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_4512411
_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 (delta, 90 K)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.283(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1355(6)
_cell_length_b                   15.7332(6)
_cell_length_c                   18.3535(7)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.26
_cell_volume                     4279.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (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 0.999
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            143892
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.531
_diffrn_reflns_theta_min         2.259
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       needle
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.480
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         28435
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0435P)^2^+2.5501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                27970
_reflns_number_total             28435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501486x_si_001.cif
_cod_data_source_block           kbg146
_cod_depositor_comments
'Adding full bibliography for 4512408--4512411.cif.'
_cod_database_code               4512411
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.683
_shelx_res_checksum              37318
_shelx_hkl_checksum              32146