Positive thermal expansion facilitates the formation of argentophilic forces following an order–disorder phase transition
Juneja, Navkiran; Unruh, Daniel K.; Groeneman, Ryan H.; Hutchins, Kristin M.; New Journal of Chemistry 45 (2021) 8898–8901; doi:10.1039/D1NJ00312G

data_7060651
_publ_section_title
;
 Positive thermal expansion facilitates the formation of argentophilic
 forces following an order--disorder phase transition
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8898
_journal_page_last               8901
_journal_paper_doi               10.1039/D1NJ00312G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C27 H22 Ag F3 N2 O3 S'
_chemical_formula_sum            'C27 H22 Ag F3 N2 O3 S'
_chemical_formula_weight         619.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-01-13 deposited with the CCDC.	2021-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.635(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6960(7)
_cell_length_b                   12.8357(5)
_cell_length_c                   18.1558(5)
_cell_measurement_reflns_used    12920
_cell_measurement_temperature    290.05(10)
_cell_measurement_theta_max      72.4570
_cell_measurement_theta_min      3.9560
_cell_volume                     5271.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.05(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     86.00 129.00   0.50    0.70    --  107.75  77.00 150.00   86
  2  \w    147.00 173.00   0.50    0.70    --  107.75  77.00   0.00   52
  3  \w     90.00 126.00   0.50    0.70    --  107.75  77.00-150.00   72
  4  \w     85.00 121.00   0.50    0.70    --  107.75  77.00-180.00   72
  5  \w    150.00 176.00   0.50    0.70    --  107.75  77.00-180.00   52
  6  \w     89.00 145.00   0.50    0.70    --  107.75  77.00-120.00  112
  7  \w     91.00 159.00   0.50    0.70    --  107.75  61.00-120.00  136
  8  \w     94.00 142.00   0.50    0.70    --  107.75  61.00-150.00   96
  9  \w    138.00 167.00   0.50    0.70    --  107.75  45.00  30.00   58
 10  \w     94.00 178.00   0.50    0.70    --  107.75  52.00 105.00  168
 11  \w    141.00 177.00   0.50    0.70    --  107.75  77.00 150.00   72
 12  \w     92.00 156.00   0.50    0.70    --  107.75  61.00 150.00  128
 13  \w     35.00 121.00   0.50    0.18    --   48.09  52.00 105.00  172
 14  \w    108.00 172.00   0.50    0.70    --  107.75  45.00  90.00  128
 15  \w    111.00 177.00   0.50    0.70    --  107.75  45.00  60.00  132
 16  \w    100.00 133.00   0.50    0.70    --  107.75  45.00  30.00   66
 17  \w     95.00 153.00   0.50    0.70    --  107.75  15.00-120.00  116
 18  \w     36.00 121.00   0.50    0.18    --   48.09  38.00 -90.00  170
 19  \w    -23.00  62.00   0.50    0.18    --   48.09 -52.00 -39.00  170
 20  \w    -26.00  28.00   0.50    0.18    --   48.09 -19.00-180.00  108
 21  \w    -26.00  28.00   0.50    0.18    --   48.09 -19.00 -30.00  108
 22  \w    -26.00  28.00   0.50    0.18    --   48.09 -19.00   0.00  108
 23  \w     35.00 104.00   0.50    0.70    --  107.75 -94.00  30.00  138
 24  \w     36.00 103.00   0.50    0.70    --  107.75 -77.00  60.00  134
 25  \w     42.00  88.00   0.50    0.70    --  107.75-125.00  30.00   92
 26  \w     35.00  63.00   0.50    0.70    --  107.75 -61.00  30.00   56
 27  \w     67.00  99.00   0.50    0.70    --  107.75 -77.00 -60.00   64
 28  \w     36.00  72.00   0.50    0.70    --  107.75 -61.00 -60.00   72
 29  \w     36.00  73.00   0.50    0.70    --  107.75 -61.00 -90.00   74
 30  \w     35.00  61.00   0.50    0.70    --  107.75 -52.00 -39.00   52
 31  \w     37.00  77.00   0.50    0.70    --  107.75-125.00-120.00   80
 32  \w     35.00 106.00   0.50    0.70    --  107.75 -77.00-120.00  142
 33  \w     35.00  63.00   0.50    0.70    --  107.75 -61.00-120.00   56
 34  \w     43.00  72.00   0.50    0.70    --  107.75 -61.00-180.00   58
