Engineering Hydrogen-Bonded Molecular Crystals Built from Derivatives of Hexaphenylbenzene and Related Compounds
Kenneth E. Maly; Thierry Maris; James D. Wuest; J. Am. Chem. Soc. 129 (2007) 4306–4322; doi:10.1021/ja067571x

data_4103737
_publ_section_title
;
 Engineering Hydrogen-Bonded Molecular Crystals Built from Derivatives of
 Hexaphenylbenzene and Related Compounds
;
_journal_name_full               'J. Am. Chem. Soc.'
_journal_page_first              4306
_journal_page_last               4322
_journal_paper_doi               10.1021/ja067571x
_journal_volume                  129
_journal_year                    2007
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety
'C60 H48 N30, 7(C4 H8 O), 9(C2 H6 O S), 3(H2 O)'
_chemical_formula_sum            'C106 H164 N30 O19 S9'
_chemical_formula_weight         2451.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.400(6)
_cell_angle_beta                 110.518(5)
_cell_angle_gamma                103.475(6)
_cell_formula_units_Z            2
_cell_length_a                   17.770(2)
_cell_length_b                   21.235(3)
_cell_length_c                   21.691(2)
_cell_measurement_reflns_used    6587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.37
_cell_measurement_theta_min      2.27
_cell_volume                     7217.9(15)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker AXS Smart 4K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55733
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  1440
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_T_max  0.8800
_exptl_absorpt_correction_T_min  0.7300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.018
_refine_diff_density_min         -0.049
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1398
_refine_ls_number_reflns         23987
_refine_ls_number_restraints     290
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.1160
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2902
_refine_ls_wR_factor_ref         0.2974
_reflns_number_gt                9075
_reflns_number_total             23987
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw817
_cod_original_cell_volume        7217.9(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4103737