Building Large Structures with Curved Aromatic Surfaces by Complexing Metals with Phosphangulene.
Heskia, Alice; Maris, Thierry; Aguiar, Pedro M.; Wuest, James D.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b08179

data_4129099
_publ_section_title
;
 Building Large Structures with Curved Aromatic Surfaces by Complexing
 Metals with Phosphangulene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b08179
_journal_year                    2019
_chemical_formula_moiety         '2(C44 H26 Ag F3 O9 P2 S), 3(C7 H8), 2(C60)'
_chemical_formula_sum            'C229 H76 Ag2 F6 O18 P4 S2'
_chemical_formula_weight         3632.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                86.369(4)
_cell_angle_beta                 80.154(5)
_cell_angle_gamma                89.061(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1347(9)
_cell_length_b                   17.4030(14)
_cell_length_c                   20.810(2)
_cell_measurement_reflns_used    4900
_cell_measurement_temperature    150
_cell_measurement_theta_max      52.880
_cell_measurement_theta_min      2.814
_cell_volume                     3609.0(6)
_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 0.456
_diffrn_measured_fraction_theta_max 0.458
_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  0.0861
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.456
_diffrn_reflns_Laue_measured_fraction_max 0.458
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12677
_diffrn_reflns_point_group_measured_fraction_full 0.456
_diffrn_reflns_point_group_measured_fraction_max 0.458
_diffrn_reflns_theta_full        53.225
_diffrn_reflns_theta_max         53.225
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.197
_exptl_absorpt_correction_T_min  0.0809
_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 85272 reflections, Rint = 0.0861
 (57213 with I > 3sig(I), Rint = 0.0821)
;
_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    1.671
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1834
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1377
_refine_ls_number_reflns         12677
_refine_ls_number_restraints     1166
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.1053
_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^)+(0.1951P)^2^+5.3206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2958
_refine_ls_wR_factor_ref         0.3192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10127
_reflns_number_total             12677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_002.cif
_cod_data_source_block           jw21211
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4129099
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.493
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.550(4)
 0.450(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C4F-C7F
 1.55 with sigma of 0.02
 C3F-C7F \\sim C5F-C7F
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
C1F \\sim C2F \\sim C3F \\sim C4F \\sim C5F \\sim C6F \\sim C7F: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.02
C1E \\sim C2E \\sim C3E \\sim C4E \\sim C5E \\sim C6E \\sim C7E: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.02
C1H \\sim C2H \\sim C3H \\sim C4H \\sim C5H \\sim C6H \\sim C7H \\sim C8H \\sim
C9H \\sim C10H \\sim C11H \\sim C12H \\sim C13H \\sim C14H \\sim C15H \\sim
C16H \\sim C17H \\sim C18H \\sim C19H \\sim C20H \\sim C21H \\sim C22H \\sim
C23H \\sim C24H \\sim C25H \\sim C26H \\sim C27H \\sim C28H \\sim C29H \\sim
C30H \\sim C31H \\sim C32H \\sim C33H \\sim C34H \\sim C35H \\sim C36H \\sim
C37H \\sim C38H \\sim C39H \\sim C40H \\sim C41H \\sim C42H \\sim C43H \\sim
C44H \\sim C45H \\sim C46H \\sim C47H \\sim C48H \\sim C49H \\sim C50H \\sim
C51H \\sim C52H \\sim C53H \\sim C54H \\sim C55H \\sim C56H \\sim C57H \\sim
C58H \\sim C59H \\sim C60H: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02
5. Others
 Sof(C1H)=Sof(C2H)=Sof(C3H)=Sof(C4H)=Sof(C5H)=Sof(C6H)=Sof(C7H)=Sof(C8H)=
 Sof(C9H)=Sof(C10H)=Sof(C11H)=Sof(C12H)=Sof(C13H)=Sof(C14H)=Sof(C15H)=Sof(C16H)=
 Sof(C17H)=Sof(C18H)=Sof(C19H)=Sof(C20H)=Sof(C21H)=Sof(C22H)=Sof(C23H)=
 Sof(C24H)=Sof(C25H)=Sof(C26H)=Sof(C27H)=Sof(C28H)=Sof(C29H)=Sof(C30H)=
 Sof(C31H)=Sof(C32H)=Sof(C33H)=Sof(C34H)=Sof(C35H)=Sof(C36H)=Sof(C37H)=
 Sof(C38H)=Sof(C39H)=Sof(C40H)=Sof(C41H)=Sof(C42H)=Sof(C43H)=Sof(C44H)=
 Sof(C45H)=Sof(C46H)=Sof(C47H)=Sof(C48H)=Sof(C49H)=Sof(C50H)=Sof(C51H)=
 Sof(C52H)=Sof(C53H)=Sof(C54H)=Sof(C55H)=Sof(C56H)=Sof(C57H)=Sof(C58H)=
 Sof(C59H)=Sof(C60H)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=FVAR(1)
 Fixed Sof: C1F(0.5) H1F(0.5) C2F(0.5) H2F(0.5) C3F(0.5) H3F(0.5) C4F(0.5)
 C5F(0.5) H5F(0.5) C6F(0.5) H6F(0.5) C7F(0.5) H7FA(0.5) H7FB(0.5) H7FC(0.5)
6.a Free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,
 C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,
 C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,C51,C52,C53,C54,C55,C56,C57,C58,C59,
 C60), C1H(C2H,C3H,C4H,C5H,C6H,C7H,C8H,C9H,C10H,C11H,C12H,C13H,C14H,C15H,C16H,
 C17H,C18H,C19H,C20H,C21H,C22H,C23H,C24H,C25H,C26H,C27H,C28H,C29H,C30H,C31H,
 C32H,C33H,C34H,C35H,C36H,C37H,C38H,C39H,C40H,C41H,C42H,C43H,C44H,C45H,C46H,
 C47H,C48H,C49H,C50H,C51H,C52H,C53H,C54H,C55H,C56H,C57H,C58H,C59H,C60H)
6.b Me refined with riding coordinates:
 C7D(H7DA,H7DB,H7DC), C7E(H7EA,H7EB,H7EC), C7F(H7FA,H7FB,H7FC)
6.c Aromatic/amide H refined with riding coordinates:
 C1D(H1D), C2D(H2D), C3A(H3A), C3B(H3B), C3D(H3D), C4A(H4A), C4B(H4B),
 C5A(H5A), C5B(H5B), C5D(H5D), C6D(H6D), C9A(H9A), C9B(H9B), C10A(H10A),
 C10B(H10B), C11A(H11A), C11B(H11B), C15A(H15A), C15B(H15B), C16A(H16A),
 C16B(H16B), C17A(H17A), C17B(H17B), C2E(H2E), C3E(H3E), C4E(H4E), C5E(H5E),
 C6E(H6E), C1F(H1F), C2F(H2F), C3F(H3F), C5F(H5F), C6F(H6F)
6.d Fitted hexagon refined as free rotating group:
 C1E(C2E,C3E,C4E,C5E,C6E), C1F(C2F,C3F,C4F,C5F,C6F)
;
_shelx_res_checksum              96999
_shelx_hkl_checksum              69492
_olex2_submission_special_instructions 'No special instructions were received'