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_1555078
_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         'C29 H20 I4 O4'
_chemical_formula_sum            'C29 H20 I4 O4'
_chemical_formula_weight         940.09
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                60.520(7)
_cell_angle_beta                 87.603(6)
_cell_angle_gamma                86.921(7)
_cell_formula_units_Z            6
_cell_length_a                   12.1779(11)
_cell_length_b                   21.8512(15)
_cell_length_c                   21.9539(15)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    175
_cell_measurement_theta_max      24.5990
_cell_measurement_theta_min      1.9130
_cell_volume                     5077.5(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.763
_diffrn_measurement_details
;
  1 omega  -17.00   76.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -        5.4593   38.0000  -90.0000 93

  2 omega  -63.00   28.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -        5.4593  -38.0000   90.0000 91

  3 omega   19.00   46.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -        5.4593 -100.0000  120.0000 27

  4 omega  -61.00  -10.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -        5.4593  -38.0000  -30.0000 51

  5 omega    0.00   27.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -        5.4593  -38.0000  -30.0000 27

  6 omega  -23.00   32.00   1.0000  255.0000
omega____ theta____ kappa____ phi______ frames
    -       -6.1625 -100.0000  -30.0000 55

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0138886000
_diffrn_orient_matrix_UB_12      0.0289500000
_diffrn_orient_matrix_UB_13      -0.0329698000
_diffrn_orient_matrix_UB_21      0.0218381000
_diffrn_orient_matrix_UB_22      -0.0235508000
_diffrn_orient_matrix_UB_23      -0.0113366000
_diffrn_orient_matrix_UB_31      -0.0522984000
_diffrn_orient_matrix_UB_32      -0.0005569000
_diffrn_orient_matrix_UB_33      -0.0127645000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13664
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         1.845
_exptl_absorpt_coefficient_mu    3.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         4.71
_refine_diff_density_min         -2.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         9882
_refine_ls_number_restraints     322
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1138
_refine_ls_shift/su_max          0.0006390
_refine_ls_shift/su_mean         0.0000159
_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: 
 8.74 4.58 5.00 2.40 -0.804 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1501
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1235
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              24
_reflns_limit_k_min              -20
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                9882
_reflns_number_total             13664
_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   0.1138
_oxford_refine_ls_scale          0.4127(12)
_oxford_reflns_number_all        13582
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b01576_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2022-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C86 H56 I12 O12'
_cod_original_formula_weight         2804.11
_cod_original_formula_moiety         'C29 H20 I4 O4, C29 H19 I4 O4, C28 H17 I4 O4'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5077.5(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1555078
_cell_oxdiff_length_a            12.1750(10)
_cell_oxdiff_length_b            21.8460(15)
_cell_oxdiff_length_c            21.9487(14)
_cell_oxdiff_angle_alpha         60.522(7)
_cell_oxdiff_angle_beta          87.614(6)
_cell_oxdiff_angle_gamma         86.923(6)
_cell_oxdiff_volume              5074.0(6)
_montpellier_reflns_maxres       0.94
_montpellier_reflns_completeness_maxres 95.82
_montpellier_reflns_redundancy_maxres 2.51