B(C6F5)3-Catalyzed Synthesis of Benzofused-Siloles
Curless, Liam D.; Ingleson, Michael J.; Organometallics 33 (2014) 7241–; doi:10.1021/om501033p

data_4084961
_publ_section_title
;
 B(C6F5)3-Catalyzed Synthesis of Benzofused-Siloles
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7241
_journal_paper_doi               10.1021/om501033p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C21 H18 Si'
_chemical_formula_sum            'C21 H18 Si'
_chemical_formula_weight         298.46
_chemical_name_systematic        1,1-diphenyl-2-methyl-1-silaindene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.925(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6476(10)
_cell_length_b                   9.6898(4)
_cell_length_c                   19.1479(11)
_cell_measurement_reflns_used    5584
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      28.4050
_cell_measurement_theta_min      3.5340
_cell_volume                     3272.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9959
_diffrn_measurement_details
;
  1 omega -103.00  -39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.8673  178.0000    0.0000 64

  2 omega  -88.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.8673  -77.0000 -180.0000 96

  3 omega   -2.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   57.0000   60.0000 92

  4 omega  -49.00   45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360  -57.0000  -90.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0249808000
_diffrn_orient_matrix_UB_12      -0.0077582000
_diffrn_orient_matrix_UB_13      -0.0366220000
_diffrn_orient_matrix_UB_21      -0.0309827000
_diffrn_orient_matrix_UB_22      -0.0073952000
_diffrn_orient_matrix_UB_23      0.0135529000
_diffrn_orient_matrix_UB_31      -0.0058353000
_diffrn_orient_matrix_UB_32      0.0724277000
_diffrn_orient_matrix_UB_33      -0.0025181000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20525
_diffrn_reflns_theta_full        25.9994
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2114
_exptl_crystal_description       block
_exptl_crystal_F_000             1265.0777
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.0619
_refine_diff_density_min         -0.3906
_refine_diff_density_rms         0.1271
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             6.7426
_refine_ls_goodness_of_fit_ref   1.0689
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0689
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1280P)^2^+2.6650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2280
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -23
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                4787
_reflns_number_total             6389
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om501033p_si_003.cif
_cod_data_source_block           amji186abs
_cod_depositor_comments
'Adding full bibliography for 4084960--4084961.cif.'
_cod_database_code               4084961
_chemical_oxdiff_formula         C21H18Si
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C17(H17), C26(H26), C28(H28), C30(H30),
 C34(H34), C43(H43), C46(H46), C58(H58), C59(H59), C62(H62), C63(H63), C70(H70),
  C71(H71), C85(H85), C90(H90), C96(H96), C98(H98), C104(H104), C105(H105),
 C108(H108), C117(H117), C123(H123), C133(H133), C148(H148), C161(H161),
 C164(H164), C165(H165)
2.b Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'