Synthesis of 4:5-Benzo-1-cobalta-2-silacyclopentenes and their Reactions with Alkynes and Alkenes: An Expedient Route to Silicon-Containing Polycyclic Frameworks
Agenet, Nicolas; Mirebeau, Jean-Hugues; Petit, Marc; Thouvenot, René; Gandon, Vincent; Malacria, Max; Aubert, Corinne; Organometallics 26 (2007) 819–; doi:10.1021/om0607245

data_4072501
_publ_section_title
;
 Synthesis of 4:5-Benzo-1-cobalta-2-silacyclopentenes and their Reactions
 with Alkynes and Alkenes:&#x00A0; An Expedient Route to
 Silicon-Containing Polycyclic Frameworks
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              819
_journal_paper_doi               10.1021/om0607245
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C42 H36 Co1 P1 Si1'
_chemical_formula_sum            'C42 H36 Co P Si'
_chemical_formula_weight         658.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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             04-11-10
_audit_creation_method           CRYSTALS_ver_12.24
_cell_angle_alpha                90
_cell_angle_beta                 99.46(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.742(5)
_cell_length_b                   18.117(9)
_cell_length_c                   20.848(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      12.0
_cell_volume                     6610(5)
_computing_cell_refinement       'Cad4 Express, (Straver, 1992)'
_computing_data_collection       'Cad4 Express, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin, Prout & Lilley, 1994)'
_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      295
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius Mach3'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12435
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         1.398
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.94
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1635
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         3791
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2233
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.000172
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.34 -0.448 1.46 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1561
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0785
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3791
_reflns_number_total             11597
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om0607245si20060809_100020.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C42 H36 Co1 P1 Si1'
_cod_database_code               4072501