Synthesis and Electrochemistry of Novel Dumbbell-Shaped Bis-pyrazolino[60]fullerene Derivatives Formed Using Microwave Radiation
BinSabt, Mohammad H.; Al-Matar, Hamad M.; Balch, Alan L.; Shalaby, Mona A.; ACS Omega  (2021) –; doi:10.1021/acsomega.1c02245

data_4518922
_publ_section_title
;
 Synthesis and Electrochemistry of Novel Dumbbell-Shaped
 Bis-pyrazolino[60]fullerene Derivatives Formed Using Microwave Radiation
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.1c02245
_journal_year                    2021
_chemical_formula_moiety         'C26 H22 N4 O'
_chemical_formula_sum            'C26 H22 N4 O'
_chemical_formula_weight         406.49
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.434(6)
_cell_angle_beta                 89.453(6)
_cell_angle_gamma                83.523(6)
_cell_formula_units_Z            2
_cell_length_a                   5.6471(7)
_cell_length_b                   9.3471(12)
_cell_length_c                   20.515(2)
_cell_measurement_reflns_used    3680
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      3.06
_cell_volume                     1073.9(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b46'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b46'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7387
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.014
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_min         3.054
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             428.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3718
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1544
_reflns_number_total             3718
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ao1c02245_si_002.cif
_cod_data_source_block           6b
_cod_database_code               4518922
_shelx_res_checksum              47275
_shelx_hkl_checksum              53223