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_7128872
_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_absolute_configuration syn
_chemical_formula_moiety         'C32 H24'
_chemical_formula_sum            'C32 H24'
_chemical_formula_weight         408.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-20 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.109(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2667(12)
_cell_length_b                   12.9527(18)
_cell_length_c                   9.9631(16)
_cell_measurement_reflns_used    1707
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.8170
_cell_measurement_theta_min      2.1010
_cell_volume                     1043.1(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      123
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.879
_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   40.00    --  -20.00  45.00   0.00  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      -0.0210115000
_diffrn_orient_matrix_UB_12      -0.0057469000
_diffrn_orient_matrix_UB_13      -0.0723521000
_diffrn_orient_matrix_UB_21      0.0024286000
_diffrn_orient_matrix_UB_22      -0.0544720000
_diffrn_orient_matrix_UB_23      0.0075666000
_diffrn_orient_matrix_UB_31      -0.0851881000
_diffrn_orient_matrix_UB_32      -0.0002130000
_diffrn_orient_matrix_UB_33      0.0023058000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5071
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.686
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.056
_diffrn_reflns_theta_min         2.091
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83619
_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    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             432
_exptl_crystal_recrystallization_method CH2Cl2/MeOH
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 680 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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4589
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0800
_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^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.501
_reflns_Friedel_fraction_full    0.694
_reflns_Friedel_fraction_max     0.476
_reflns_number_gt                2719
_reflns_number_total             4589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03320d2.cif
_cod_data_source_block           20200131-t1-r
_cod_depositor_comments
'Adding full bibliography for 7128869--7128874.cif.'
_cod_database_code               7128872
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H24
_reflns_odcompleteness_completeness 87.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.99
_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:
 C00H(H00A,H00C), C00O(H00D,H00F), C00U(H00G,H00H), C00V(H00I,H00J)
2.b Aromatic/amide H refined with riding coordinates:
 C001(H001), C004(H004), C006(H006), C007(H007), C009(H009), C00B(H00B),
 C00E(H00E), C00K(H00K), C00L(H00L), C00M(H00M), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00W(H00W)
;
_shelx_res_checksum              37548
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id motoki-T1-R
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.847