Supramolecular assemblies of a nitrogen-embedded buckybowl dimer with C<sub>60</sub>.
Yokoi, Hiroki; Hiroto, Satoru; Sakamaki, Daisuke; Seki, Shu; Shinokubo, Hiroshi; Chemical science 9 (2018) 819–824; doi:10.1039/c7sc04453d

data_1548144
_publ_section_title
;
 Supramolecular assemblies of a nitrogen-embedded buckybowl dimer with
 C<sub>60</sub>.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              819
_journal_page_last               824
_journal_paper_doi               10.1039/c7sc04453d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C247.73 H123.18 N2'
_chemical_formula_weight         3127.42
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1579(2)
_cell_length_b                   37.8588(7)
_cell_length_c                   30.9277(5)
_cell_measurement_reflns_used    49186
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.6060
_cell_measurement_theta_min      1.7340
_cell_volume                     15316.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            130177
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.647
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6494
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and acetonitrile'
_exptl_crystal_size_max          0.695
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3503
_refine_ls_number_reflns         26953
_refine_ls_number_restraints     4422
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.1090
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1915P)^2^+27.5688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20125
_reflns_number_total             26953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04453d2.cif
_cod_data_source_block           yokoi160607-vm_a
_cod_depositor_comments
'Adding full bibliography for 1548144--1548145.cif.'
_cod_database_code               1548144
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              87982