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_4512410
_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 (gamma, 293 K)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.302(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1733(9)
_cell_length_b                   15.8931(9)
_cell_length_c                   18.5781(10)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.23
_cell_volume                     4385.9(4)
_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      293(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 ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60195
_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         28.292
_diffrn_reflns_theta_min         2.234
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.868
_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         1.068
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1722
_refine_ls_number_reflns         10897
_refine_ls_number_restraints     20035
_refine_ls_restrained_S_all      0.681
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0702
_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^)+(0.1087P)^2^+9.9454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8471
_reflns_number_total             10897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501486x_si_001.cif
_cod_data_source_block           kbg145
_cod_depositor_comments
'Adding full bibliography for 4512408--4512411.cif.'
_cod_database_code               4512410
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.553
_shelx_estimated_absorpt_t_max   0.689
_exptl_absorpt_special_details
;
 Several crystals were examined for single-crystal X-ray diffraction
 studies. During the course of investigation, it was observed that the
 crystals were highly twinned. Upon cutting of the crystals, intensity
 was lost with little improvement in regard to eliminating the twin.
 Therefore, we selected the best single crystal, however large. The
 experimental absorption coefficient is 0.839 mm^-1^, thereby negating
 concerns of absorption.

 This system undergoes a phase change. This structure was collected at
 room temperature (293 K).
;
_shelx_res_checksum              96750
_shelx_hkl_checksum              44439