Superphenylphosphines: Nanographene-based Ligands That Control Coordination Geometry and Drive Supramolecular Assembly.
Smith, Jordan Neale; Hook, James M.; Lucas, Nigel T.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b12251

data_4126996
_publ_section_title
;
 Superphenylphosphines: Nanographene-based Ligands That Control
 Coordination Geometry and Drive Supramolecular Assembly.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12251
_journal_year                    2017
_chemical_formula_moiety         'C148 H134 Cl2 P2 Pd, 6(C H Cl3)'
_chemical_formula_sum            'C154 H140 Cl20 P2 Pd'
_chemical_formula_weight         2867.99
_chemical_name_systematic
;
trans-Dichlorobis{[5,8,11,14,17-penta(tert-butyl)hexa-peri-
hexabenzocoronen-2-yl]diphenylphosphine}palladium(II)
;
_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   geom
_audit_block_code                ntl1627_JNS-181
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                94.3330(10)
_cell_angle_beta                 103.992(2)
_cell_angle_gamma                101.5530(10)
_cell_formula_units_Z            2
_cell_length_a                   15.6602(3)
_cell_length_b                   17.6075(2)
_cell_length_c                   28.2455(5)
_cell_measurement_reflns_used    35358
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.109
_cell_measurement_theta_min      3.472
_cell_volume                     7340.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.37.33 (Rigaku OD, 2014)'
_computing_data_collection       'CrysAlisPro 1.171.37.33 (Rigaku OD, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.37.33 (Rigaku OD, 2014)'
_computing_molecular_graphics    'Mercury CSD 3.9 (CCDC, 2016)'
_computing_publication_material  'enCIFer 1.6 (CCDC, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0(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 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 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            66264
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.37.33 (Rigaku Oxford Diffraction, 2014)
Numerical absorption correction based on gaussian integration 
over a multifaceted crystal model. 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_preparation
;
Crystals were grown by vapour diffusion of petroleum ether into a 
chloroform solution at RT over 1 week. The crystals lost solvent over minutes 
becoming cloudy, then cracking. Fresh crystals were quickly mounted using 
Paratone N oil and cooled immediately in the cryostream at 100 K.
;
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.856
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1702
_refine_ls_number_reflns         29046
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1263P)^2^+29.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26419
_reflns_number_total             29046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12251_si_003.cif
_cod_data_source_block           trans-PdCl2_1_2
_cod_database_code               4126996
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.230
_shelx_estimated_absorpt_t_max   0.693
_shelx_res_checksum              57501
_shelx_hkl_checksum              91209
_shelx_fab_checksum              7244