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_1549934
_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            1
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 94.091(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0567(5)
_cell_length_b                   14.2086(3)
_cell_length_c                   28.6868(6)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6850
_cell_measurement_theta_min      4.3780
_cell_volume                     10593.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.953
_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     25.00  98.00   1.00   10.00    --   40.84-125.00 -30.00   73
  2  \w     25.00 134.00   1.00   25.00    --  102.39 -77.00 -30.00  109
  3  \w     72.00 147.00   1.00   25.00    --  102.39  30.00  90.00   75
  4  \w     94.00 177.00   1.00   25.00    --  102.39 125.00   0.00   83
  5  \w     72.00 176.00   1.00   25.00    --  102.39  61.00 120.00  104
  6  \w   -115.00 -13.00   1.00   10.00    --  -40.84 -57.00 150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0323272000
_diffrn_orient_matrix_UB_12      0.0845554000
_diffrn_orient_matrix_UB_13      0.0186158000
_diffrn_orient_matrix_UB_21      -0.0497254000
_diffrn_orient_matrix_UB_22      0.0562999000
_diffrn_orient_matrix_UB_23      0.0059268000
_diffrn_orient_matrix_UB_31      -0.0015351000
_diffrn_orient_matrix_UB_32      -0.0377942000
_diffrn_orient_matrix_UB_33      0.0501400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34160
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.900
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         19489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0757P)^2^+5.3557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14107
_reflns_number_total             19489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03404d2.cif
_cod_data_source_block           1
_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               1549934
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         chno
_reflns_odcompleteness_completeness 98.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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:
 C02U(H02c,H02h), C02W(H02k,H02l), C034(H03a,H03b), C037(H03c,H03d), C03D(H03g,
 H03h), C03G(H03j,H03k), C03H(H03l,H03m), C03J(H03o,H03p), C03M(H03s,H03t),
 C03N(H03u,H03v), C03O(H03w,H03x), C03P(H03y,H), C03R(H03z,Ha), C03S(H03,Hb),
 C03T(H0aa,Hc), C03U(H1aa,Hd), C03V(H2aa,He), C03W(H3aa,Hf), C03X(H4aa,Hg),
 C03Z(H6aa,Hh), C040(H04a,H04b), C042(H04c,H04d), C043(H04e,H04f), C044(H04g,
 H04h)
2.b Aromatic/amide H refined with riding coordinates:
 C012(H012), C014(H014), C015(H015), C01B(H01B), C01D(H01D), C01I(H01I),
 C01L(H01L), C01M(H01M), C01Q(H01Q), C01U(H01U), C01V(H01V), C01X(H01X),
 C01Y(H01Y), C01Z(H01Z), C022(H022), C023(H023), C024(H024), C026(H026),
 C027(H027), C02A(H02A), C02B(H02B), C02D(H02D), C02E(H02E), C02F(H02F),
 C02G(H02G), C02I(H02I), C02J(H02J), C02M(H02M), C02O(H02O), C02P(H02P),
 C02Q(H02Q), C02R(H02R), C02T(H02T), C02V(H02V), C02X(H02X), C02Y(H02Y),
 C032(H032), C033(H033), C036(H036), C039(H039), C03A(H03e), C03C(H03f),
 C03F(H03i), C03I(H03n), C03K(H03q), C03L(H03r), C03Y(H5aa), C041(H041)
2.c Idealised tetrahedral OH refined as rotating group:
 O004(H004), O005(H005), O006(H006), O007(H007), O008(H008), O009(H009),
 O00A(H00A), O00B(H00B), O00C(H00C), O00D(H00D), O00F(H00F), O00H(H00H)
;
_shelx_res_checksum              62580
_shelx_fab_checksum              87287
_olex2_submission_original_sample_id 'FRSs 1'
_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.798