O6-Corona[6]arenes with Expanded Cavities for Specific Complexation with C70.
Lu, Yao; Fu, Zhan-Da; Guo, Qing-Hui; Wang, Mei-Xiang; Organic letters 19 (2017) 1590–1593; doi:10.1021/acs.orglett.7b00409

data_1545961
_publ_section_title
;
 O6-Corona[6]arenes with Expanded Cavities for Specific Complexation with
 C70.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1590
_journal_page_last               1593
_journal_paper_doi               10.1021/acs.orglett.7b00409
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C57 H42 N6 O6, 3(C H2 Cl2)'
_chemical_formula_sum            'C60 H48 Cl6 N6 O6'
_chemical_formula_weight         1161.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                105.366(5)
_cell_angle_beta                 101.194(5)
_cell_angle_gamma                101.131(3)
_cell_formula_units_Z            2
_cell_length_a                   11.034(4)
_cell_length_b                   13.836(5)
_cell_length_c                   19.748(7)
_cell_measurement_reflns_used    7922
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4802
_cell_measurement_theta_min      1.5801
_cell_volume                     2754.9(17)
_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  'CIFTAB (Sheldrick, 2013)'
_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 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 40.0421
              2theta: -20.2618
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 40.0421
              2theta: -20.2618
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 40.0421
              2theta: -20.2618
;
_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      -0.0573
_diffrn_orient_matrix_UB_12      -0.0305
_diffrn_orient_matrix_UB_13      -0.0703
_diffrn_orient_matrix_UB_21      -0.0320
_diffrn_orient_matrix_UB_22      -0.0653
_diffrn_orient_matrix_UB_23      0.0271
_diffrn_orient_matrix_UB_31      -0.0504
_diffrn_orient_matrix_UB_32      0.0115
_diffrn_orient_matrix_UB_33      0.0169
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37321
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.107
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         12602
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0876
_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^)+(0.0634P)^2^+2.2783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8981
_reflns_number_total             12602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00409_si_005.cif
_cod_data_source_block           mx4159
_cod_original_cell_volume        2754.8(16)
_cod_database_code               1545961
_diffrn_number_total             12603
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl4A \\sim C0AA \\sim C0AB \\sim Cl3A \\sim Cl3: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C0AA) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl3A)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(H02C)=Sof(H02D)=Sof(Cl6A)=Sof(Cl5A)=1-FVAR(1)
 Sof(Cl5)=Sof(Cl6)=Sof(H02B)=Sof(H02A)=FVAR(1)
 Sof(Cl3A)=Sof(C0AB)=Sof(H0AC)=Sof(H0AD)=Sof(Cl4A)=1-FVAR(2)
 Sof(Cl3)=Sof(Cl4)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C025(H02E,
 H02F), C0AA(H0AA,H0AB), C026(H02B,H02A), C026(H02C,H02D), C0AB(H0AC,H0AD)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19),
 C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38),
  C47(H47), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57)
;
_shelx_res_checksum              67618
_shelx_hkl_checksum              95352
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'