Functionalized O6-Corona[6]arenes: Synthesis, Structure, and Fullerene Complexation Property.
Ren, Wen-Sheng; Zhao, Liang; Wang, Mei-Xiang; Organic letters 18 (2016) 3126–3129; doi:10.1021/acs.orglett.6b01330

data_1543496
_publ_section_title
;
 Functionalized O6-Corona[6]arenes: Synthesis, Structure, and Fullerene
 Complexation Property.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3126
_journal_page_last               3129
_journal_paper_doi               10.1021/acs.orglett.6b01330
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C54 H48 O18, C4 H8 O2'
_chemical_formula_sum            'C58 H56 O20'
_chemical_formula_weight         1073.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.656(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7437(16)
_cell_length_b                   24.157(5)
_cell_length_c                   14.585(3)
_cell_measurement_reflns_used    7704
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4775
_cell_measurement_theta_min      1.3967
_cell_volume                     2727.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 13.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.2443
              2theta: -19.8665
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 13.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.2443
              2theta: -19.8665
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0197
_diffrn_orient_matrix_UB_12      -0.1040
_diffrn_orient_matrix_UB_13      0.0741
_diffrn_orient_matrix_UB_21      0.0378
_diffrn_orient_matrix_UB_22      -0.0045
_diffrn_orient_matrix_UB_23      -0.0163
_diffrn_orient_matrix_UB_31      0.0263
_diffrn_orient_matrix_UB_32      0.0384
_diffrn_orient_matrix_UB_33      0.0504
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22251
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         0.843
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2886 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11669
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0793
_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^)+(0.0656P)^2^+1.1889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                9755
_reflns_number_total             11669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b01330_si_001.cif
_cod_data_source_block           mx3562a
_cod_depositor_comments          'Adding full bibliography for 1543496.cif.'
_cod_original_cell_volume        2727.3(10)
_cod_database_code               1543496
_diffrn_number_total             6402
_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. Restrained distances
 C18A-C17A
 1.54 with sigma of 0.01
3. Others
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(O12A)=Sof(C32A)=Sof(H32C)=
 Sof(H32D)=1-FVAR(1)
 Sof(O12)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 FVAR(1)
 Sof(O10A)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=1-FVAR(2)
 Sof(O10)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C17(H17A,H17B), C32(H32A,H32B), C35(H35A,H35B), C50(H50A,
 H50B), C53(H53A,H53B), C57(H57A,H57B), C32A(H32C,H32D), C17A(H17C,H17D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C12(H12), C20(H20), C21(H21),
 C23(H23), C24(H24), C27(H27), C30(H30), C38(H38), C39(H39), C41(H41), C42(H42),
  C44(H44), C47(H47)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C33A(H33A,H33B,H33C), C36(H36A,H36B,
 H36C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C58(H58A,
 H58B,H58C), C33(H33D,H33E,H33F), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              98836
_shelx_hkl_checksum              31682
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'