Potassium salt promoted regioselective three-component coupling synthesis of 1,4-asymmetrical [60]fullerene bisadducts with superior electron transport properties.
Li, Fei; Shang, Yanbo; Niu, Chuang; Li, Chao; Huang, Xinmin; Xu, Guoyong; Xuan, Jun; Zhou, Hongping; Yang, Shangfeng; Chemical communications (Cambridge, England) 56 (2020) 9513–9516; doi:10.1039/d0cc03857a

data_7126810
_publ_section_title
;
 Potassium salt promoted regioselective three-component coupling synthesis
 of 1,4-asymmetrical [60]fullerene bisadducts with superior electron
 transport properties.
;
_journal_issue                   66
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9513
_journal_page_last               9516
_journal_paper_doi               10.1039/d0cc03857a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C81 H19 Cl O'
_chemical_formula_sum            'C81 H19 Cl O'
_chemical_formula_weight         1043.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-05 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                76.859(15)
_cell_angle_beta                 76.555(14)
_cell_angle_gamma                72.955(13)
_cell_formula_units_Z            2
_cell_length_a                   10.0045(17)
_cell_length_b                   14.860(3)
_cell_length_c                   16.494(3)
_cell_measurement_reflns_used    22165
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.79
_cell_measurement_theta_min      4.56
_cell_volume                     2246.5(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'DECTRIS PILATUS 300K'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.873
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16530
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.787
_diffrn_reflns_theta_min         4.564
_exptl_absorpt_coefficient_mu    0.517
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.071
_exptl_crystal_description       needle
_exptl_crystal_F_000             48
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         7084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0805
_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^)+(0.1474P)^2^+1.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4702
_reflns_number_total             7084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03857a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
          Adding full bibliography for 7126810.cif.

2025-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C H Cl O S'
_cod_original_formula_weight         96.53
_cod_original_formula_moiety         '2(C81 H19 Cl O)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2246.4(7)
_cod_database_code               7126810
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00U(H00D,H00E), C018(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00F(H00F), C00R(H00R), C00Y(H00Y), C012(H012), C013(H013),
 C014(H014), C015(H015), C017(H017), C019(H019), C01K(H01K), C022(H022)
2.c Idealised Me refined as rotating group:
 C004(H00A,H00B,H00C)
;
_shelx_res_checksum              25605
_shelx_hkl_checksum              64885
_shelx_fab_checksum              78176
_olex2_submission_special_instructions 'No special instructions were received'