Single-crystal to single-crystal synthesis of a gold(I)-ammonia complex and H/D exchange <i>in crystallo</i> with D<sub>2</sub>O.
Johnson, Chloe L.; Altus, Kristof M.; Navarro, Miquel; Campos, Jesús; Duckett, Simon B.; Weller, Andrew S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16673–16676; doi:10.1039/d5dt02464a

data_7719775
_publ_section_title
;
 Single-crystal to single-crystal synthesis of a gold(I)-ammonia complex
 and H/D exchange <i>in crystallo</i> with D<sub>2</sub>O.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16673
_journal_page_last               16676
_journal_paper_doi               10.1039/d5dt02464a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C60 H75 Au Cl0.828 P, C32 H12 B F24, 0.972(N), C1.532 H0.833 F0.382'
_chemical_formula_sum            'C93.53 H87.83 Au B Cl0.83 F24.38 N0.97 P'
_chemical_formula_weight         1956.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-06 deposited with the CCDC.	2025-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.81560(10)
_cell_length_b                   33.8381(3)
_cell_length_c                   19.0978(2)
_cell_measurement_reflns_used    29176
_cell_measurement_temperature    110.01(10)
_cell_measurement_theta_max      77.0070
_cell_measurement_theta_min      2.7620
_cell_volume                     9088.12(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_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     62.00  87.00   0.50    4.00    --   48.70 152.00 -19.00   50
  2  \w     56.00  81.00   0.50    4.00    --   48.70-122.00  98.00   50
  3  \w    -81.00 -56.00   0.50    4.00    --  -49.95 122.00 179.00   50
  4  \w   -118.00 -57.00   0.50    4.00    --  -49.95-152.00 -62.00  122
  5  \w   -144.00-119.00   0.50    4.00    --  -92.27-122.00  98.00   50
  6  \w   -110.00 -68.00   0.50    4.00    --  -92.27-152.00 -62.00   84
  7  \w   -103.00 -78.00   0.50    4.00    --  -92.27 152.00 -19.00   50
  8  \w   -108.00 -82.00   0.50    4.00    --  -92.27 122.00 179.00   52
  9  \w    102.00 127.00   0.50    4.00    --  103.47 122.00 179.00   50
 10  \w     71.00 125.00   0.50    4.00    --  111.41-152.00 -62.00  108
 11  \w    103.00 128.00   0.50    4.00    --  111.41 122.00 179.00   50
 12  \w     62.00  91.00   0.50    4.00    --  111.41-122.00  98.00   58
 13  \w     85.00 110.00   0.50    4.00    --  111.41 152.00 -19.00   50
 14  \w    -29.00  42.00   0.50    4.00    --   48.70 -38.00-150.00  142
 15  \w    -11.00  23.00   0.50    4.00    --   48.70 -19.00 150.00   68
 16  \w     86.00 121.00   0.50    4.00    --   48.70 125.00 120.00   70
 17  \w    -29.00  27.00   0.50    4.00    --   48.70 -19.00 -90.00  112
 18  \w    -98.00 -73.00   0.50    4.00    --  -92.27-125.00  60.00   50
 19  \w    -49.00 -18.00   0.50    4.00    --  -92.27  45.00 -30.00   62
 20  \w   -163.00-133.00   0.50    4.00    --  -92.27-125.00  60.00   60
 21  \w    -48.00 -18.00   0.50    4.00    --  -92.27  45.00 -90.00   60
 22  \w    -50.00 -16.00   0.50    4.00    --  -92.27  45.00 -60.00   68
 23  \w    -50.00 -16.00   0.50    4.00    --  -92.27  45.00   0.00   68
 24  \w    -47.00 -18.00   0.50    4.00    --  -92.27  45.00  30.00   58
 25  \w    -50.00 -18.00   0.50    4.00    --  -92.27  45.00  60.00   64
 26  \w   -119.00 -69.00   0.50    4.00    --  -99.00 137.00  66.78  100
 27  \w     39.00  82.00   0.50    4.00    --  103.47 -95.00  90.00   86
 28  \w     35.00  99.00   0.50    4.00    --  103.47 -77.00 -90.00  128
 29  \w     91.00 171.00   0.50    4.00    --  111.41  30.00   0.00  160
 30  \w     39.00  67.00   0.50    4.00    --  111.41 -61.00 -30.00   56
 31  \w     52.00 102.00   0.50    4.00    --  111.41-125.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72897
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.387
_diffrn_reflns_theta_min         2.612
_exptl_absorpt_coefficient_mu    4.259
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
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_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             3953
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         11.339
_refine_diff_density_min         -7.807
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1274
_refine_ls_number_reflns         18509
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+143.6470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15488
_reflns_number_total             18509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02464a2.cif
_cod_data_source_block           asw25007_autored
_cod_depositor_comments
'Adding full bibliography for 7719775--7719776.cif.'
