Palladium-catalyzed cocyclotrimerization of arynes with a pyramidalized alkene.
Alonso, José M; Quiroga, Sabela; Codony, Sandra; Turcu, Andreea L.; Barniol-Xicota, Marta; Pérez, Dolores; Guitián, Enrique; Vázquez, Santiago; Peña, Diego; Chemical communications (Cambridge, England) 54 (2018) 5996–5999; doi:10.1039/c8cc03188f

data_7121716
_publ_section_title
;
 Palladium-catalyzed cocyclotrimerization of arynes with a pyramidalized
 alkene.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5996
_journal_page_last               5999
_journal_paper_doi               10.1039/c8cc03188f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C34 H32, C H Cl3'
_chemical_formula_sum            'C35 H33 Cl3'
_chemical_formula_weight         559.96
_chemical_name_systematic        GR1JM537C
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-11-25T11:32:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-06-03 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                73.4435(14)
_cell_angle_beta                 72.2898(11)
_cell_angle_gamma                73.1598(11)
_cell_formula_units_Z            2
_cell_length_a                   9.5957(2)
_cell_length_b                   12.2865(3)
_cell_length_c                   13.2430(3)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.32
_cell_measurement_theta_min      2.29
_cell_measurement_wavelength     0.71073
_cell_volume                     1389.97(6)
_computing_cell_refinement       'SAINT V8.35A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      -0.029855
_diffrn_orient_matrix_UB_12      -0.032928
_diffrn_orient_matrix_UB_13      0.079718
_diffrn_orient_matrix_UB_21      0.028723
_diffrn_orient_matrix_UB_22      -0.080211
_diffrn_orient_matrix_UB_23      -0.014272
_diffrn_orient_matrix_UB_31      0.104278
_diffrn_orient_matrix_UB_32      -0.008169
_diffrn_orient_matrix_UB_33      0.00565
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.045
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63677
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.546
_diffrn_reflns_theta_min         1.653
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+0.1081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0
_reflns_number_gt                6099
_reflns_number_total             8507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03188f2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7121715--7121716.cif.'
_cod_original_cell_volume        1389.99(5)
_cod_database_code               7121716
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              46799
_shelx_hkl_checksum              96689