 35  \w    -57.00  24.00   0.50    0.18    --  -48.09  52.00 105.00  162
 36  \w    -57.00 -14.00   0.50    0.70    --  -86.25  52.00 105.00   86
 37  \w    -49.00 -14.00   0.50    0.70    --  -86.25  45.00  60.00   70
 38  \w    -49.00 -14.00   0.50    0.70    --  -86.25  45.00 -60.00   70
 39  \w    -49.00 -14.00   0.50    0.70    --  -86.25  45.00-120.00   70
 40  \w    -49.00 -14.00   0.50    0.70    --  -86.25  45.00-150.00   70
 41  \w   -161.00 -73.00   0.50    0.70    --  -86.25 -30.00-150.00  176
 42  \w   -159.00 -63.00   0.50    0.70    --  -86.25 -77.00-150.00  192
 43  \w   -159.00 -63.00   0.50    0.70    --  -86.25 -77.00-120.00  192
 44  \w   -121.00 -36.00   0.50    0.18    --  -48.09 -38.00-180.00  170
 45  \w   -158.00 -73.00   0.50    0.70    --  -86.25 -45.00 -90.00  170
 46  \w   -159.00 -72.00   0.50    0.70    --  -86.25 -52.00 -39.00  174
 47  \w   -120.00 -34.00   0.50    0.18    --  -48.09 -52.00 -39.00  172
 48  \w   -121.00 -73.00   0.50    0.18    --  -48.09-125.00  30.00   96
 49  \w   -121.00 -73.00   0.50    0.18    --  -48.09-125.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144558000
_diffrn_orient_matrix_UB_12      -0.0613864000
_diffrn_orient_matrix_UB_13      0.0721244000
_diffrn_orient_matrix_UB_21      0.0571213000
_diffrn_orient_matrix_UB_22      -0.0411148000
_diffrn_orient_matrix_UB_23      -0.0301876000
_diffrn_orient_matrix_UB_31      0.0341370000
_diffrn_orient_matrix_UB_32      0.0945887000
_diffrn_orient_matrix_UB_33      0.0336846000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30335
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.860
_diffrn_reflns_theta_min         3.908
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.339
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.147
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5144
_refine_ls_number_restraints     449
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0651
_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^)+(0.1210P)^2^+3.1573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3021
_reflns_number_total             5144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00312g2.cif
_cod_data_source_block           hut20_101_11_290_00
_cod_depositor_comments
'Adding full bibliography for 7060642--7060658.cif.'
_cod_database_code               7060651
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C6A-C7A = C6B-C7B
 1.32268 with sigma of 0.02
 C3A-C6A = C3B-C6B = C7A-C8 = C7B-C8
 1.49331 with sigma of 0.02
 S1-O1A = S1-O2A = S1-O3 = S1-O1B = S1-O2B
 1.43 with sigma of 0.02
 C27A-F1A = C27A-F2A = C27A-F3A
 1.35784 with sigma of 0.02
 C27B-F1B = C27B-F2B = C27B-F3B
 1.35784 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C6A \\sim C7A \\sim C6B \\sim C7B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N1B \\sim C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim N1A \\sim C1A \\sim
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C6B \\sim C7A \\sim C7B:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
S1 \\sim O1A \\sim O2A \\sim O3 \\sim C27A \\sim F1A \\sim F2A \\sim F3A \\sim
C27B \\sim F1B \\sim F2B \\sim F3B \\sim O1B \\sim O2B: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(N1B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=
 Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(C27B)=1-FVAR(5)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(C27A)=FVAR(5)
 1(DFIX)=1(DFIX)=FVAR(6)
5.a Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C2B(H2B), C4B(H4B), C5B(H5B), C6A(H6A), C7A(H7A), C6B(H6B),
 C7B(H7B), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A)
5.b Fitted hexagon refined as free rotating group:
 N1B(C1B,C2B,C3B,C4B,C5B)
;
_shelx_res_checksum              377
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.705
_oxdiff_exptl_absorpt_empirical_full_min 0.399