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_4517249
_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         '6(C18 H9 O4 P), C H4 O, 4(C60)'
_chemical_formula_sum            'C349 H58 O25 P6'
_chemical_formula_weight         4835.77
_chemical_name_common
;
sesquikis(12cH-4,8,12-trioxa-12c-phosphadibenzo[cd,mn]pyren-12c-one) 
C60 fullerene methanol solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.3952(9)
_cell_length_b                   13.3563(6)
_cell_length_c                   39.9166(19)
_cell_measurement_reflns_used    9121
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.733
_cell_measurement_theta_min      3.037
_cell_volume                     9779.5(8)
_computing_cell_refinement
;        
SAINT (2013) V8.38A; 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) V8.38A; 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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            146950
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.790
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1249 before and 0.0722 after correction. 
The Ratio of minimum to maximum transmission is 0.8893. 
The \l/2 correction factor is Not present.'
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4884
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.00083(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3199
_refine_ls_number_reflns         22467
_refine_ls_number_restraints     19340
_refine_ls_restrained_S_all      1.556
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.1280
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3899
_refine_ls_wR_factor_ref         0.4139
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                18020
_reflns_number_total             22467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw2107_phango_c60_meoh.cif
_cod_data_source_block           jw2107
_cod_database_code               4517249