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_1548145
_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            'C160 H94 N2'
_chemical_formula_weight         2044.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 100.4840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0175(8)
_cell_length_b                   28.9186(13)
_cell_length_c                   22.7929(10)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.9573
_cell_measurement_theta_min      2.2999
_cell_volume                     11029.6(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_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      113(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.1013
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75648
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.166
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform and hexane'
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 7797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4135
_refine_ls_number_reflns         34976
_refine_ls_number_restraints     6697
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0969
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1362P)^2^+10.9445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2411
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                23428
_reflns_number_total             34976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc04453d2.cif
_cod_data_source_block           yokoi170905d8y_0m_c_sqd_sqd
_cod_depositor_comments
;

2019-07-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1548144--1548145.cif.
;
_cod_original_formula_sum        'C320 H188 N4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     4088.73
_cod_database_code               1548145
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              3503