Studies of iron-mediated Pauson–Khand reactions of 1,1-disubstituted-allenylsilanes: mechanistic implications for a reactive three-membered iron metallacycle
Williams, David R.; Shah, Akshay A.; Mazumder, Shivnath; Baik, Mu-Hyun; Chemical Science 4 (2013) 238–; doi:10.1039/c2sc21404k

data_1514831
_publ_section_title
;
 Studies of iron-mediated Pauson--Khand reactions of
 1,1-disubstituted-allenylsilanes: mechanistic implications for a reactive
 three-membered iron metallacycle
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              238
_journal_paper_doi               10.1039/c2sc21404k
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C25 H38 O2 Si2'
_chemical_formula_sum            'C25 H38 O2 Si2'
_chemical_formula_weight         426.75
_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
_audit_creation_date             10-10-13
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 102.587(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.129(3)
_cell_length_b                   8.192(2)
_cell_length_c                   26.318(6)
_cell_measurement_reflns_used    1810
_cell_measurement_temperature    150
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     2552.1(11)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            17208
_diffrn_reflns_theta_full        25.036
_diffrn_reflns_theta_max         25.036
_diffrn_reflns_theta_min         1.730
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9997
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.0004307
_refine_ls_shift/su_mean         0.0000241
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 5.75P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1221
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1221
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                2830
_reflns_number_total             4475
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.00
_oxford_diffrn_Wilson_scale      51.21
_oxford_refine_ls_r_factor_ref   0.0934
_oxford_refine_ls_scale          0.14896(8)
_oxford_reflns_number_all        4475
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10101_0m in P2(1)/n'
_cod_data_source_file            c2sc21404k.txt
_cod_data_source_block           10101
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2552.2(11)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               1514831