Exclusive Hydrophobic Self-Assembly of Adaptive Solid-State Networks of Octasubstituted 9,9'-Spirobifluorenes.
Pop, Lidia; Dumitru, Florina; Hădade, Niculina D; Legrand, Yves-Marie; van der Lee, Arie; Barboiu, Mihail; Grosu, Ion; Organic letters 17 (2015) 3494–3497; doi:10.1021/acs.orglett.5b01576

data_1555061
_publ_section_title
;
 Exclusive Hydrophobic Self-Assembly of Adaptive Solid-State Networks of
 Octasubstituted 9,9'-Spirobifluorenes.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3494
_journal_page_last               3497
_journal_paper_doi               10.1021/acs.orglett.5b01576
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C33 H20 N4 O4, C H2 Cl2'
_chemical_formula_sum            'C34 H22 Cl2 N4 O4'
_chemical_formula_weight         621.46
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6177(9)
_cell_length_b                   21.038(3)
_cell_length_c                   26.249(2)
_cell_measurement_reflns_used    2205
_cell_measurement_temperature    175
_cell_measurement_theta_max      27.0480
_cell_measurement_theta_min      1.9460
_cell_volume                     5863.4(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
  1 omega   -6.00   40.00   1.0000  368.4750
omega____ theta____ kappa____ phi______ frames
    -       16.3118   19.0000  -60.0000 46

  2 omega  -16.00   21.00   1.0000  368.4750
omega____ theta____ kappa____ phi______ frames
    -      -17.2493 -100.0000  -30.0000 37

  3 omega  -43.00   37.00   1.0000  368.4750
omega____ theta____ kappa____ phi______ frames
    -      -17.2493   19.0000 -150.0000 80

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0348401000
_diffrn_orient_matrix_UB_12      -0.0136584000
_diffrn_orient_matrix_UB_13      0.0203060000
_diffrn_orient_matrix_UB_21      0.0155456000
_diffrn_orient_matrix_UB_22      0.0262401000
_diffrn_orient_matrix_UB_23      0.0157414000
_diffrn_orient_matrix_UB_31      -0.0548878000
_diffrn_orient_matrix_UB_32      0.0160640000
_diffrn_orient_matrix_UB_33      -0.0084528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_av_unetI/netI     0.1351
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18989
_diffrn_reflns_theta_full        25.162
_diffrn_reflns_theta_max         29.259
_diffrn_reflns_theta_min         1.552
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'transparant yellow'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         2970
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.0002984
_refine_ls_shift/su_mean         0.0000328
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 -0.414 -9.97 -3.89 -3.85 -2.11 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0928
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0458
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                2970
_reflns_number_total             6887
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0780
_oxford_refine_ls_scale          0.6683(14)
_oxford_reflns_number_all        6884
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b01576_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        5863.4(5)
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               1555061
_cell_oxdiff_length_a            10.6112(8)
_cell_oxdiff_length_b            21.0711(18)
_cell_oxdiff_length_c            26.224(2)
_cell_oxdiff_angle_alpha         89.995(7)
_cell_oxdiff_angle_beta          90.038(6)
_cell_oxdiff_angle_gamma         90.053(6)
_cell_oxdiff_volume              5863.4(8)
_montpellier_reflns_maxres       0.97
_montpellier_reflns_completeness_maxres 99.89
_montpellier_reflns_redundancy_maxres 3.28