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_1553184
_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         'C76 H19 N3 O5'
_chemical_formula_sum            'C76 H19 N3 O5'
_chemical_formula_weight         1053.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.060(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0600(8)
_cell_length_b                   13.2703(7)
_cell_length_c                   29.7423(18)
_cell_measurement_reflns_used    3762
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.3170
_cell_measurement_theta_min      3.3710
_cell_volume                     5134.6(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.699
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_details
;
  1 omega  -20.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -99.0000   60.0000 73

  2 omega  -81.00   13.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -57.0000  150.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0025364000
_diffrn_orient_matrix_UB_12      -0.0163830000
_diffrn_orient_matrix_UB_13      0.0227672000
_diffrn_orient_matrix_UB_21      -0.0078929000
_diffrn_orient_matrix_UB_22      -0.0504689000
_diffrn_orient_matrix_UB_23      -0.0073841000
_diffrn_orient_matrix_UB_31      0.0538730000
_diffrn_orient_matrix_UB_32      -0.0065506000
_diffrn_orient_matrix_UB_33      -0.0000107000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1193
_diffrn_reflns_av_unetI/netI     0.1636
_diffrn_reflns_Laue_measured_fraction_full 0.699
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13765
_diffrn_reflns_point_group_measured_fraction_full 0.699
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.816
_diffrn_reflns_theta_min         3.146
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60802
_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    1.363
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0005(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         6501
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0965
_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^)+(0.1101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1980
_refine_ls_wR_factor_ref         0.2328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3438
_reflns_number_total             6501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qo00265f2.cif
_cod_data_source_block           exp_5473-sr
_cod_original_cell_volume        5134.5(5)
_cod_database_code               1553184
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C75 H1 O3 N3'
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.966
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C59) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
Uanis(C10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C19(H19)
3.b Tetrahedral OH refined with riding coordinates:
 O4(H4), O5(H5A)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'