Putting Fullerenes in Their Place: Cocrystallizing C60 and C70 with Phosphangulene Chalcogenides
Alice Heskia; Thierry Maris; James D. Wuest; Crystal growth and Design 19 (2019) 5418–; doi:10.1021/acs.cgd.9b00954

data_4517254
_publ_contact_author_email       thierry.maris@umontreal.ca
_publ_contact_author_id_orcid    0000-0001-9731-4046
_publ_contact_author_name        'Thierry Maris'
_publ_contact_author_phone       '514 340 4177 2579'
_publ_section_title
;
 Putting Fullerenes in Their Place: Cocrystallizing C60 and C70 with
 Phosphangulene Chalcogenides
;
_journal_name_full               'Crystal growth and Design'
_journal_page_first              5418
_journal_paper_doi               10.1021/acs.cgd.9b00954
_journal_volume                  19
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H9 O3 P S, C S2, C70'
_chemical_formula_sum            'C89 H9 O3 P S3'
_chemical_formula_weight         1253.11
_chemical_name_systematic
;
12cH-4,8,12-trioxa-12\L5-phosphadibenzo[cd,mn]pyrene-12c-thione 
C70 fullerene carbon disulfide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.153(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2521(15)
_cell_length_b                   14.4547(15)
_cell_length_c                   25.261(3)
_cell_measurement_reflns_used    7190
_cell_measurement_temperature    100
_cell_measurement_theta_max      55.026
_cell_measurement_theta_min      3.281
_cell_volume                     4838.9(9)
_computing_cell_refinement
;
SAINT (2013) V8.37A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2013) V8.37A; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1765
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_number            9747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.859
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  0.750824
_exptl_absorpt_correction_T_min  0.255513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1556 before and 0.1035 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1831 before and 0.1164 after correction.
 The Ratio of minimum to maximum transmission is 0.34.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 169457 reflections, Rint = 0.1765
 (89615 with I > 3sig(I), Rint = 0.1444)
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       Block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.272
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because
 only 0 suitable Friedel pairs available.
;
_refine_ls_abs_structure_Flack   0.32(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1730
_refine_ls_number_reflns         9738
_refine_ls_number_restraints     1621
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0926
_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^)+(0.1559P)^2^+10.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2402
_refine_ls_wR_factor_ref         0.2470
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                8708
_reflns_number_total             9738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw18803_phangs_c70_cs2.cif
_cod_data_source_block           jw18803
_cod_database_code               4517254
_cod_database_fobs_code 4517254