Molecular Tectonics. Porous Hydrogen-Bonded Networks Built from Derivatives of 2,2',7,7'-Tetraphenyl-9,9'-spirobi[9H-fluorene]
Eric Demers; Thierry Maris; James D. Wuest; Cryst. Growth & Design 5 (2005) 1227–1235; doi:10.1021/cg049575o

data_4500074
_publ_section_title
;
 Molecular Tectonics. Porous Hydrogen-Bonded Networks Built from
 Derivatives of 2,2',7,7'-Tetraphenyl-9,9'-spirobi[9H-fluorene]
;
_journal_name_full               'Cryst. Growth & Design'
_journal_page_first              1227
_journal_page_last               1235
_journal_paper_doi               10.1021/cg049575o
_journal_volume                  5
_journal_year                    2005
_chemical_absolute_configuration unk
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         '2(C61 H44 N20), 14 (C2 H6 O S), 3 (H2 O)'
_chemical_formula_sum            'C150 H178 N40 O17 S14'
_chemical_formula_weight         3262.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                81.076(8)
_cell_angle_beta                 74.960(8)
_cell_angle_gamma                70.755(8)
_cell_formula_units_Z            1
_cell_length_a                   13.458(2)
_cell_length_b                   17.788(2)
_cell_length_c                   20.721(3)
_cell_measurement_reflns_used    345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.00
_cell_measurement_theta_min      5.20
_cell_volume                     4509.6(11)
_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    'SIR2000 (Burla et al, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_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  0.078
_diffrn_reflns_av_sigmaI/netI    0.0981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30221
_diffrn_reflns_theta_full        68.61
_diffrn_reflns_theta_max         68.61
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        -0.17
_diffrn_standards_interval_time  1440
_diffrn_standards_number         113
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  0.8500
_exptl_absorpt_correction_T_min  0.7900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1718
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_Flack   0.44(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1731
_refine_ls_number_reflns         15187
_refine_ls_number_restraints     729
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2289
_reflns_number_gt                9973
_reflns_number_total             15187
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw831
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4500074