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_4517251
_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         'C18 H9 O4 P, C6 H5 Cl, 1(C60)'
_chemical_formula_sum            'C84 H14 Cl O4 P'
_chemical_formula_weight         1153.37
_chemical_name_systematic
;
12cH-4,8,12-trioxa-12c-phosphadibenzo[cd,mn]pyren-12c-one 
C60 fullerene chlorobenzene solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.888(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0298(4)
_cell_length_b                   22.4623(8)
_cell_length_c                   10.1970(4)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    105
_cell_measurement_theta_max      60.272
_cell_measurement_theta_min      3.425
_cell_volume                     2280.73(15)
_computing_cell_refinement
;        
SAINT (2013) V8.34A; 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) V8.34A; 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    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      105
_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 0.992
_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  0.0778
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42649
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.750
_diffrn_reflns_theta_min         3.424
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.4146
_exptl_absorpt_correction_T_min  0.3021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction. 
wR2(int) was 0.1682 before and 0.0781 after correction. 
The Ratio of minimum to maximum transmission is 0.7287. 
The \l/2 correction factor is 0.00150.'
;
_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    1.679
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1164
_exptl_crystal_recrystallization_method 'crystallized in chlorobenzene'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1005
_refine_ls_number_reflns         8349
_refine_ls_number_restraints     2558
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.642
_reflns_Friedel_fraction_max     0.596
_reflns_number_gt                6150
_reflns_number_total             8349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw18092_phango_c60_phcl.cif
_cod_data_source_block           jw18092
_cod_database_code               4517251
_cod_database_fobs_code 4517251