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_4127002
_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         'C130 H119 O P, C H Cl3'
_chemical_formula_sum            'C131 H120 Cl3 O P'
_chemical_formula_weight         1847.58
_chemical_name_systematic
;
Bis[5,8,11,14,17-penta(tert-butyl)hexa-peri-
hexabenzocoronen-2-yl]phenylphosphine oxide
;
_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                ntl1764_JNS-PA-60
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                112.906(6)
_cell_angle_beta                 94.953(6)
_cell_angle_gamma                96.491(6)
_cell_formula_units_Z            2
_cell_length_a                   13.7498(10)
_cell_length_b                   20.5393(13)
_cell_length_c                   24.0662(15)
_cell_measurement_reflns_used    5225
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.555
_cell_measurement_theta_min      3.711
_cell_volume                     6157.1(8)
_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    'SHELXS-2014/7 (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 0.995
_diffrn_measured_fraction_theta_max 0.941
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44478
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         75.904
_diffrn_reflns_theta_min         3.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.518
_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    0.997
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_preparation
;
Crystals were grown by layered diffusion of ethanol into a 
chloroform solution at RT. The crystals lost solvent over minutes 
so were rapidly mounted using Paratone N oil.
;
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         24172
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.1065
_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^)+(0.1932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2927
_refine_ls_wR_factor_ref         0.3619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10290
_reflns_number_total             24172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12251_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4127002
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.956
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              14906
_shelx_hkl_checksum              41960
_shelx_fab_checksum              5986