A simple synthetic entryway into new families of NHC-gold-amido complexes and their in vitro antitumor activity
Nolan, Steven P.; Martynova, Ekaterina A.; Van Hecke, Kristof; Rizzolio, Flavio; Peng, Min; Cavarzenari, Enrico; Scattolin, Thomas; Dalton Transactions  (2022) –; doi:10.1039/D2DT00239F

data_7709431
_publ_section_title
;
 A simple synthetic entryway into new families of NHC-gold-amido complexes
 and their in vitro antitumor activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00239F
_journal_year                    2022
_chemical_formula_moiety         'C35 H40 Au N3 S'
_chemical_formula_sum            'C35 H40 Au N3 S'
_chemical_formula_weight         731.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.07582(15)
_cell_length_b                   18.5823(2)
_cell_length_c                   28.4054(5)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.6000
_cell_measurement_theta_min      3.0750
_cell_volume                     5846.23(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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    -83.00  38.00   1.00    1.20    --  -41.68  19.00  60.00  121
  2  \w     27.00  98.00   1.00    1.20    --   41.68-125.00   0.00   71
  3  \w     97.00 178.00   1.00    6.30    --  106.01 125.00  60.00   81
  4  \w    103.00 178.00   1.00    6.30    --  106.01  77.00 -90.00   75
  5  \w     77.00 178.00   1.00    6.30    --  106.01  61.00-120.00  101
  6  \w    103.00 178.00   1.00    6.30    --  106.01  77.00 150.00   75
  7  \w   -116.00 -17.00   1.00    1.20    --  -41.68 -37.00   8.00   99
  8  \w   -115.00 -14.00   1.00    1.20    --  -41.68 -57.00 -90.00  101
  9  \w     77.00 178.00   1.00    6.30    --  106.01  61.00   0.00  101
 10  \w     78.00 122.00   1.00    6.30    --  106.01  30.00 120.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0042757000
_diffrn_orient_matrix_UB_12      -0.0467927000
_diffrn_orient_matrix_UB_13      0.0447202000
_diffrn_orient_matrix_UB_21      0.0654439000
_diffrn_orient_matrix_UB_22      0.0609627000
_diffrn_orient_matrix_UB_23      0.0264055000
_diffrn_orient_matrix_UB_31      -0.1227100000
_diffrn_orient_matrix_UB_32      0.0310204000
_diffrn_orient_matrix_UB_33      0.0156381000
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28502
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.866
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.340
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_preparation       synthesis
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.077
_refine_diff_density_max         2.644
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0563P)^2^+3.6478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4684
_reflns_number_total             5832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00239f2.cif
_cod_data_source_block           em180-2
_cod_original_cell_volume        5846.22(14)
_cod_database_code               7709431
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H52 Au N3 S'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C18(H18), C20(H20), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,
 H13B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
 C33(H33), C34(H34)
;
_shelx_res_checksum              79019
_olex2_date_sample_data_collection 2021-04-07
_olex2_exptl_crystal_mounting_method 'Mounted on a LithoLoop'
_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 2.899
_oxdiff_exptl_absorpt_empirical_full_min 0.634