Construction of helical structures with planar chiral [2.2]paracyclophane: fusing helical and planar chiralities.
Tsuchiya, Motoki; Maeda, Hazuki; Inoue, Ryo; Morisaki, Yasuhiro; Chemical communications (Cambridge, England) 57 (2021) 9256–9259; doi:10.1039/d1cc03320d

data_7128874
_publ_section_title
;
 Construction of helical structures with planar chiral
 [2.2]paracyclophane: fusing helical and planar chiralities.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9256
_journal_page_last               9259
_journal_paper_doi               10.1039/d1cc03320d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C40 H32'
_chemical_formula_sum            'C40 H32'
_chemical_formula_weight         512.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.3890(2)
_cell_length_b                   21.6023(6)
_cell_length_c                   30.9026(8)
_cell_measurement_reflns_used    27724
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.3720
_cell_measurement_theta_min      2.2920
_cell_volume                     5600.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_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   -110.00  70.00   0.50   20.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   20.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50   20.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50   20.00    --  -20.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0044644000
_diffrn_orient_matrix_UB_12      0.0244221000
_diffrn_orient_matrix_UB_13      -0.0152970000
_diffrn_orient_matrix_UB_21      -0.0096687000
_diffrn_orient_matrix_UB_22      -0.0216179000
_diffrn_orient_matrix_UB_23      -0.0170732000
_diffrn_orient_matrix_UB_31      -0.0838731000
_diffrn_orient_matrix_UB_32      0.0037982000
_diffrn_orient_matrix_UB_33      0.0011576000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            109620
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.216
_diffrn_reflns_theta_min         1.997
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 2562 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.9(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         16867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0676
_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^)+(0.0402P)^2^+0.6192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                8550
_reflns_number_total             16867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03320d2.cif
_cod_data_source_block           20210529-t2'
_cod_depositor_comments
'Adding full bibliography for 7128869--7128874.cif.'
_cod_database_code               7128874
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H32
_reflns_odcompleteness_completeness 95.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.15
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C014(H01A,H01B), C018(H01C,H01D), C01F(H01N,H01P), C01K(H01F,
 H01H), C01P(H01V,H01X), C01X(H0AA,H), C01Y(H1AA,HA)
2.b Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C008(H008), C009(H009), C00A(H00C), C00D(H00D),
 C00F(H00F), C00H(H00H), C00J(H00J), C00L(H00L), C00Q(H00Q), C00S(H00S),
 C00U(H00U), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C015(H015), C019(H019), C01A(H01J), C01C(H01K), C01D(H01M),
 C01E(H01E), C01G(H01G), C01H(H01R), C01I(H01I), C01L(H01L), C01N(H01T),
 C01O(H01O), C01Q(H01Q), C01R(H01Y), C01S(H01S), C01T(H01Z), C01U(H01U),
 C01V(H01), C01W(H01W), C01Z(H2AA), C020(H020), C021(H021), C022(H022),
 C023(H023), C024(H024), C025(H025), C026(H026), C027(H027), C028(H028)
;
_shelx_res_checksum              23018
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id 20210531-T2'-Sp
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.808