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_4517252
_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_formula_moiety         'C60, 3(C18 H9 O4 P), 3(C8 H10)'
_chemical_formula_sum            'C138 H57 O12 P3'
_chemical_formula_weight         1999.74
_chemical_name_systematic
;
tris(12cH-4,8,12-trioxa-12c-phosphadibenzo[cd,mn]pyren-12c-one) 
C60 fullerene 1,2-xylene solvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 119.1907(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1567(14)
_cell_length_b                   13.6785(7)
_cell_length_c                   27.0976(13)
_cell_measurement_reflns_used    4493
_cell_measurement_temperature    100
_cell_measurement_theta_max      60.678
_cell_measurement_theta_min      2.801
_cell_volume                     8787.4(8)
_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  'XL (Sheldrick, 2008)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.990
_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  0.1068
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39117
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.794
_diffrn_reflns_theta_min         1.621
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1318 before and 0.0870 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 0.1445 before and 0.0772 after correction.
 The Ratio of minimum to maximum transmission is 0.67.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 178590 reflections, Rint = 0.1068
 (103128 with I > 3sig(I), Rint = 0.0920)
;
_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    1.512
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.968
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00082(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1378
_refine_ls_number_reflns         39117
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.1029
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1882P)^2^+11.8920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3189
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                30259
_reflns_number_total             39117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw18722_phango_c60_oxylene.cif
_cod_data_source_block           jw18722
_cod_database_code               4517252