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_4129102
_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         'C25 H17 Ag Cl O7 P'
_chemical_formula_sum            'C25 H17 Ag Cl O7 P'
_chemical_formula_weight         603.67
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.495(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8082(7)
_cell_length_b                   16.1007(9)
_cell_length_c                   12.8381(7)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    150
_cell_measurement_theta_max      54.975
_cell_measurement_theta_min      2.388
_cell_volume                     2314.7(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.028
_diffrn_reflns_theta_min         3.859
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    6.153
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1157 before and 0.0830 after correction. The Ratio of minimum to maximum transmission is 0.6841. 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    1.732
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.0094(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   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0980P)^2^+4.7038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4135
_reflns_number_total             4417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08179_si_012.cif
_cod_data_source_block           jw20462
_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               4129102
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.578
_shelx_estimated_absorpt_t_min   0.358
_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
 C3C-C7C = C2D-C7D
 1.52 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim
C16A \\sim C17A \\sim C18A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.02
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim
C16B \\sim C17B \\sim C18B: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.02
C1C \\sim C2C \\sim C3C \\sim C4C \\sim C5C \\sim C6C \\sim C7C \\sim C1D \\sim
C2D \\sim C3D \\sim C4D \\sim C5D \\sim C6D \\sim C7D: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.02
4. Others
 Sof(P1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=
 Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(C7B)=Sof(C8B)=Sof(C9B)=
 Sof(H9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(C13B)=Sof(C14B)=
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=1-FVAR(1)
 Sof(P1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=
 Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=FVAR(1)
 Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(C3D)=Sof(H3D)=Sof(C4D)=Sof(H4D)=Sof(C5D)=
 Sof(H5D)=Sof(C6D)=Sof(H6D)=Sof(C7D)=Sof(H7DA)=Sof(H7DB)=Sof(H7DC)=1-FVAR(2)
 Sof(C1C)=Sof(H1C)=Sof(C2C)=Sof(H2C)=Sof(C3C)=Sof(C4C)=Sof(H4C)=Sof(C5C)=
 Sof(H5C)=Sof(C6C)=Sof(H6C)=Sof(C7C)=Sof(H7CA)=Sof(H7CB)=Sof(H7CC)=FVAR(2)
5.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), C3B(H3B), C4B(H4B), C5B(H5B), C9B(H9B), C10B(H10B),
 C11B(H11B), C15B(H15B), C16B(H16B), C17B(H17B), C1C(H1C), C2C(H2C), C4C(H4C),
 C5C(H5C), C6C(H6C), C1D(H1D), C3D(H3D), C4D(H4D), C5D(H5D), C6D(H6D)
5.b Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C7A(C8A,C9A,C10A,C11A,C12A), C13A(C14A,C15A,C16A,
 C17A,C18A), C1B(C2B,C3B,C4B,C5B,C6B), C7B(C8B,C9B,C10B,C11B,C12B), C13B(C14B,
 C15B,C16B,C17B,C18B), C1C(C2C,C3C,C4C,C5C,C6C), C1D(C2D,C3D,C4D,C5D,C6D)
5.c Idealised Me refined as rotating group:
 C7C(H7CA,H7CB,H7CC), C7D(H7DA,H7DB,H7DC)
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_shelx_res_checksum              5587
_shelx_hkl_checksum              46291
_olex2_submission_special_instructions 'No special instructions were received'