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_7125196
_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         'C142 H130 Cl2 N6 Pd1'
_chemical_formula_sum            'C142 H130 Cl2 N6 Pd'
_chemical_formula_weight         2097.82
_chemical_name_common            '[PdCl2{Bn-tzl-HBC(tBu)5}2]'
_chemical_name_systematic
Dichlorobis(1-benzyl-4-[5,8,11,14,17-penta(tert-butyl)-2-hexa-peri-hexabenzocoronenyl]-1,2,3-triazole)palladium(II)
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                jrw_139
_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                90.00
_cell_angle_beta                 99.711(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0530(6)
_cell_length_b                   39.391(3)
_cell_length_c                   14.3467(6)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      72.7380
_cell_measurement_theta_min      3.8720
_cell_volume                     12284.3(11)
_computing_cell_refinement       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_collection       'CrysAlisPro (Agilent, V 1.171.36.28)'
_computing_data_reduction        'CrysAlisPro (Agilent, V 1.171.36.28)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.967
_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  0.1036
_diffrn_reflns_av_sigmaI/netI    0.1688
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            51510
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.86
_diffrn_reflns_theta_min         3.32
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.004
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.36.28
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_preparation
;
Crystals were grown by slow evaporation of a dichloromethane solution.
;
_exptl_crystal_size_max          0.2110
_exptl_crystal_size_mid          0.0612
_exptl_crystal_size_min          0.0287
_platon_squeeze_details
;
The contents of each region of disordered solvent could not be effectively 
modelled and have been treated as a diffuse contribution to the overall 
scattering using PLATON SQUEEZE (total: 2303 \A^3^/cell, 341 e/cell).
The electron count and volume of each void region is consistent with 
4 CH3CN and 8 H2O molecules, which give a total electron count 
of 168e/void and  total volume of 1096 \A^3^/void. 
;
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1390
_refine_ls_number_reflns         24388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                11339
_reflns_number_total             24388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc07413h2.cif
_cod_data_source_block           2b
_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 
;
_cod_original_cell_volume        12284.2(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7125196
_platon_squeeze_void_probe_radius 1.20