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_7060654
_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             2020-09-21
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.0819(2)
_cell_length_b                   12.66420(10)
_cell_length_c                   18.3777(2)
_cell_measurement_reflns_used    13816
_cell_measurement_temperature    210.05(10)
_cell_measurement_theta_max      73.2340
_cell_measurement_theta_min      4.0260
_cell_volume                     5092.83(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      210.05(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_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    -24.00  83.00   0.50    0.15    --    0.00  19.00  90.00  214
  2  \w     19.00 139.00   0.50    0.59    --   57.66  57.00  90.00  240
  3  \w    101.00 178.00   0.50    0.59    --  115.32  81.00  56.00  154
  4  \w     95.00 140.00   0.50    0.59    --   57.66 125.00 -30.00   90
  5  \w    103.00 178.00   0.50    0.59    --  115.32 111.00-120.00  150
  6  \w    103.00 178.00   0.50    0.59    --  115.32 111.00   0.00  150
  7  \w     72.00 178.00   0.50    0.59    --  115.32  50.00   0.00  212
  8  \w     63.00 146.00   0.50    0.59    --  115.32 178.00-120.00  166
  9  \w     12.00 140.00   0.50    0.59    --   57.66  77.00-180.00  256
 10  \w     32.00  59.00   0.50    0.59    --  115.32 -50.00 -30.00   54
 11  \w     33.00  76.00   0.50    0.59    --  115.32 -63.00 -30.00   86
 12  \w     32.00  59.00   0.50    0.59    --  115.32 -50.00   0.00   54
 13  \w     32.00  59.00   0.50    0.59    --  115.32 -50.00  60.00   54
 14  \w     33.00  76.00   0.50    0.59    --  115.32 -63.00 150.00   86
 15  \w    -21.00 106.00   0.50    0.59    --   57.66 -81.00 -66.00  254
 16  \w     23.00 163.00   0.50    0.59    --  115.32 -81.00 -66.00  280
 17  \w     33.00  76.00   0.50    0.59    --  115.32 -63.00-150.00   86
 18  \w     32.00  59.00   0.50    0.59    --  115.32 -50.00 -90.00   54
 19  \w     12.00 140.00   0.50    0.59    --   57.66  77.00 -60.00  256
 20  \w     12.00  96.00   0.50    0.59    --   57.66  77.00   0.00  168
 21  \w    -20.00  47.00   0.50    0.15    --    0.00 -81.00 -66.00  134
 22  \w    -24.00  25.00   0.50    0.59    --  -57.66  19.00  60.00   98
 23  \w    -24.00  25.00   0.50    0.59    --  -57.66  19.00 150.00   98
 24  \w    -24.00  25.00   0.50    0.59    --  -57.66  19.00  30.00   98
 25  \w    -48.00  43.00   0.50    0.15    --    0.00  81.00  56.00  182
 26  \w    -24.00  25.00   0.50    0.59    --  -57.66  19.00-120.00   98
 27  \w    -24.00  25.00   0.50    0.59    --  -57.66  19.00-180.00   98
 28  \w    -55.00 -22.00   0.50    0.59    -- -104.25  50.00 -90.00   66
 29  \w    -55.00 -22.00   0.50    0.59    -- -104.25  50.00-150.00   66
 30  \w    -82.00 -22.00   0.50    0.59    -- -104.25 111.00-180.00  120
 31  \w    -55.00 -22.00   0.50    0.59    -- -104.25  50.00   0.00   66
 32  \w    -55.00 -22.00   0.50    0.59    -- -104.25  50.00  30.00   66
 33  \w    -55.00 -22.00   0.50    0.59    -- -104.25  50.00  60.00   66
 34  \w   -105.00  25.00   0.50    0.59    --  -57.66  81.00  56.00  260
 35  \w    -46.00  83.00   0.50    0.15    --    0.00  77.00 150.00  258
 36  \w   -100.00 -41.00   0.50    0.15    --    0.00-178.00  90.00  118
 37  \w   -100.00 -41.00   0.50    0.15    --    0.00-178.00 120.00  118
 38  \w   -149.00 -80.00   0.50    0.59    --  -57.66 -81.00 -66.00  138
 39  \w   -177.00 -79.00   0.50    0.59    -- -104.25 -81.00 -66.00  196
 40  \w    -98.00 -39.00   0.50    0.15    --    0.00 178.00-120.00  118
;
_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      -0.0348013000
_diffrn_orient_matrix_UB_12      0.1042291000
_diffrn_orient_matrix_UB_13      -0.0179018000
_diffrn_orient_matrix_UB_21      0.0092582000
_diffrn_orient_matrix_UB_22      -0.0112990000
_diffrn_orient_matrix_UB_23      -0.0812676000
_diffrn_orient_matrix_UB_31      -0.0604751000
_diffrn_orient_matrix_UB_32      -0.0616770000
_diffrn_orient_matrix_UB_33      -0.0153604000
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.671
_diffrn_reflns_theta_min         4.033
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.597
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.000074(10)
_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   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5011
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0325P)^2^+5.1086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4569
_reflns_number_total             5011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00312g2.cif
_cod_data_source_block           hut20_77_2_210_00
_cod_depositor_comments
'Adding full bibliography for 7060642--7060658.cif.'
_cod_database_code               7060654
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'S O C N H F Ag'
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.365
_reflns_odcompleteness_completeness 99.71
_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
 1.32011 with sigma of 0.02
 C3-C6A = C3-C6B = C7A-C8 = C7B-C8
 1.49696 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
4. Others
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), 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)
;
_shelx_res_checksum              19996
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.697