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_7128870
_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         'C32 H28'
_chemical_formula_sum            'C32 H28'
_chemical_formula_weight         412.54
_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             2020-09-23
_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                 96.319(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7972(6)
_cell_length_b                   8.0733(3)
_cell_length_c                   18.9373(7)
_cell_measurement_reflns_used    10005
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.1760
_cell_measurement_theta_min      2.1570
_cell_volume                     2248.55(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.924
_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    5.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    5.00    --  -20.00  45.00  90.00  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      0.0445720000
_diffrn_orient_matrix_UB_12      0.0015754000
_diffrn_orient_matrix_UB_13      0.0180868000
_diffrn_orient_matrix_UB_21      -0.0180426000
_diffrn_orient_matrix_UB_22      0.0202886000
_diffrn_orient_matrix_UB_23      0.0320880000
_diffrn_orient_matrix_UB_31      -0.0034995000
_diffrn_orient_matrix_UB_32      -0.0854986000
_diffrn_orient_matrix_UB_33      0.0079478000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21741
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.170
_diffrn_reflns_theta_min         1.661
_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  0.62029
_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    1.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 3087 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.8(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12690
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.1482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                9411
_reflns_number_total             12690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03320d2.cif
_cod_data_source_block           20200122-motoki-heck-s
_cod_depositor_comments
'Adding full bibliography for 7128869--7128874.cif.'
_cod_database_code               7128870
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H28
_reflns_odcompleteness_completeness 92.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.10
_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:
 C015(H01A,H01B), C017(H01C,H01D), C01G(H01Q,H01R), C01H(H01F,H01G), C01J(H01T,
 H01U), C01O(H01X,H01Y), C01Q(H01Z,H), C01S(H01H,H01I)
2.b Aromatic/amide H refined with riding coordinates:
 C003(H003), C005(H005), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F),
 C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013),
 C014(H014), C016(H016), C018(H018), C019(H019), C01A(H01J), C01B(H01K),
 C01C(H01E), C01D(H01L), C01E(H01O), C01I(H01S), C01K(H01V), C01L(H01W),
 C01M(H01M), C01N(H01N), C01P(H01P), C01R(H01)
;
_shelx_res_checksum              7986
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id motoki-stilbene-S
_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 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.625