Straightforward Access to the [3.2.2]Nonatriene Structural Framework via Intramolecular Cyclopropenation/Buchner Reaction/Cope Rearrangement Cascade.
Xu, Xinfang; Wang, Xiangbo; Zavalij, Peter Y.; Doyle, Michael P.; Organic letters 17 (2015) 790–793; doi:10.1021/ol503498n

data_1518718
_publ_section_title
;
 Straightforward Access to the [3.2.2]Nonatriene Structural Framework via
 Intramolecular Cyclopropenation/Buchner Reaction/Cope Rearrangement
 Cascade.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              790
_journal_page_last               793
_journal_paper_doi               10.1021/ol503498n
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C18 H26 O4 Si'
_chemical_formula_sum            'C18 H26 O4 Si'
_chemical_formula_weight         334.48
_chemical_name_common            Organics
_chemical_name_systematic
;
Organics
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2012 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.759(4)
_cell_length_b                   7.4334(18)
_cell_length_c                   30.141(7)
_cell_measurement_reflns_used    15001
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.4
_cell_volume                     3754.9(15)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2012'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.1148329
_diffrn_orient_matrix_UB_12      0.0309985
_diffrn_orient_matrix_UB_13      0.0012379
_diffrn_orient_matrix_UB_21      -0.0027987
_diffrn_orient_matrix_UB_22      -0.0023994
_diffrn_orient_matrix_UB_23      0.0331456
_diffrn_orient_matrix_UB_31      0.0700328
_diffrn_orient_matrix_UB_32      -0.0509342
_diffrn_orient_matrix_UB_33      -0.0008067
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            46484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+2.2880P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             3887
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'Available on request'
_cod_data_source_file            ol503498n_si_002.cif
_cod_data_source_block           2545
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 1518718--1518719.cif.
;
_cod_original_cell_volume        3754.8(16)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1518718
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.989
_iucr_refine_reflections_details 'Available on request'
_diffrn_measurement_frame_width-ccd 512