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_4126997
_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         'C260 H238 Cl2 P2 Pd, 3(C H Cl3), C6H14'
_chemical_formula_sum            'C269 H255 Cl11 P2 Pd'
_chemical_formula_weight         4046.00
_chemical_name_systematic
;
trans-Dichlorobis{bis[5,8,11,14,17-penta(tert-butyl)hexa-peri-
hexabenzocoronen-2-yl]phenylphosphine}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                ntl1756_JNS-PA-38
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                76.185(2)
_cell_angle_beta                 76.758(2)
_cell_angle_gamma                82.901(2)
_cell_formula_units_Z            2
_cell_length_a                   17.3586(3)
_cell_length_b                   23.9116(4)
_cell_length_c                   31.8705(7)
_cell_measurement_reflns_used    26919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.010
_cell_measurement_theta_min      3.755
_cell_volume                     12471.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT-2014/5 (Sheldrick, 2014)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.959
_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  0.0805
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            179711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.860
_diffrn_reflns_theta_min         3.497
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            orange
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             4264
_exptl_crystal_preparation
;
Crystals were grown by vapour diffusion of hexane into a 
chloroform/CS2 solution at RT over 4-5 days. The crystals were 
mounted using Paratone N oil.
;
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2679
_refine_ls_number_reflns         49168
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.0911
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1609P)^2^+5.1850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27998
_reflns_number_total             49168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12251_si_003.cif
_cod_data_source_block           trans-PdCl2_2_2
_cod_database_code               4126997
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.880
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              88713
_shelx_hkl_checksum              25602
_shelx_fab_checksum              79773