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_7060643
_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                 98.0560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.0404(2)
_cell_length_b                   12.65120(10)
_cell_length_c                   18.30820(10)
_cell_measurement_reflns_used    34543
_cell_measurement_temperature    170.05(10)
_cell_measurement_theta_max      77.3080
_cell_measurement_theta_min      4.0260
_cell_volume                     5054.63(7)
_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      N~2~
_diffrn_ambient_temperature      170.05(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_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      0.0183632000
_diffrn_orient_matrix_UB_12      -0.0625976000
_diffrn_orient_matrix_UB_13      0.0718783000
_diffrn_orient_matrix_UB_21      0.0577870000
_diffrn_orient_matrix_UB_22      -0.0403676000
_diffrn_orient_matrix_UB_23      -0.0297313000
_diffrn_orient_matrix_UB_31      0.0361408000
_diffrn_orient_matrix_UB_32      0.0963363000
_diffrn_orient_matrix_UB_33      0.0342409000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30135
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.489
_diffrn_reflns_theta_min         4.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.655
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.153
_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    1.628
_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         1.461
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5157
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0503P)^2^+10.4735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4890
_reflns_number_total             5157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00312g2.cif
_cod_data_source_block           hut20_101_05_170_00
_cod_depositor_comments
'Adding full bibliography for 7060642--7060658.cif.'
_cod_database_code               7060643
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.66
_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
 1.33281 with sigma of 0.02
 C3A-C6A = C3B-C6B = C7A-C8 = C7B-C8
 1.48847 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
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)
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              96514
_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 2.205
_oxdiff_exptl_absorpt_empirical_full_min 0.404