Bis(phosphangulene)iminium Salts. Holding on to Fullerenes with Phangs
Alice Heskia; Thierry Maris; James D. Wuest; Cryst. Growth & Design 20 (2020) 1319–1327; doi:10.1021/acs.cgd.9b01568

data_4517398
_publ_section_title
;
 Bis(phosphangulene)iminium Salts. Holding on to Fullerenes with Phangs
;
_journal_name_full               'Cryst. Growth & Design'
_journal_page_first              1319
_journal_page_last               1327
_journal_paper_doi               10.1021/acs.cgd.9b01568
_journal_volume                  20
_journal_year                    2020
_chemical_formula_moiety
'4(C36 H18 N O6 P2), Ag4 Br8, 2(C6 H5 Cl), H2 O'
_chemical_formula_sum            'C156 H84 Ag4 Br8 Cl2 N4 O25 P8'
_chemical_formula_weight         3803.69
_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             2019-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.837(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9625(5)
_cell_length_b                   16.9936(5)
_cell_length_c                   25.4614(8)
_cell_measurement_reflns_used    5504
_cell_measurement_temperature    150
_cell_measurement_theta_max      59.206
_cell_measurement_theta_min      3.042
_cell_volume                     6842.2(4)
_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)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.977
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            100896
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.189
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    6.142
_exptl_absorpt_correction_T_max  0.3397
_exptl_absorpt_correction_T_min  0.1839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 146895 reflections, Rint = 0.0674
 (90089 with I > 3sig(I), Rint = 0.0611)
;
_exptl_crystal_colour            'clear light Colorless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       needle
_exptl_crystal_F_000             3740
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15154
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0638
_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^)+(0.1068P)^2^+17.6897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12256
_reflns_number_total             15154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jw20712___Phang_2N_4_Ag4Br8_PhCl.cif
_cod_data_source_block           jw20712
_cod_database_code               4517398
_cod_database_fobs_code 4517398