The Utility of Sodium Diisopropylamide (NADA): Formation of a New Transition Metalate via Silyl Migration Chemistry, [(η5-Me3SiC5H4)Fe(CO)(PPh3)]−Na+(SiFpPNa), and Resulting Thermal Rearrangements of the Complexes SiFpP−CH2SiMe2R (R = H, SiMe3) to SiFpP−SiMe2CH2R
Munguia, Teresita; Bakir, Zaynab A.; Cervantes-Lee, Francisco; Metta-Magana, Alejandro; Pannell, Keith H.; Organometallics 28 (2009) 5777–; doi:10.1021/om9006032

data_4070077
_publ_section_title
;
 The Utility of Sodium Diisopropylamide (NADA): Formation of a New
 Transition Metalate via Silyl Migration Chemistry,
 [(\h5-Me3SiC5H4)Fe(CO)(PPh3)]&#x2212;Na+(SiFpPNa), and Resulting Thermal
 Rearrangements of the Complexes SiFpP&#x2212;CH2SiMe2R (R = H, SiMe3) to
 SiFpP&#x2212;SiMe2CH2R
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5777
_journal_paper_doi               10.1021/om9006032
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C36 H48 Fe O P Si3'
_chemical_formula_weight         667.83
_chemical_name_systematic
; 
 (carbonyl)(triphenylphosphine)(1,3-tetramethyl-1,2-di-silabutyl)(trimethylsylylcyclopentadienyl)iron(III) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.349(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2515(9)
_cell_length_b                   18.0499(16)
_cell_length_c                   22.205(2)
_cell_measurement_reflns_used    4170
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.701
_cell_measurement_theta_min      2.437
_cell_volume                     3697.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22503
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8043
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+1.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                6446
_reflns_number_total             8043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9006032_si_001.cif
_cod_data_source_block           116tm1ms
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3697.4(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4070077