Single-crystal-to-single-crystal intercalation of a low-bandgap superatomic crystal
Evan S. O'Brien; M. Tuan Trinh; Rose L. Kann; Jia Chen; Giselle A. Elbaz; Amrita Masurkar; Timothy L. Atallah; Maria V. Paley; Nilam Patel; Daniel W. Paley; Ioannis Kymissis; Andrew C. Crowther; Andrew J. Millis; David R. Reichman; X.-Y. Zhu; Xavier Roy; Nature Chemistry 9 (2017) 1170–1174; doi:10.1038/nchem.2844

data_1551544
_publ_section_title
;
 Single-crystal-to-single-crystal intercalation of a low-bandgap
 superatomic crystal
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              1170
_journal_page_last               1174
_journal_paper_doi               10.1038/nchem.2844
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C54 H126 Co6 P6 Te8, 3(C60)'
_chemical_formula_sum            'C234 H126 Co6 P6 Te8'
_chemical_formula_weight         4497.54
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.9985(4)
_cell_length_b                   16.9985(4)
_cell_length_c                   55.6840(15)
_cell_measurement_reflns_used    10265
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.8330
_cell_measurement_theta_min      3.7620
_cell_volume                     13934.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1098
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0246088000
_diffrn_orient_matrix_UB_12      -0.0052605000
_diffrn_orient_matrix_UB_13      0.0095514000
_diffrn_orient_matrix_UB_21      -0.0054028000
_diffrn_orient_matrix_UB_22      0.0320155000
_diffrn_orient_matrix_UB_23      0.0069220000
_diffrn_orient_matrix_UB_31      -0.0410633000
_diffrn_orient_matrix_UB_32      -0.0356259000
_diffrn_orient_matrix_UB_33      0.0048077000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            39807
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        23.253
_diffrn_reflns_theta_max         23.253
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6594
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         2483
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0933
_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^)+(0.2000P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2857
_refine_ls_wR_factor_ref         0.3068
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1938
_reflns_number_total             2483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2844-s3.cif
_cod_data_source_block           desolvated
_cod_original_cell_volume        13934.2(7)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               1551544