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_1555077
_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_absolute_configuration ad
_chemical_formula_moiety         ' 	C29 H20 N4 O12, C H2 Cl2 '
_chemical_formula_sum            'C30 H22 Cl2 N4 O12'
_chemical_formula_weight         701.42
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_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            4
_cell_length_a                   10.6627(3)
_cell_length_b                   10.6627(3)
_cell_length_c                   29.5381(18)
_cell_measurement_reflns_used    2513
_cell_measurement_temperature    175
_cell_measurement_theta_max      26.2900
_cell_measurement_theta_min      2.0010
_cell_volume                     3358.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SHELXT (Sheldrick, 2015)'
_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 0.877
_diffrn_measurement_details
;
  1 omega  -10.00   81.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -       16.6243   19.0000   90.0000 122

  2 omega  -79.00  -38.50   0.7500   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4056  139.0000    0.0000 54

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0576975000
_diffrn_orient_matrix_UB_12      -0.0077432000
_diffrn_orient_matrix_UB_13      0.0115908000
_diffrn_orient_matrix_UB_21      -0.0330405000
_diffrn_orient_matrix_UB_22      -0.0165104000
_diffrn_orient_matrix_UB_23      0.0199964000
_diffrn_orient_matrix_UB_31      0.0015227000
_diffrn_orient_matrix_UB_32      -0.0639351000
_diffrn_orient_matrix_UB_33      -0.0065848000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            5833
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         28.981
_diffrn_reflns_theta_min         1.910
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellow transparent'
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_platon_squeeze_details
;
;
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details 'Flack (1983), 1817 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.016(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4404
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.0012161
_refine_ls_shift/su_mean         0.0001158
_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: 
 1.78 1.91 1.11 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0978
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0848
_reflns_limit_h_max              10
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -39
_reflns_number_gt                4404
_reflns_number_total             5833
_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   0.0713
_oxford_refine_ls_scale          0.3168(9)
_oxford_reflns_number_all        5833
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b01576_si_004.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 43 '
_cod_original_formula_sum        ' C30 H22 Cl2 N4 O12	'
_cod_database_code               1555077
_cell_oxdiff_length_a            10.6653(6)
_cell_oxdiff_length_b            10.6686(4)
_cell_oxdiff_length_c            29.514(2)
_cell_oxdiff_angle_alpha         90.040(4)
_cell_oxdiff_angle_beta          89.931(6)
_cell_oxdiff_angle_gamma         90.018(4)
_cell_oxdiff_volume              3358.3(4)
_montpellier_reflns_maxres       0.79
_montpellier_reflns_completeness_maxres 99.72
_montpellier_reflns_redundancy_maxres 2.55