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_4075492
_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            'C13 H22 Fe O2 Si3'
_chemical_formula_weight         350.43
_chemical_name_systematic
; 
 (?5-cyclopentadienyl)iron(dicarbonyl)hexamethyltrisilacyclopentane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.183(5)
_cell_length_b                   10.707(5)
_cell_length_c                   13.350(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1808.3(13)
_computing_cell_refinement       'as above'
_computing_data_collection       'Siemens P3 data coll. progr. 1988'
_computing_data_reduction        'as above'
_computing_molecular_graphics    'Siemens XP (Sheldrick 1988)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens R3m/V diffractometer'
_diffrn_measurement_method       '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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3480
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0.3%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   'semi-empirical SHELXTL 1988'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+0.2913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                2423
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060320csi20060410_054123.cif
_cod_data_source_block           795t50
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4075492