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_4103736
_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         'C44 H38 N20,  4(C2 H6 O S), 2 (H2 O)'
_chemical_formula_sum            'C52 H66 N20 O6 S4'
_chemical_formula_weight         1195.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.318(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.706(2)
_cell_length_b                   14.9704(9)
_cell_length_c                   12.0264(7)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.74
_cell_measurement_theta_min      2.55
_cell_volume                     6246.8(6)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_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      150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.1463
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            82959
_diffrn_reflns_theta_full        58.85
_diffrn_reflns_theta_max         58.85
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        -0.17
_diffrn_standards_interval_time  1440
_diffrn_standards_number         193
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.8600
_exptl_absorpt_correction_T_min  0.7200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         8635
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                3792
_reflns_number_total             8835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jw1129
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4103736