Covalent and non-covalent albumin binding of Au(i) bis-NHCs <i>via</i> post-synthetic amide modification.
Sen, Sajal; Perrin, Mark W.; Sedgwick, Adam C.; Lynch, Vincent M.; Sessler, Jonathan L.; Arambula, Jonathan F.; Chemical science 12 (2021) 7547–7553; doi:10.1039/d1sc01055g

data_1562121
_publ_section_title
;
 Covalent and non-covalent albumin binding of Au(i) bis-NHCs <i>via</i>
 post-synthetic amide modification.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              7547
_journal_page_last               7553
_journal_paper_doi               10.1039/d1sc01055g
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety
'2 C27 H36 N2, C14 H15 N2 O2 1-, C14 H16 N2 O2, 2 Au 1+, Br 1-'
_chemical_formula_sum            'C82 H102 Au2 Br N8 O4'
_chemical_formula_weight         1737.55
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-02-10 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                86.368(4)
_cell_angle_beta                 88.416(4)
_cell_angle_gamma                78.854(3)
_cell_formula_units_Z            2
_cell_length_a                   13.630(2)
_cell_length_b                   15.952(2)
_cell_length_c                   19.288(3)
_cell_measurement_reflns_used    15657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4105.8(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

Sheldrick. G. M.  (2015) SHELXT. Acta Cryst. A71, 3-8.

Sluis, P. v. d. and Spek, T. (1990). Squeeze.  Acta Cryst. A46, 194-201.

;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65764
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    4.106
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       prism
_exptl_crystal_F_000             1750
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
Two molecules of DCM were badly disordered and could not be 
modeled adequately.  SQUEEZE was used to remove their 
contributions to the scattering factors.
;
_refine_diff_density_max         3.577
_refine_diff_density_min         -3.793
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1062
_refine_ls_number_reflns         18451
_refine_ls_number_restraints     1188
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+16.8991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16450
_reflns_number_total             18451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01055g2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
'Adding full bibliography for 1562121--1562124.cif.'
_cod_database_code               1562121
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.320
_shelx_estimated_absorpt_t_max   0.709
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              1107
_shelx_hkl_checksum              88965
_shelx_fab_checksum              45408