A chiral member of the family of organic hexameric cages.
Wierzbicki, M.; Głowacka, A A; Szymański, M P; Szumna, A.; Chemical communications (Cambridge, England) 53 (2017) 5200–5203; doi:10.1039/c7cc02245j

data_7120019
_publ_section_title
;
 A chiral member of the family of organic hexameric cages.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5200
_journal_page_last               5203
_journal_paper_doi               10.1039/c7cc02245j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C288 H336 N24 O48, 13.5(C7 H8)'
_chemical_formula_sum            'C382.5 H444 N24 O48'
_chemical_formula_weight         6145.59
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-03-22 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   36.9553(7)
_cell_length_b                   36.9553(7)
_cell_length_c                   119.924(3)
_cell_measurement_reflns_used    17159
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      68.6410
_cell_measurement_theta_min      3.7210
_cell_volume                     141837(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -79.00  -34.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -180.0000 45

  2 omega  -86.00  -35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 51

  3 omega   16.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   90.0000 27

  4 omega -131.00 -104.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.4132 -125.0000  -60.0000 27

  5 omega -126.00  -72.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.4132 -125.0000 -120.0000 54

  6 omega   30.00  102.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       57.4132  -94.0000   30.0000 72

  7 omega   29.00   94.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       57.4132  -94.0000 -150.0000 65

  8 omega   43.00  121.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       57.4132   61.0000  -90.0000 78

  9 omega   -4.00   23.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -       57.4132  -94.0000 -150.0000 27

 10 omega -146.00  -54.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -77.0000  -30.0000 92

 11 omega  101.00  176.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  104.0000  150.0000 75

 12 omega   38.00   89.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -37.0000 -180.0000 51

 13 omega   58.00   99.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -50.0000   30.0000 41

 14 omega   50.00  149.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -77.0000  150.0000 99

 15 omega   40.00   78.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -37.0000    0.0000 38

 16 omega   84.00  141.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264   50.0000  150.0000 57

 17 omega  110.00  167.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  104.0000  120.0000 57

 18 omega  102.00  141.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  104.0000 -180.0000 39

 19 omega  113.00  145.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -77.0000   30.0000 32

 20 omega   58.00   93.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -77.0000   30.0000 35

 21 omega   40.00   76.00   1.0000  134.0000
omega____ theta____ kappa____ phi______ frames
    -      114.8264  -37.0000  120.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0218839333
_diffrn_orient_matrix_UB_12      -0.0095143333
_diffrn_orient_matrix_UB_13      0.0095674667
_diffrn_orient_matrix_UB_21      0.0133332000
_diffrn_orient_matrix_UB_22      -0.0231718000
_diffrn_orient_matrix_UB_23      -0.0082238000
_diffrn_orient_matrix_UB_31      0.0407715333
_diffrn_orient_matrix_UB_32      0.0410556667
_diffrn_orient_matrix_UB_33      -0.0024227333
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -73
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       99
_diffrn_reflns_limit_l_min       -88
_diffrn_reflns_number            30276
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.214
_diffrn_reflns_theta_min         3.673
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.863
_exptl_crystal_F_000             39492
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1373
_refine_ls_number_reflns         30276
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1311P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10031
_reflns_number_total             30276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02245j2.cif
_cod_data_source_block           hexamer_3
_cod_depositor_comments          'Adding full bibliography for 7120019.cif.'
_cod_original_cell_volume        141838(6)
_cod_original_formula_sum        'C382.50 H444 N24 O48'
_cod_database_code               7120019
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C211-C212
 0.005 with sigma of 1.505
 C247-C241
 2.52 with sigma of 0.01
 C243-C241
 2.52 with sigma of 0.01
3. Restrained planarity
 C247, C242, C243, C241
 with sigma of 0.05
4. Rigid bond restraints
 C241, C242, C247, C246, C245
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C222, C223, C224, C225
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: H22A(0.5) H22B(0.5) H22C(0.5)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C13(H13), C31(H31), C33(H33), C51(H51), C53(H53), C71(H71),
 C73(H73), C91(H91), C93(H93), C111(H111), C113(H113), C131(H131), C133(H133),
 C151(H151), C153(H153)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C32(H32A,H32B), C52(H52A,H52B), C72(H72A,H72B), C92(H92A,
 H92B), C112(H11A,H11B), C132(H13A,H13B), C152(H15D,H15E)
6.c Me refined with riding coordinates:
 C241(H24A,H24B,H24C), C211(H21A,H21B,H21C), C201(H20A,H20B,H20C), C231(H23A,
 H23B,H23C), C221(H22A,H22B,H22C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C22(H22), C29(H29), C42(H42), C49(H49), C62(H62), C69(H69),
 C82(H82), C89(H89), C102(H102), C109(H109), C122(H122), C129(H129), C142(H142),
  C149(H149), C247(H247), C246(H246), C245(H245), C244(H244), C243(H243),
 C213(H213), C214(H214), C215(H215), C216(H216), C217(H217), C203(H203),
 C204(H204), C205(H205), C206(H206), C207(H207), C233(H233), C234(H234),
 C235(H235), C236(H236), C237(H237), C223(H223), C224(H224), C225(H225)
6.e Fitted hexagon refined as free rotating group:
 C242(C247,C246,C245,C244,C243), C212(C213,C214,C215,C216,C217)
6.f Tetrahedral OH refined with riding coordinates:
 O147(H147)
6.g Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C114(H11C,H11D,H11E),
 C115(H11F,H11G,H11H), C134(H13C,H13D,H13E), C135(H13F,H13G,H13H), C154(H15F,
 H15G,H15H), C155(H15I,H15J,H15K)
6.h Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8), O27(H27), O28(H28), O47(H47), O48(H48), O67(H67), O68(H68),
 O87(H87), O88(H88), O107(H107), O108(H108), O127(H127), O128(H128), O148(H148)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'