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_7060658
_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                 94.599(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.6895(5)
_cell_length_b                   12.8292(4)
_cell_length_c                   18.1655(3)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    290.06(11)
_cell_measurement_theta_max      54.8460
_cell_measurement_theta_min      3.9050
_cell_volume                     5270.7(2)
_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      air
_diffrn_ambient_temperature      290.06(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 0.979
_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      -0.0336235000
_diffrn_orient_matrix_UB_12      0.1027912000
_diffrn_orient_matrix_UB_13      -0.0163842000
_diffrn_orient_matrix_UB_21      0.0102567000
_diffrn_orient_matrix_UB_22      -0.0106537000
_diffrn_orient_matrix_UB_23      -0.0824825000
_diffrn_orient_matrix_UB_31      -0.0583423000
_diffrn_orient_matrix_UB_32      -0.0611061000
_diffrn_orient_matrix_UB_33      -0.0130920000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_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            25274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.586
_diffrn_reflns_theta_min         3.909
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.341
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.588
_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    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     581
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1010P)^2^+3.0045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2680
_reflns_number_total             5198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00312g2.cif
_cod_data_source_block           hut20_77_6_290_00
_cod_depositor_comments
'Adding full bibliography for 7060642--7060658.cif.'
_cod_database_code               7060658
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag2 N4 C54 H30 O6 F6 S2'
_shelx_estimated_absorpt_t_max   0.545
_shelx_estimated_absorpt_t_min   0.375
_reflns_odcompleteness_completeness 99.92
_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
 1.32552 with sigma of 0.02
 C3-C6A = C3-C6B = C7A-C8 = C7B-C8
 1.48886 with sigma of 0.02
 S1-O1A = S1-O2A = S1-O3
 1.40302 with sigma of 0.02
 S1-O1B = S1-O2B
 1.48886 with sigma of 0.02
 C27A-F1A = C27A-F2A = C27A-F3A
 1.3566 with sigma of 0.02
 C27B-F1B = C27B-F2B = C27B-F3B
 1.3566 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              62722
_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 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.546