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_1518719
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2012 & ZCIF'
_cell_angle_alpha                91.4680(9)
_cell_angle_beta                 95.3024(10)
_cell_angle_gamma                90.1840(11)
_cell_formula_units_Z            4
_cell_length_a                   6.1239(5)
_cell_length_b                   16.8945(12)
_cell_length_c                   17.8873(13)
_cell_measurement_reflns_used    7603
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.4
_cell_volume                     1842.1(2)
_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      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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      -0.0745462
_diffrn_orient_matrix_UB_12      0.0523270
_diffrn_orient_matrix_UB_13      -0.0060473
_diffrn_orient_matrix_UB_21      0.0064704
_diffrn_orient_matrix_UB_22      0.0070852
_diffrn_orient_matrix_UB_23      0.0558376
_diffrn_orient_matrix_UB_31      0.1459323
_diffrn_orient_matrix_UB_32      0.0267888
_diffrn_orient_matrix_UB_33      0.0002751
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27859
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_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^+1.1570P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6253
_reflns_number_total             7515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol503498n_si_003.cif
_cod_data_source_block           2546
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      P-1
_cod_database_code               1518719
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2012-9
_shelx_res_checksum              20737
_shelx_hkl_checksum              728