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_7128873
_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         'C26 H27 Br O4'
_chemical_formula_sum            'C26 H27 Br O4'
_chemical_formula_weight         483.38
_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             2019-11-22
_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                 91.457(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1381(3)
_cell_length_b                   7.2746(2)
_cell_length_c                   16.3470(5)
_cell_measurement_reflns_used    8246
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1720
_cell_measurement_theta_min      2.4840
_cell_volume                     1086.33(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.918
_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    0.50    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    0.50    --  -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      -0.0541726000
_diffrn_orient_matrix_UB_12      0.0274762000
_diffrn_orient_matrix_UB_13      0.0278217000
_diffrn_orient_matrix_UB_21      0.0550960000
_diffrn_orient_matrix_UB_22      0.0141311000
_diffrn_orient_matrix_UB_23      0.0307193000
_diffrn_orient_matrix_UB_31      0.0076834000
_diffrn_orient_matrix_UB_32      0.0924250000
_diffrn_orient_matrix_UB_33      -0.0129635000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10203
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.160
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70232
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       needle
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 2290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.828
_reflns_number_gt                5699
_reflns_number_total             6149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03320d2.cif
_cod_data_source_block           20191121maeda-ms
_cod_depositor_comments
'Adding full bibliography for 7128869--7128874.cif.'
_cod_database_code               7128873
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H27O4Br
_reflns_odcompleteness_completeness 91.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.09
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00C), C00J(H00D,H00E), C00L(H00H,H00I), C00N(H00N,H00O), C00S(H00T,
 H00U), C00U(H00V,H00W)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00F(H00F), C00G(H00G), C00K(H00K), C00Q(H00Q)
2.c Idealised Me refined as rotating group:
 C00M(H00J,H00L,H00M), C00R(H00P,H00R,H00S), C00V(H00X,H00Y,H)
;
_shelx_res_checksum              45652
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id '20191121maeda mS'
_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 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.594