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_7719776
_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         'C60.036 H78.107 Au N P, C31.643 H12 B F24'
_chemical_formula_sum            'C91.68 H90.1 Au B F24 N P'
_chemical_formula_weight         1900.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-03
_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                75.532(5)
_cell_angle_beta                 68.977(6)
_cell_angle_gamma                89.130(5)
_cell_formula_units_Z            2
_cell_length_a                   15.6853(10)
_cell_length_b                   16.4299(10)
_cell_length_c                   19.4505(12)
_cell_measurement_reflns_used    37647
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      76.1590
_cell_measurement_theta_min      3.9900
_cell_volume                     4515.1(5)
_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_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_unetI/netI     0.1169
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50070
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.171
_diffrn_reflns_theta_min         3.927
_exptl_absorpt_coefficient_mu    4.042
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_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
Empricial absorption correciton using spherical
harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.109
_refine_diff_density_max         3.919
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1255
_refine_ls_number_reflns         18248
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.1221
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1725P)^2^+13.5467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2866
_refine_ls_wR_factor_ref         0.3356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10760
_reflns_number_total             18248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02464a2.cif
_cod_data_source_block           asw23022_autored-copy
_cod_depositor_comments
'Adding full bibliography for 7719775--7719776.cif.'
_cod_original_formula_sum        'C91.68 H90.10 Au B F24 N P'
_cod_database_code               7719776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C28 \\sim C25-C28A \\sim C25-C26 \\sim C25-C27 \\sim C25-C27A \\sim
C25-C26A
 with sigma of 0.02
 C58A-C56A \\sim C58-C56 \\sim C59A-C56A \\sim C59-C56 \\sim C57A-C56A \\sim
C57-C56
 with sigma of 0.02
 C26-C27 \\sim C26-C28 \\sim C27-C28 \\sim C27A-C28A \\sim C26A-C27A \\sim
C26A-C28A
 with sigma of 0.04
 F16-F17 \\sim F16-F18 \\sim F17-F18 \\sim F16A-F17A \\sim F16A-F18A \\sim
F17A-F18A
 with sigma of 0.04
 C68-F13 \\sim C68-F14 \\sim C68-F15 \\sim C68-F13A \\sim C68-F14A \\sim
C68-F15A
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15 \\sim F13A-F14A \\sim F14A-F15A \\sim
F13A-F15A
 with sigma of 0.04
 C89-F1 \\sim C89-F2 \\sim C89-F3 \\sim C89-F1A \\sim C89-F2A \\sim C89-F3A
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C58 \\sim C58A \\sim C59 \\sim C59A \\sim C56 \\sim C56A \\sim C57A \\sim C57:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C26 \\sim C26A \\sim C27 \\sim C27A \\sim C28 \\sim C28A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
F16 \\sim F16A \\sim F17 \\sim F17A \\sim F18 \\sim F18A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=FVAR(2)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(3)
 Sof(F16)=Sof(F17)=Sof(F18)=Sof(C65)=FVAR(3)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(4)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(4)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(5)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(5)
 Sof(C58A)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C56A)=Sof(C57A)=Sof(H57E)=
 Sof(H57F)=Sof(H57G)=Sof(C59A)=Sof(H59C)=Sof(H59D)=Sof(H59E)=1-FVAR(6)
 Sof(C56)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H57D)=FVAR(6)
5.a Me refined with riding coordinates:
 C58(H58A,H58B,H58C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C12(H12), C13(H13), C20(H20), C21(H21), C23(H23),
 C29(H29), C30(H30), C33(H33), C34(H34), C40(H40), C41(H41), C43(H43), C49(H49),
  C50(H50), C53(H53), C54(H54), C60(H60), C61(H61), C63(H), C66(HA), C69(HB),
 C71(HC), C74(HD), C77(HE), C79(HF), C82(HG), C85(HH), C87(HI), C90(HJ), C93(HK)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C),
 C26A(H26D,H26E,H26F), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C28(H28A,H28B,
 H28C), C28A(H28D,H28E,H28F), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C57(H57A,H57B,H57C), C59(H59A,H59B,H57D), C58A(H58D,H58E,H58F),
 C57A(H57E,H57F,H57G), C59A(H59C,H59D,H59E)
;
_shelx_res_checksum              28544
_olex2_submission_special_instructions 'No special instructions were received'