Chelation-Assisted C-C Bond Activation of Biphenylene by Gold(I) Halides
Beucher, Helene; Schoergenhumer, Johannes; Merino, Estíbaliz; Nevado, Cristina; Chemical Science  (2021) –; doi:10.1039/D1SC03814A

data_1565054
_publ_section_title
;
 Chelation-Assisted C-C Bond Activation of Biphenylene by Gold(I) Halides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03814A
_journal_year                    2021
_chemical_formula_moiety         'C32 H12 B F24 1-, C34 H41 Cl P 1+'
_chemical_formula_sum            'C66 H53 B Cl F24 P'
_chemical_formula_weight         1379.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-25 deposited with the CCDC.	2021-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3246(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.60588(14)
_cell_length_b                   12.96449(11)
_cell_length_c                   25.8472(3)
_cell_measurement_reflns_used    27887
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.9610
_cell_measurement_theta_min      2.3580
_cell_volume                     6229.62(10)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.40.71a (Rigaku Oxford Diffraction, 2020)'
_computing_data_collection
'CrysAlisPro, Version 1.171.40.71a (Rigaku Oxford Diffraction, 2020)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.40.71a (Rigaku Oxford Diffraction, 2020)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2018 and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            'Atlas CCD area detector on \k goniostat'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle \k-geometry diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59306
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.056
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray source'
_exptl_absorpt_coefficient_mu    1.803
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model 
plus an empirical absorption correction using spherical harmonics, 
implemented in the SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         12308
_refine_ls_number_restraints     973
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1091P)^2^+7.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10634
_reflns_number_total             12308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03814a2.cif
_cod_data_source_block           NV2004
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565054
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.806
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              72732
_shelx_hkl_checksum              21468