Open-cage fullerene with a stopper acts as a molecular vial for a single water molecule
Xu, Liang; Liang, Sisi; Sun, Jiahao; Gan, Liangbing; Organic Chemistry Frontiers 2 (2015) 1500–; doi:10.1039/C5QO00265F

data_1553185
_publ_section_title
;
 Open-cage fullerene with a stopper acts as a molecular vial for a single
 water molecule
;
_journal_issue                   11
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1500
_journal_paper_doi               10.1039/C5QO00265F
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C82 H27 N5 O5'
_chemical_formula_sum            'C82 H27 N5 O5'
_chemical_formula_weight         1162.08
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-11
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
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2015-07-22 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.87(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.987(3)
_cell_length_b                   18.451(4)
_cell_length_c                   19.171(4)
_cell_measurement_reflns_used    1131
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      20.2560
_cell_measurement_theta_min      3.3880
_cell_volume                     5624(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -22.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   77.0000 -150.0000 26

  2 omega  -15.00   10.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   38.0000   90.0000 25

  3 omega  -68.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -77.0000  120.0000 108

  4 omega   -8.00   17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -77.0000 -150.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0153074000
_diffrn_orient_matrix_UB_12      0.0074959000
_diffrn_orient_matrix_UB_13      -0.0407092000
_diffrn_orient_matrix_UB_21      0.0061271000
_diffrn_orient_matrix_UB_22      0.0375986000
_diffrn_orient_matrix_UB_23      0.0084394000
_diffrn_orient_matrix_UB_31      0.0414612000
_diffrn_orient_matrix_UB_32      -0.0028197000
_diffrn_orient_matrix_UB_33      0.0048054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1546
_diffrn_reflns_av_unetI/netI     0.3486
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22175
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.2279
_refine_ls_R_factor_gt           0.0870
_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^)+(0.0631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.2221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3261
_reflns_number_total             9720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00265f2.cif
_cod_data_source_block           exp_5250-sr
_cod_original_cell_volume        5625(2)
_cod_database_code               1553185
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 O1 N1'
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.991
_reflns_odcompleteness_completeness 97.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C18(H18), C19(H19),
 C26(H26), C27(H27), C28(H28), C29(H29), N1(H1), N2(H2)
2.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O4(H4), O5(H5)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'