Shape-selective crystallisation of fluxional carbon cages.
Bismillah, Aisha N.; Sturala, Jiri; Chapin, Brette M.; Yufit, Dmitry S.; Hodgkinson, Paul; McGonigal, Paul R.; Chemical science 9 (2018) 8631–8636; doi:10.1039/c8sc04303e

data_1550087
_publ_section_title
;
 Shape-selective crystallisation of fluxional carbon cages.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              8631
_journal_page_last               8636
_journal_paper_doi               10.1039/c8sc04303e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C21 H16 F2 O'
_chemical_formula_sum            'C21 H16 F2 O'
_chemical_formula_weight         322.34
_chemical_name_systematic
;
(+/-)1,9-Bis(4-fluorophenyl)tricyclo[3.3.1.0^2,8^]nona-3,6-dien-9-ol
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-23 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.602(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8240(5)
_cell_length_b                   6.3040(4)
_cell_length_c                   25.0331(18)
_cell_measurement_reflns_used    2121
_cell_measurement_temperature    370(2)
_cell_measurement_theta_max      25.2050
_cell_measurement_theta_min      2.4330
_cell_volume                     1550.23(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      370.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    6.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029   77.0000    0.0000 98

  2 omega   59.00   85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029  178.0000   30.0000 26

  3 omega   56.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029  178.0000  150.0000 50

  4 omega   44.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029   77.0000  150.0000 28

  5 omega    9.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029 -100.0000  120.0000 64

  6 omega  -19.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029 -100.0000 -120.0000 96

  7 omega  -39.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9029    0.0000 -150.0000 128
;
_diffrn_measurement_device       'Xcalibur, Sapphire3'
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0370685000
_diffrn_orient_matrix_UB_12      0.0657660000
_diffrn_orient_matrix_UB_13      -0.0176870000
_diffrn_orient_matrix_UB_21      -0.0600131000
_diffrn_orient_matrix_UB_22      0.0173652000
_diffrn_orient_matrix_UB_23      -0.0153450000
_diffrn_orient_matrix_UB_31      -0.0154331000
_diffrn_orient_matrix_UB_32      0.0896252000
_diffrn_orient_matrix_UB_33      0.0159563000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'sealed tubeEnhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2158
_reflns_number_total             4124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04303e2.cif
_cod_data_source_block           1b_370k
_cod_depositor_comments
'Adding full bibliography for 1550083--1550094.cif.'
_cod_original_cell_volume        1550.22(17)
_cod_database_code               1550087
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C21 H16 F2 O1'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C21(H21), C15(H15), C5(H5), C18(H18), C7(H7), C11(H11),
 C20(H20), C8(H8), C14(H14), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'