Switchable Cyclopalladation of Substrates Containing Two Directing Groups: on the Way to Non-symmetrical [2.2]-Dipalladaparacyclophanes
Korábková, Tereza; Bartáček, Jan; Marek, Lukáš; Hanusek, Jiri; R°užička, Aleš; Váňa, Jiří; Dalton Transactions  (2023) –; doi:10.1039/D3DT02019C

data_7713465
_publ_section_title
;
 Switchable Cyclopalladation of Substrates Containing Two Directing
 Groups: on the Way to Non-symmetrical [2.2]-Dipalladaparacyclophanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02019C
_journal_year                    2023
_chemical_formula_moiety         'C6 H19 B9 O2'
_chemical_formula_sum            'C6 H19 B9 O2'
_chemical_formula_weight         220.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc247jpm
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-12-21 deposited with the CCDC.	2023-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.494(3)
_cell_length_b                   11.359(5)
_cell_length_c                   13.096(5)
_cell_measurement_reflns_used    12334
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1263.5(9)
_computing_cell_refinement       'APEX3 v2016.9-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12334
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.374
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.143
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 917 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0501P)^2^+0.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2487
_reflns_number_total             2895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02019c2.cif
_cod_data_source_block           jhl180918O1_1
_cod_original_cell_volume        1263.6(8)
_cod_database_code               7713465
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.892
;
_shelxl_version_number           2013-4
_shelx_res_checksum              85571