Carbon-rich "Click" 1,2,3-triazoles: hexaphenylbenzene and hexa-peri-hexabenzocoronene-based ligands for Suzuki-Miyaura catalysts.
Wright, James R.; Crowley, James D.; Lucas, Nigel T.; Chemical communications (Cambridge, England) 52 (2016) 12976–12979; doi:10.1039/c6cc07413h

data_7125197
_publ_section_title
;
 Carbon-rich &quot;Click&quot; 1,2,3-triazoles: hexaphenylbenzene and
 hexa-peri-hexabenzocoronene-based ligands for Suzuki-Miyaura catalysts.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12976
_journal_page_last               12979
_journal_paper_doi               10.1039/c6cc07413h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '2(C84 H83 Br2 N5 Pd1)'
_chemical_formula_sum            'C168 H166 Br4 N10 Pd2'
_chemical_formula_weight         2857.55
_chemical_name_common            '[PdBr2(iPr2-bimy){Bn-tzl-HBC(tBu5)}]'
_chemical_name_systematic
Dibromo(1,3-diisopropylbenzimidazol-2-ylidene){1-benzyl-4-(5,8,11,14,17-penta-tert-butylhexa-peri-hexabenzocoronenyl)-1H-1,2,3-triazole}palladium(II)
_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_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                jrw-319
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                97.6040(10)
_cell_angle_beta                 92.4960(10)
_cell_angle_gamma                92.4870(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6518(2)
_cell_length_b                   16.6609(2)
_cell_length_c                   33.4649(4)
_cell_measurement_reflns_used    36633
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      74.2510
_cell_measurement_theta_min      3.9080
_cell_volume                     8079.70(18)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.37.33)'
_computing_molecular_graphics    'Mercury (Macrae, 2016)'
_computing_publication_material  'enCIFer (CCDC, 2014)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_crystal_treatment
; 
Crystal was attached with Paratone N oil to a 0.3 mm CryoLoop supported 
in a copper mounting pin, then quenched in a cold nitrogen gas from a gas
stream from an Oxford Cryosystems Cryostream.
;
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            90409
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         3.93
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.330
_exptl_absorpt_correction_T_max  0.8003
_exptl_absorpt_correction_T_min  0.4451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.33
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2952
_exptl_crystal_preparation
;
The crystals were grown from a layered diffusion of methanol
into a dichloromethane solution of the compound at room temperature.
Crystals were visible after 2-3 days.
;
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
SQUEEZE identifies one void region per unit cell.
The contents of the void (total: 398 electrons, 1692 \%A3) were treated as 
a diffuse contribution to the overall scattering which could not be 
effectively modelled. The electron count and volume are consistent with 
22 methanol molecules, having with an electron count of 396 and volume of 
ca 1540 \%A3 per void.
;
_refine_diff_density_max         2.055
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1926
_refine_ls_number_reflns         32171
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+7.3757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                26439
_reflns_number_total             32171
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc07413h2.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               7125197