Development of a novel highly anti-proliferative family of gold complexes: Au(i)-phosphonium-phosphines.
Rousselle, Benjamin; Bouyer, Florence; Bayardon, Jérôme; Laly, Myriam; Ghiringhelli, François; Rousselin, Yoann; Bodio, Ewen; Malacea-Kabbara, Raluca; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4880–4889; doi:10.1039/d0dt03708g

data_7706785
_publ_section_title
;
 Development of a novel highly anti-proliferative family of gold
 complexes: Au(i)-phosphonium-phosphines.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4880
_journal_page_last               4889
_journal_paper_doi               10.1039/d0dt03708g
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C32 H27 Au Br0.534 Cl0.466 P2, C H2 Cl2, 0.294(Br), 0.706(Cl)'
_chemical_formula_sum            'C33 H29 Au Br0.83 Cl3.17 P2'
_chemical_formula_weight         863.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2021-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.312(2)
_cell_length_b                   9.6184(7)
_cell_length_c                   13.5131(9)
_cell_measurement_reflns_used    917
_cell_measurement_temperature    110.0(1)
_cell_measurement_theta_max      19.06
_cell_measurement_theta_min      2.72
_cell_volume                     3289.9(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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_temperature      110.0(1)
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_detector_type            APEX2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.1347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17639
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.660
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.854
_exptl_absorpt_correction_T_max  0.0206
_exptl_absorpt_correction_T_min  0.0047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1002 before and 0.0807 after correction. The Ratio of minimum to maximum transmission is 0.4338. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Flack x determined using 1084 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3384
_reflns_number_total             5751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03708g2.cif
_cod_data_source_block           compound_If
_cod_depositor_comments
'Adding full bibliography for 7706784--7706785.cif.'
_cod_database_code               7706785
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.699
_shelx_estimated_absorpt_t_min   0.558
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: Br1(0.534) Br2(0.294) Cl1(0.466) Cl2(0.706)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C32(H32),
 C31(H31), C30(H30), C29(H29), C28(H28), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2),
  C24(H24), C12(H12), C11(H11), C10(H10), C9(H9), C8(H8)
4.c Fitted hexagon refined as free rotating group:
 C14(C15,C16,C17,C18,C13), C27(C32,C31,C30,C29,C28), C1(C6,C5,C4,C3,C2),
 C7(C12,C11,C10,C9,C8)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              12199
_shelx_hkl_checksum              86044
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'