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_4129093
_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(C26 H17 Ag F3 O6 P S)'
_chemical_formula_sum            'C52 H34 Ag2 F6 O12 P2 S2'
_chemical_formula_weight         1306.59
_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             2019-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.999(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.711(1)
_cell_length_b                   11.6334(6)
_cell_length_c                   20.2589(10)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    150
_cell_measurement_theta_max      57.200
_cell_measurement_theta_min      3.781
_cell_volume                     4942.5(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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.986
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60590
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.509
_diffrn_reflns_theta_min         1.833
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    5.754
_exptl_absorpt_correction_T_max  0.3709
_exptl_absorpt_correction_T_min  0.1917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1461 before and 0.0921 after correction. The Ratio of minimum to maximum transmission is 0.5169. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.641
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00024(5)
_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   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         10157
_refine_ls_number_restraints     519
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+15.8138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8289
_reflns_number_total             10157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_004.cif
_cod_data_source_block           jw2062
_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               4129093
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24B-C26B
 1.55 with sigma of 0.005
 C26B-C23B \\sim C26B-C25B
 with sigma of 0.02
 S1B-O4B \\sim S1B-O5B \\sim S1B-O6B
 with sigma of 0.005
 C19B-F2B \\sim C19B-F3B
 with sigma of 0.005
3. Restrained planarity
 C20B, C21B, C22B, C23B, C24B, C25B, C26B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim
C20B \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.02
S1B \\sim O4B \\sim O5B \\sim O6B \\sim C19B \\sim F1B \\sim F2B \\sim F3B
\\sim S1C \\sim O4C \\sim O5C \\sim O6C \\sim C19C \\sim F1C \\sim F2C \\sim
F3C: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(S1B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O6B)
\\sim Ueq, Uanis(C19B) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F2B) \\sim Ueq,
Uanis(F3B) \\sim Ueq, Uanis(S1C) \\sim Ueq, Uanis(O4C) \\sim Ueq, Uanis(O5C)
\\sim Ueq, Uanis(O6C) \\sim Ueq, Uanis(C19C) \\sim Ueq, Uanis(F1C) \\sim Ueq,
Uanis(F2C) \\sim Ueq, Uanis(F3C) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
5. Same fragment restrains
{S1A, O4A, O5A, O6A, C19A, F1A, F2A, F3A} sigma for 1-2: 0.005, 1-3: 0.04
as
{S1B, O4B, O5B, O6B, C19B, F1B, F2B, F3B}
{S1A, O4A, O5A, O6A, C19A, F1A, F2A, F3A} sigma for 1-2: 0.005, 1-3: 0.04
as
{S1C, O4C, O5C, O6C, C19C, F1C, F2C, F3C}
6. Others
 Sof(S1C)=Sof(O4C)=Sof(O5C)=Sof(O6C)=Sof(C19C)=Sof(F1C)=Sof(F2C)=Sof(F3C)=1-
 FVAR(1)
 Sof(S1B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C19B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=
 FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C9A(H9A), C10A(H10A), C11A(H11A), C15A(H15A),
 C16A(H16A), C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A),
 C25A(H25A), C3B(H3B), C4B(H4B), C5B(H5B), C9B(H9B), C10B(H10B), C11B(H11B),
 C15B(H15B), C16B(H16B), C17B(H17B), C20B(H20B), C21B(H21B), C22B(H22B),
 C23B(H23B), C25B(H25B)
7.b Fitted hexagon refined as free rotating group:
 C20A(C21A,C22A,C23A,C24A,C25A), C20B(C21B,C22B,C23B,C24B,C25B)
7.c Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F)
;
_shelx_res_checksum              67849
_shelx_hkl_checksum              69346
_olex2_submission_special_instructions 'No special instructions were received'