Synthesis of an open-cage fullerene-based unidirectional H-bonding network and its coordination with titanium
Zhang, Hao; Su, Jie; Pan, Changwang; Lu, Xing; Gan, Liangbing; Organic Chemistry Frontiers 6 (2019) 1397–; doi:10.1039/C9QO00188C

data_1554770
_publ_section_title
;
 Synthesis of an open-cage fullerene-based unidirectional H-bonding
 network and its coordination with titanium
;
_journal_issue                   9
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1397
_journal_paper_doi               10.1039/C9QO00188C
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C70 H22.75 N O4.88 S2'
_chemical_formula_weight         1019.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-03 deposited with the CCDC.	2019-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4203(2)
_cell_length_b                   27.3088(4)
_cell_length_c                   10.35690(10)
_cell_measurement_reflns_used    16925
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.2940
_cell_measurement_theta_min      2.4570
_cell_volume                     4067.70(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26233
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.458
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             2083
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 3325 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         8361
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+2.4007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.795
_reflns_number_gt                7981
_reflns_number_total             8361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00188c2.cif
_cod_data_source_block           3_CCDC1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1554770
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              73618
_shelx_hkl_checksum              6759