Pentalenes with novel topologies: exploiting the cascade carbopalladation reaction between alkynes and gem-dibromoolefins
London, Gábor; von Wantoch Rekowski, Margarete; Dumele, Oliver; Schweizer, W. Bernd; Gisselbrecht, Jean-Paul; Boudon, Corinne; Diederich, François; Chemical Science 5 (2014) 965–; doi:10.1039/c3sc52623b

data_1513670
_publ_section_title
;
 Pentalenes with novel topologies: exploiting the cascade carbopalladation
 reaction between alkynes and gem-dibromoolefins
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              965
_journal_paper_doi               10.1039/c3sc52623b
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C39 H38 O2 Si1'
_chemical_formula_sum            'C39 H38 O2 Si'
_chemical_formula_weight         566.78
_space_group_IT_number           2
_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-97
_cell_angle_alpha                85.804(18)
_cell_angle_beta                 87.160(19)
_cell_angle_gamma                66.309(15)
_cell_formula_units_Z            4
_cell_length_a                   14.703(15)
_cell_length_b                   14.833(16)
_cell_length_c                   15.051(16)
_cell_measurement_reflns_used    1330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.27
_cell_measurement_theta_min      5.70
_cell_volume                     2997(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Platon, Ortep'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement
'OLEX2 (Dolomanov, 2009), SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2188
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            8295
_diffrn_reflns_theta_full        23.49
_diffrn_reflns_theta_max         23.49
_diffrn_reflns_theta_min         5.71
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_correction_T_min  0.9866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         8295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.2153
_refine_ls_R_factor_gt           0.1187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3035
_refine_ls_wR_factor_ref         0.3506
_reflns_number_gt                3970
_reflns_number_total             8295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52623b.txt
_cod_data_source_block           d081112_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C39 H38 O2 Si1'
_cod_database_code               1513670