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_4500073
_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_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         '2(C61 H44 N20), 5(C2 H6 O S), 2.5(C H4 O)'
_chemical_formula_sum            'C134.5 H128 N40 O7.5 S5'
_chemical_formula_weight         2585.07
_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                93.026(3)
_cell_angle_beta                 94.690(4)
_cell_angle_gamma                96.419(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2162(10)
_cell_length_b                   21.2975(17)
_cell_length_c                   30.884(2)
_cell_measurement_reflns_used    5983
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      44.83
_cell_measurement_theta_min      2.46
_cell_volume                     7942.5(10)
_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    'SIR2000 (Burla et al., 2000)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'Bruker Smart 2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.1646
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            97194
_diffrn_reflns_theta_full        69.99
_diffrn_reflns_theta_max         69.99
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        -0.05
_diffrn_standards_interval_time  1440
_diffrn_standards_number         197
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_T_max  0.8730
_exptl_absorpt_correction_T_min  0.8010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2710
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1533
_refine_ls_number_reflns         25334
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0929
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                8975
_reflns_number_total             25334
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw624
_cod_original_cell_volume        7942.6(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C134.50 H128 N40 O7.50 S5'
_cod_database_code               4500073