Synthesis and 83Kr NMR Spectroscopy of Kr@C60
Hoffman, Gabriela; Bacanu, George Razvan; Marsden, Elizabeth S.; Walkey, Mark C.; Sabba, Mohamed; Bloodworth, Sally; Tizzard, Graham J.; Levitt, Malcolm H.; Whitby, Richard J.; Chemical Communications  (2022) –; doi:10.1039/D2CC03398D

data_7130702
_publ_section_title
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 Synthesis and 83Kr NMR Spectroscopy of Kr@C60
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03398D
_journal_year                    2022
_chemical_formula_moiety         'Kr, C60, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C108 H56 Kr N4 Ni'
_chemical_formula_weight         1552.07
_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             2020-12-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-01-13 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                87.620(2)
_cell_angle_beta                 75.874(2)
_cell_angle_gamma                75.664(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1170(3)
_cell_length_b                   14.3635(4)
_cell_length_c                   17.2002(4)
_cell_measurement_reflns_used    27963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1930
_cell_measurement_theta_min      1.9100
_cell_volume                     3276.23(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -97.00  22.00   0.50    6.00    --   -8.10 -38.00 -30.00  238
  2  \w    -97.00  21.00   0.50    6.00    --   -8.10 -57.00 120.00  236
  3  \w    -97.00  22.00   0.50    6.00    --   -8.10 -60.00-120.00  238
  4  \w    -84.00  53.00   0.50    6.00    --    5.00 -19.00  90.00  274
  5  \w    -38.00  74.00   0.50    6.00    --   -8.10  60.00 -30.00  224
  6  \w    -38.00  81.00   0.50    6.00    --   -8.10  38.00 -90.00  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0018094000
_diffrn_orient_matrix_UB_12      -0.0450618000
_diffrn_orient_matrix_UB_13      -0.0164478000
_diffrn_orient_matrix_UB_21      -0.0203892000
_diffrn_orient_matrix_UB_22      0.0237507000
_diffrn_orient_matrix_UB_23      -0.0314116000
_diffrn_orient_matrix_UB_31      0.0493651000
_diffrn_orient_matrix_UB_32      -0.0020641000
_diffrn_orient_matrix_UB_33      -0.0234903000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.654
_diffrn_reflns_theta_min         1.843
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method 'The material was as supplied'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         20140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0348P)^2^+3.9486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15700
_reflns_number_total             20140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03398d2.cif
_cod_data_source_block           Kr@C60
_cod_database_code               7130702
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C108 H106 Kr N4 Ni '
_chemical_oxdiff_usercomment     GS/610?Kr@60
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.782
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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:
 C121(H12A,H12B), C123(H12F,H12G), C125(H12K,H12L), C127(H12P,H12Q), C129(H12U,
 H12V), C131(H13D,H13E), C133(H13I,H13J), C135(H13N,H13O)
2.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C107(H107), C112(H112), C117(H117), C201(H201), C202(H202),
 C203(H203), C204(H204), C205(H205), C206(H206), C301(H301), C302(H302),
 C303(H303), C304(H304), C305(H305), C306(H306)
2.c Idealised Me refined as rotating group:
 C122(H12C,H12D,H12E), C124(H12H,H12I,H12J), C126(H12M,H12N,H12O), C128(H12R,
 H12S,H12T), C130(H13A,H13B,H13C), C132(H13F,H13G,H13H), C134(H13K,H13L,H13M),
 C136(H13P,H13Q,H13R)
;
_shelx_res_checksum              84028
_shelx_hkl_checksum              24440
_olex2_date_sample_data_collection 2020-12-11
_olex2_date_sample_submission    2020-12-10
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id GS/610/Kr@60
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.929
_oxdiff_exptl_absorpt_empirical_full_min 0.648