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_7060657
_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 H21 Ag F3 N2 O3 S'
_chemical_formula_sum            'C27 H21 Ag F3 N2 O3 S'
_chemical_formula_weight         618.39
_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                 94.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6955(4)
_cell_length_b                   12.7839(3)
_cell_length_c                   18.1157(3)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    270.07(11)
_cell_measurement_theta_max      63.2160
_cell_measurement_theta_min      3.9070
_cell_volume                     5238.60(18)
_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      270.07(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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      -0.0334879000
_diffrn_orient_matrix_UB_12      0.1033723000
_diffrn_orient_matrix_UB_13      -0.0161619000
_diffrn_orient_matrix_UB_21      0.0100840000
_diffrn_orient_matrix_UB_22      -0.0104099000
_diffrn_orient_matrix_UB_23      -0.0827566000
_diffrn_orient_matrix_UB_31      -0.0584241000
_diffrn_orient_matrix_UB_32      -0.0610605000
_diffrn_orient_matrix_UB_33      -0.0131765000
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.457
_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    7.386
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5170
_refine_ls_number_restraints     581
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0734P)^2^+3.7245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3090
_reflns_number_total             5170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00312g2.cif
_cod_data_source_block           hut20_77_5_270_00
_cod_depositor_comments
'Adding full bibliography for 7060642--7060658.cif.'
_cod_database_code               7060657
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag O C N H F S'
_shelx_estimated_absorpt_t_max   0.514
_shelx_estimated_absorpt_t_min   0.365
_reflns_odcompleteness_completeness 99.90
_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
 1.30724 with sigma of 0.02
 C3-C6A = C3-C6B = C7A-C8 = C7B-C8
 1.50537 with sigma of 0.02
 S1-O1A = S1-O2A = S1-O3
 1.39971 with sigma of 0.02
 S1-O1B = S1-O2B
 1.50537 with sigma of 0.02
 C27A-F1A = C27A-F2A = C27A-F3A
 1.3599 with sigma of 0.02
 C27B-F1B = C27B-F2B = C27B-F3B
 1.3599 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=FVAR(1)
 1(DFIX)=1(DFIX)=FVAR(3)
 1(DFIX)=1(DFIX)=FVAR(5)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(C27B)=1-FVAR(6)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(C27A)=FVAR(6)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6A(H6A), C6B(H6B), C7A(H7A), 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)
;
_shelx_res_checksum              72452
_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 2.050
_oxdiff_exptl_absorpt_empirical_full_min 0.744