New Insights into the Structural Complexity of C60·2S8: Two Crystal Morphologies, Two Phase Changes, Four Polymorphs
Ghiassi, Kamran B.; Chen, Susanne Y.; Wescott, Joseph; Balch, Alan L.; Olmstead, Marilyn M.; Crystal Growth & Design 15 (2015) 404–; doi:10.1021/cg501486x

data_4512409
_publ_section_title
;
 New Insights into the Structural Complexity of C60&#x00B7;2S8: Two
 Crystal Morphologies, Two Phase Changes, Four Polymorphs
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              404
_journal_paper_doi               10.1021/cg501486x
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C60, 2(S8)'
_chemical_formula_sum            'C60 S16'
_chemical_formula_weight         1233.56
_chemical_name_common            'C60 . 2 S8 (beta, 90 K)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                84.122(3)
_cell_angle_beta                 84.602(3)
_cell_angle_gamma                75.664(3)
_cell_formula_units_Z            4
_cell_length_a                   10.365(2)
_cell_length_b                   14.694(3)
_cell_length_c                   29.000(7)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.19
_cell_volume                     4245.9(16)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
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_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
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_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26115
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.522
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       lath
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         26115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+3.0541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23447
_reflns_number_total             26115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501486x_si_001.cif
_cod_data_source_block           kbg175
_cod_depositor_comments
'Adding full bibliography for 4512408--4512411.cif.'
_cod_original_cell_volume        4245.8(17)
_cod_database_code               4512409
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.509
_shelx_estimated_absorpt_t_max   0.781
_shelx_res_checksum              65335
_shelx_hkl_checksum              31043