 
 ? 
;
_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                   12.3293(17)
_cell_length_b                   12.9894(18)
_cell_length_c                   18.476(3)
_cell_measurement_reflns_used    4328
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      50.423
_cell_measurement_theta_min      4.409
_cell_volume                     2958.9(8)
_computing_cell_refinement       'Bruker SMART V5.625, 2001'
_computing_data_collection       'Bruker SMART V5.625, 2001'
_computing_data_reduction        'Bruker SAINT V5.622, 2001'
_computing_molecular_graphics    'Bruker SHELXTL V6.10, 2000'
_computing_publication_material  'Bruker SHELXTL V6.10, 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega sacns'
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18918
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.8759
_exptl_absorpt_correction_T_min  0.8219
_exptl_absorpt_correction_type   'Bruker SADABS V2.05'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                6147
_reflns_number_total             6953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061141y.cif
_cod_data_source_block           164mk1m
_cod_original_cell_volume        2959.0(7)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4072930