Synthesis of modified fullerenes for oxygen reduction reactions
María Girón, Rosa; Marco-Martínez, Juan; Bellani, Sebastiano; Insuasty, Alberto; Comas Rojas, Hansel; Tullii, Gabriele; Antognazza, Maria Rosa; Filippone, Salvatore; Martín, Nazario; Journal of Materials Chemistry A 4 (2016) 14284–; doi:10.1039/C6TA06573B

data_7236348
_publ_section_title
;
 Synthesis of modified fullerenes for oxygen reduction reactions
;
_journal_issue                   37
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              14284
_journal_paper_doi               10.1039/C6TA06573B
_journal_volume                  4
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C80 H23 Cl1 Ir1 N1 O2'
_chemical_formula_sum            'C80 H23 Cl Ir N O2'
_chemical_formula_weight         1257.64
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-22T11:48:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2013-09-12 deposited with the CCDC.
2016-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.7078(6)
_cell_length_b                   34.7078(6)
_cell_length_c                   18.0586(3)
_cell_measurement_reflns_used    7627
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8964
_cell_measurement_theta_min      2.5441
_cell_measurement_wavelength     0.71073
_cell_volume                     21754.0(6)
_computing_cell_refinement
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_collection
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_data_reduction
'CrysAlis Pro (Oxford Diffraction Ltd., 2011)'
_computing_molecular_graphics    'Diamond v.3.2f (Crystal Impact GbR, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov et al, 2010)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -87.00  -46.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756 -168.0000  -41.0000 41

  2 omega  -40.00   54.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756  -19.0000   90.0000 94

  3 omega   30.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  150.0000 39

  4 omega   38.00   68.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -90.0000 30

  5 omega   30.00   63.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  120.0000 33

  6 omega   33.00   62.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000   60.0000 29

  7 omega   82.00  150.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000 -150.0000 68

  8 omega   39.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000 -150.0000 27

  9 omega   31.00   56.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000  -60.0000 25

 10 omega  -93.00   -3.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5756  125.0000  -60.0000 90

 11 omega   33.00   98.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756 -125.0000  150.0000 65

 12 omega   14.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5756   38.0000  -90.0000 90

 13 omega  -64.00  -14.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   45.0000  -30.0000 50

 14 omega   43.00  108.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000 -150.0000 65

 15 omega   55.00  104.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  150.0000 49

 16 omega   31.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -120.0000 38

 17 omega  120.00  145.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000   90.0000 25

 18 omega   32.00   59.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -30.0000 -180.0000 27

 19 omega   49.00  125.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   15.0000   90.0000 76

 20 omega   49.00  106.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000  -60.0000 57

 21 omega   78.00  112.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  125.0000   90.0000 34

 22 omega   78.00  151.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   61.0000  -90.0000 73

 23 omega   39.00  117.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -61.0000  -30.0000 78

 24 omega   57.00  106.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -94.0000   90.0000 49

 25 omega   40.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000   90.0000 32

 26 omega   90.00  131.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609   45.0000 -180.0000 41

 27 omega   34.00   60.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609  -45.0000 -180.0000 26

 28 omega   83.00  122.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      108.3609 -125.0000   60.0000 39

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0205191
_diffrn_orient_matrix_UB_12      0.0370506
_diffrn_orient_matrix_UB_13      0.0256291
_diffrn_orient_matrix_UB_21      -0.0225337
_diffrn_orient_matrix_UB_22      -0.0234135
_diffrn_orient_matrix_UB_23      0.0581437
_diffrn_orient_matrix_UB_31      0.032221
_diffrn_orient_matrix_UB_32      0.0072178
_diffrn_orient_matrix_UB_33      0.056933
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1488
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            86819
_diffrn_reflns_theta_full        72.46
_diffrn_reflns_theta_max         72.46
_diffrn_reflns_theta_min         2.55
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.636
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             9920
_exptl_crystal_size_max          0.2544
_exptl_crystal_size_mid          0.0197
_exptl_crystal_size_min          0.0161
_refine_diff_density_max         1.646
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         10773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                6872
_reflns_number_total             10773
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ta06573b2.cif
_cod_data_source_block           jmba103
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_database_code               7236348