Chiral molecular face-rotating sandwich structures constructed through restricting the phenyl flipping of tetraphenylethylene.
Qu, Hang; Tang, Xiao; Wang, Xinchang; Li, Zhihao; Huang, Zheyu; Zhang, Hui; Tian, Zhongqun; Cao, Xiaoyu; Chemical science 9 (2018) 8814–8818; doi:10.1039/c8sc03404d

data_1549935
_publ_section_title
;
 Chiral molecular face-rotating sandwich structures constructed through
 restricting the phenyl flipping of tetraphenylethylene.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              8814
_journal_page_last               8818
_journal_paper_doi               10.1039/c8sc03404d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C114 H108 N16 O12'
_chemical_formula_sum            'C114 H108 N16 O12'
_chemical_formula_weight         1894.16
_chemical_melting_point          ?
_chemical_name_common            2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-17 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0205(3)
_cell_length_b                   20.3813(4)
_cell_length_c                   30.1755(5)
_cell_measurement_reflns_used    16748
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3760
_cell_measurement_theta_min      2.7370
_cell_volume                     11697.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -88.00 -30.00   0.50    0.50    --    0.00 -72.00-150.00  116
  2  \w    -67.00 -41.00   0.50    0.50    --    0.00 -19.00-120.00   52
  3  \w     -7.00  53.00   0.50    0.50    --    0.00  72.00-150.00  120
  4  \w    -16.00  12.00   0.50    0.50    --    0.00 -72.00-150.00   56
  5  \w    -55.00 -11.00   0.50    0.93    --  -98.80  72.00 -30.00   88
  6  \w   -120.00 -86.00   0.50    0.93    --  -98.80 -19.00-150.00   68
  7  \w   -110.00 -68.00   0.50    0.93    --  -98.80  72.00 -30.00   84
  8  \w   -185.00 -85.00   0.50    0.93    --  -98.80 -19.00 -60.00  200
  9  \w   -105.00 -16.00   0.50    0.93    --  -98.80  57.00 -30.00  178
 10  \w   -111.00 -16.00   0.50    0.93    --  -98.80  38.00  90.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026026000
_diffrn_orient_matrix_UB_12      -0.0451981000
_diffrn_orient_matrix_UB_13      -0.0408355000
_diffrn_orient_matrix_UB_21      0.0268807000
_diffrn_orient_matrix_UB_22      -0.0565829000
_diffrn_orient_matrix_UB_23      0.0292900000
_diffrn_orient_matrix_UB_31      -0.0764032000
_diffrn_orient_matrix_UB_32      -0.0216126000
_diffrn_orient_matrix_UB_33      0.0089010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            41067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.691
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         11538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+2.4632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9210
_reflns_number_total             11538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03404d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'Not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1549934--1549935.cif.
;
_cod_database_code               1549935
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C01K(H01A,H01C), C01L(H01G,H01I), C01O(H01K,H01L), C01P(H01O,H01P), C01R(H01Q,
 H01R), C01T(H01T,H01U), C01U(H01V,H01W), C01V(H01X,H01Y), C01W(H01Z,H),
 C01X(H01,HA), C01Y(H0AA,HB), C01Z(H1AA,HC)
2.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00W(H00W), C00X(H00X), C00Z(H00Z), C010(H010), C011(H011),
 C013(H013), C014(H014), C019(H019), C01B(H01B), C01D(H01D), C01E(H01E),
 C01F(H01F), C01H(H01H), C01J(H01J), C01M(H01M), C01N(H01N), C01S(H01S)
2.c Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003), O004(H004), O005(H005), O007(H007)
;
_shelx_res_checksum              28324
_shelx_fab_checksum              32050
_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 1.256
_oxdiff_exptl_absorpt_empirical_full_min 0.761