Carbon-phosphorus stapled Au(I) anticancer agents <i>via</i> bisphosphine induced reductive elimination.
Gilpatrick, Sean T.; Obisesan, Oluwatosin A.; Parkin, Sean; Awuah, Samuel G.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18974–18982; doi:10.1039/d4dt01929f

data_7716832
_publ_section_title
;
 Carbon-phosphorus stapled Au(I) anticancer agents <i>via</i> bisphosphine
 induced reductive elimination.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18974
_journal_page_last               18982
_journal_paper_doi               10.1039/d4dt01929f
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C47 H36 Au Cl N O P2, C4 H10 O, C H2 Cl2, Cl, H2 O'
_chemical_formula_sum            'C52 H50 Au Cl4 N O3 P2'
_chemical_formula_weight         1137.63
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-06-26 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                69.840(1)
_cell_angle_beta                 76.071(1)
_cell_angle_gamma                80.548(1)
_cell_formula_units_Z            1
_cell_length_a                   9.5743(4)
_cell_length_b                   10.8642(3)
_cell_length_c                   13.1587(5)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.49
_cell_volume                     1242.12(8)
_computing_cell_refinement       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_reduction        '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2019/2</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58572
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.606
_diffrn_reflns_theta_min         2.005
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.283
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause <i>et al</i>., 2015)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
; 
Flack 'x' determined using 5196 quotients [(I+)-(I-)]/[(I+)+(I-)] 
[Parsons, Flack and Wagner (2013)]. 
;
_refine_ls_abs_structure_Flack   0.012(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11334
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0245
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                11161
_reflns_number_total             11334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01929f2.cif
_cod_data_source_block           m24077
_cod_depositor_comments
'Adding full bibliography for 7716832--7716833.cif.'
_cod_database_code               7716832
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.605
_shelx_estimated_absorpt_t_max   0.803
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by X-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the X-ray beam cross section, absorption by the crystal 
mount, scan truncation etc. These account, by and large, for the difference 
between SHELX estimates of Tmin and Tmax and the _exptl_absorpt_correction_ 
values. 
;
_shelx_res_checksum              63485
_shelx_hkl_checksum              87722