Chiral cyclic [n]spirobifluorenylenes: carbon nanorings consisting of helically arranged quaterphenyl rods illustrating partial units of woven patterns
Zhu, Kaige KZ; Kamochi, Kosuke KK; Kodama, Takuya; Tobisu, Mamoru; Amaya, Toru; Chemical Science  (2020) –; doi:10.1039/D0SC02452J

data_1558858
_publ_section_title
;
 Chiral cyclic [n]spirobifluorenylenes: carbon nanorings consisting of
 helically arranged quaterphenyl rods illustrating partial units of woven
 patterns
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02452J
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C50 H28'
_chemical_formula_sum            'C50 H28'
_chemical_formula_weight         628.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc24v72b
_audit_creation_date             2020-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-13 deposited with the CCDC.	2020-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.6264(2)
_cell_length_b                   30.0390(4)
_cell_length_c                   26.9101(4)
_cell_measurement_reflns_used    16823
_cell_measurement_temperature    123
_cell_measurement_theta_max      73.8010
_cell_measurement_theta_min      3.3460
_cell_volume                     9398.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -44.00  31.00   0.50    2.99    --  -42.93  76.00 -61.00  150
  2  \w     74.00 115.00   0.50    2.99    --   42.93 125.00  30.00   82
  3  \w     72.00 106.00   0.50    2.99    --   42.93 125.00 -30.00   68
  4  \w     22.00  91.00   0.50    2.99    --   42.93  57.00-150.00  138
  5  \w    -86.00 -32.00   0.50   11.97    -- -106.00  76.00 -61.00  108
  6  \w    -84.00 -28.00   0.50   11.97    -- -106.00  37.00 -90.00  112
  7  \w    -95.00 -34.00   0.50   11.97    -- -106.00 125.00 -30.00  122
  8  \w    -89.00 -32.00   0.50   11.97    -- -106.00 125.00-120.00  114
  9  \w   -104.00 -74.00   0.50   11.97    -- -106.00 122.00-177.00   60
 10  \w   -135.00 -34.00   0.50   11.97    -- -106.00  77.00-150.00  202
 11  \w   -117.00 -36.00   0.50   11.97    -- -106.00 125.00   0.00  162
 12  \w   -118.00 -84.00   0.50   11.97    -- -106.00 151.00 -16.00   68
 13  \w   -128.00 -90.00   0.50   11.97    -- -106.00  37.00 -90.00   76
 14  \w   -177.00 -98.00   0.50   11.97    -- -106.00 -45.00 -32.00  158
 15  \w   -110.00 -85.00   0.50   11.97    -- -106.00 -99.00-120.00   50
 16  \w   -116.00 -53.00   0.50    2.99    --  -42.93-151.00 -60.00  126
 17  \w   -135.00-105.00   0.50   11.97    -- -106.00 -99.00  30.00   60
 18  \w   -177.00-148.00   0.50   11.97    -- -106.00 -37.00  30.00   58
 19  \w   -174.00 -92.00   0.50   11.97    -- -106.00-125.00-120.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.259
_diffrn_reflns_theta_min         3.285
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.889
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 and MeOH'
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 3350 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   4.51(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0619
_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^)+(0.1282P)^2^+5.2459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.1999
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                8305
_reflns_number_total             9367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02452j2.cif
_cod_data_source_block           190426_kz_ssss
_cod_database_code               1558858
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00A), C00G(H00G), C00M(H00M), C00P(H00P), C00R(H00R),
 C00T(H00T), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C016(H016),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I)
;
_shelx_res_checksum              87969
_shelx_fab_checksum              3705
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;