Photochemical Ring-Contraction of a Tetrasilaferracyclohexane of the (η5-C5H4)Fe(CO)2System to Trisilaferracyclopentanes
Sharma, Hemant K.; Cervantes-Lee, Francisco; Pannell, Keith H.; Organometallics 25 (2006) 3969–; doi:10.1021/om060320c

data_4075493
_publ_section_title
;
 Photochemical Ring-Contraction of a Tetrasilaferracyclohexane of the
 (\h5-C5H4)Fe(CO)2System to Trisilaferracyclopentanes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3969
_journal_paper_doi               10.1021/om060320c
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C30 H37 Fe O P Si3'
_chemical_formula_weight         584.69
_chemical_name_systematic
; 
 (Eta5-cyclopentadienyl)iron(carbonyl)triphenylphosphine
hexamethyltrisilacyclopentane 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.188(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.363(2)
_cell_length_b                   14.929(3)
_cell_length_c                   31.447(5)
_cell_measurement_reflns_used    85
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     6209.6(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25325
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   'Bruker SADABS V2.05'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0824P)^2^+3.8156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                3828
_reflns_number_total             4464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060320csi20060410_054123.cif
_cod_data_source_block           884hs1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6209.3(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075493