The dipolar endofullerene HF@C60
Andrea Krachmalnicoff; Richard Bounds; Salvatore Mamone; Shamim Alom; Maria Concistre; Benno Meier; Karel Kouril; Mark E. Light; Mark R. Johnson; Stephane Rols; Anthony J. Horsewill; Anna Shugai; Urmas Nagel; Toomas Room; Marina Carravetta; Malcolm H. Levitt; Richard J. Whitby; Nature Chemistry 8 (2016) 953–957; doi:10.1038/nchem.2563

data_1551504
_publ_section_title
;
 The dipolar endofullerene HF@C60
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              953
_journal_page_last               957
_journal_paper_doi               10.1038/nchem.2563
_journal_volume                  8
_journal_year                    2016
_chemical_formula_moiety         'C60, 3/2(C S2), HF'
_chemical_formula_sum            'C61.5 H F S3'
_chemical_formula_weight         854.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90.22(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8867(6)
_cell_length_b                   25.5100(12)
_cell_length_c                   24.7353(14)
_cell_measurement_reflns_used    7838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.3030
_cell_measurement_theta_min      2.2360
_cell_volume                     6238.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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   -109.00  20.00   1.00   20.00    --  -19.00 -72.00  90.00  129
  2  \w    -93.00   7.00   1.00   20.00    --  -19.00 -36.00  30.00  100
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 FRE-VHF'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0009178000
_diffrn_orient_matrix_UB_12      -0.0219942000
_diffrn_orient_matrix_UB_13      0.0175033000
_diffrn_orient_matrix_UB_21      0.0088327000
_diffrn_orient_matrix_UB_22      -0.0169107000
_diffrn_orient_matrix_UB_23      -0.0225059000
_diffrn_orient_matrix_UB_31      0.0711785000
_diffrn_orient_matrix_UB_32      0.0017974000
_diffrn_orient_matrix_UB_33      0.0031524000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34980
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.942
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction 
using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416
_exptl_crystal_recrystallization_method
'The material was recrystallised from carbon disulfide by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         13735
_refine_ls_number_restraints     1647
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.0878
_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^)+(0.1058P)^2^+2.6236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7541
_reflns_number_total             13735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2563-s2.cif
_cod_data_source_block           2016sot0001_r_100k
_cod_depositor_comments
;

2022-04-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C123 H2 F2 S6'
_cod_original_formula_weight         1709.61
_cod_original_formula_moiety         '2(C60), 3(C S2), 2(HF)'
_cod_original_formula_units_Z            4
_cod_database_code               1551504
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6366(15) 0.3634(15)
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_shelx_res_checksum              73544
_shelx_hkl_checksum              71754