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_1555080
_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         'C37 H24 O4, C H2 Cl2'
_chemical_formula_sum            'C38 H26 Cl2 O4'
_chemical_formula_weight         617.49
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 110.556(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2235(13)
_cell_length_b                   24.195(2)
_cell_length_c                   10.2868(12)
_cell_measurement_reflns_used    1453
_cell_measurement_temperature    175
_cell_measurement_theta_max      22.0430
_cell_measurement_theta_min      2.3380
_cell_volume                     3081.6(6)
_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    '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 0.999
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_details
;
  1 omega  -68.00   15.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7402  -57.0000 -120.0000 83

  2 omega  -40.00   17.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7402  -77.0000   30.0000 57

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0105254000
_diffrn_orient_matrix_UB_12      0.0247923000
_diffrn_orient_matrix_UB_13      -0.0298611000
_diffrn_orient_matrix_UB_21      0.0487364000
_diffrn_orient_matrix_UB_22      0.0035190000
_diffrn_orient_matrix_UB_23      0.0573459000
_diffrn_orient_matrix_UB_31      0.0281998000
_diffrn_orient_matrix_UB_32      -0.0152832000
_diffrn_orient_matrix_UB_33      -0.0352437000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7610
_diffrn_reflns_theta_full        17.166
_diffrn_reflns_theta_max         22.888
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89242
_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            colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         2518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.0003212
_refine_ls_shift/su_mean         0.0000203
_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: 
 3.68 -1.10 2.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0675
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0613
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                2518
_reflns_number_total             3178
_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   0.0653
_oxford_refine_ls_scale          0.949(3)
_oxford_reflns_number_all        3176
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b01576_si_005.cif
_cod_data_source_block           1
_cod_original_cell_volume        3081.6(4)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               1555080
_cell_oxdiff_length_a            13.2316(13)
_cell_oxdiff_length_b            24.178(3)
_cell_oxdiff_length_c            10.2929(11)
_cell_oxdiff_angle_alpha         89.984(9)
_cell_oxdiff_angle_beta          110.637(9)
_cell_oxdiff_angle_gamma         90.052(9)
_cell_oxdiff_volume              3081.6(5)
_montpellier_reflns_maxres       0.91
_montpellier_reflns_completeness_maxres 75.42
_montpellier_reflns_redundancy_maxres 2.37