Suit[4]ane.
Liu, Wenqi; Stern, Charlotte L.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03408

data_4135030
_publ_section_title
;
 Suit[4]ane.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03408
_journal_year                    2020
_chemical_formula_moiety
'C96 H76 N8, C32 H20 Br2 N4, 8(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C132 H102 Br2 F48 N14 P8'
_chemical_formula_weight         3203.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.600(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.5852(9)
_cell_length_b                   21.9306(5)
_cell_length_c                   21.2989(7)
_cell_measurement_reflns_used    16288
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      32.7330
_cell_measurement_theta_min      2.1550
_cell_volume                     8442.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.933
_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    -48.00   4.00   0.50  178.93    --   24.71 -19.00  60.00  104
  2  \w    -41.00  38.00   0.50  178.93    --   24.71 -54.00 133.00  158
  3  \w      1.00  39.00   0.50  178.93    --   24.71-104.00  45.00   76
  4  \w    -87.00 -50.00   0.50  178.93    --  -25.33-178.00-120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0386851000
_diffrn_orient_matrix_UB_12      -0.0031452000
_diffrn_orient_matrix_UB_13      0.0221688000
_diffrn_orient_matrix_UB_21      0.0022938000
_diffrn_orient_matrix_UB_22      0.0309815000
_diffrn_orient_matrix_UB_23      0.0104179000
_diffrn_orient_matrix_UB_31      -0.0058928000
_diffrn_orient_matrix_UB_32      -0.0087393000
_diffrn_orient_matrix_UB_33      0.0289885000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44295
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       plate
_exptl_crystal_F_000             3228
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.996
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         19562
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.311
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.1002
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3196
_refine_ls_wR_factor_ref         0.3448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12728
_reflns_number_total             19562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03408_si_002.cif
_cod_data_source_block           cx1748
_cod_database_code               4135030
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C128H96Br2F48N12P8
_diffrn_oxdiff_digest_frames
;
0130920009b4496aa22408d1c377a0ae5f004125255
;
_diffrn_oxdiff_digest_hkl
;
01da822a5bf8f4ce6dc27cdb73692a0ebcb1c1
;
_reflns_odcompleteness_completeness 93.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P4-F19 \\sim P4-F19A
 with sigma of 0.02
 P4-F23 \\sim P4-F23A
 with sigma of 0.02
 P4-F20 \\sim P4-F20A
 with sigma of 0.02
 P4-F21 \\sim P4-F21A
 with sigma of 0.02
 P2-F9 \\sim P2-F9A
 with sigma of 0.02
 P2-F12 \\sim P2-F12A
 with sigma of 0.02
 P2-F11 \\sim P2-F11A
 with sigma of 0.02
 P2-F10 \\sim P2-F10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F9A \\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim
F12 \\sim F12A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=Sof(F23A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=Sof(F23)=FVAR(1)
 Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
 Fixed Sof: H5A(0.5) H6A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C18(H18A,H18B), C25(H25A,H25B), C42(H42A,H42B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C34(H34), C36(H36), C38(H38),
 C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C47(H47), C48(H48), N5(H5A),
 N6(H6A), C50(H50), C51(H51), C55(H55), C56(H56), C60(H60), C61(H61), C62(H62),
 C63(H63), C64(H64)
5.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              68124
_shelx_hkl_checksum              4714
_shelx_fab_checksum              25252
_olex2_date_sample_data_collection 2019-12-26
_olex2_date_sample_submission    2019-12-19
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id cx1748
_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 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.730