_cod_database_code               7719775
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Au1P1B1F24N1Cl1C90H90
_chemical_oxdiff_usercomment     CJ507
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C95-C100 = C95-C96 = C100-C99
 1.39 with sigma of 0.02
 C95-F25 = C100-F26
 1.35 with sigma of 0.02
 C99-C98 = C98-C97 = C97-C96
 1.4 with sigma of 0.02
 C95-C99 = C99-C97 = C98-C96
 2.42 with sigma of 0.04
 C95-F26
 2.37 with sigma of 0.04
 C95-C97 = C100-C98
 2.4 with sigma of 0.04
 C48-C46 \\sim C49A-C46 \\sim C49-C46 \\sim C47A-C46 \\sim C47-C46 \\sim
C48A-C46
 with sigma of 0.02
 C4-C5 \\sim C4-C5A
 with sigma of 0.02
 C4-C6 \\sim C4-C6A
 with sigma of 0.02
 C6A-C4 \\sim C6-C4 \\sim C5A-C4 \\sim C5-C4 \\sim C7-C4
 with sigma of 0.02
 F16-F17 \\sim F17-F18 \\sim F18-F16 \\sim F16A-F17A \\sim F17A-F18A \\sim
F16A-F18A
 with sigma of 0.04
 F16A-C85 \\sim F17-C85 \\sim F17A-C85 \\sim F18-C85 \\sim F18A-C85 \\sim
F16-C85
 with sigma of 0.02
 C95-F25 \\sim C100-F26
 with sigma of 0.02
 C95-C96 \\sim C97-C96 \\sim C95-C100 \\sim C98-C97 \\sim C99-C98 \\sim C100-C99
 with sigma of 0.02
 C95-F26 \\sim C99-F26 \\sim C100-F25 \\sim C96-F25
 with sigma of 0.04
 C98-C96 \\sim C99-C97 \\sim C100-C98 \\sim C95-C99 \\sim C100-C96 \\sim C95-C97
 with sigma of 0.04
3. Restrained planarity
 C95, C100, C99, C98, C97, C96, F25, F26
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C6A \\sim C6 \\sim C5A \\sim C5 \\sim C7 \\sim C4: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
F16A \\sim F16 \\sim C85 \\sim F18A \\sim F18 \\sim F17A \\sim F17: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C95 \\sim C100 \\sim C99 \\sim C98 \\sim C97 \\sim C96 \\sim F25 \\sim F26:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C20 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C19 \\sim C1 \\sim C2 \\sim
C3 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C95, C100, C99, C98, C97, C96, F25, F26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=1-FVAR(1)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 1-FVAR(2)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(2)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(3)
 Sof(F17)=Sof(F18)=Sof(F16)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C44(H44), C68(H68), C74(H74), C66(H66), C22(H22), C80(H80), C82(H82),
 C41(H41), C76(H76), C13(H13), C51(H51), C50(H50), C84(H84), C72(H72), C12(H12),
  C42(H42), C92(H92), C88(H88), C33(H33), C19(H19), C64(H64), C54(H54),
 C36(H36), C61(H61), C20(H20), C29(H29), C28(H28), C62(H62), C8(H8), C55(H55),
 C90(H90), C9(H9), C99(H99), C98(H98), C97(H97), C96(H96)
7.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C59(H59A,H59B,H59C), C5(H5A,H5B,H5C), C58(H58A,H58B,H58C), C60(H60A,
 H60B,H60C), C6(H6A,H6B,H6C), C39(H39A,H39B,H39C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C38(H38A,H38B,H38C), C25(H25A,H25B,H25C), C40(H40A,H40B,
 H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C47(H47A,H47B,H47C),
 C48A(H48D,H48E,H48F), C47A(H47D,H47E,H47F), C49A(H49D,H49E,H49F), C6A(H6AA,
 H6AB,H6AC), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              85374
_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 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.830