Aggregation of gold(i) complexes: phosphorescence vs. singlet oxygen production
Pinto, Andrea; Ward, Jas S.; Rissanen, Kari; Smith, Martin; Rodríguez, Laura; Dalton Transactions  (2022) –; doi:10.1039/D2DT01154A

data_7710358
_publ_section_title
;
 Aggregation of gold(i) complexes: phosphorescence vs. singlet oxygen
 production
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01154A
_journal_year                    2022
_chemical_formula_moiety         'C66 H54 Au Cl6 N6 P2, 4(C H4 O), Cl'
_chemical_formula_sum            'C70 H70 Au Cl7 N6 O4 P2'
_chemical_formula_weight         1566.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-11 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0915(6)
_cell_length_b                   14.5770(4)
_cell_length_c                   24.3861(7)
_cell_measurement_reflns_used    10888
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      0.407
_cell_volume                     6825.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.748
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0909 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.6745. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8486
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+26.7836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7244
_reflns_number_total             8486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01154a2.cif
_cod_data_source_block           5
_cod_database_code               7710358
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 C53, C54, C55, C56, C57, C58, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C33, C34, C35, C36, C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C31(H31A,H31B), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 N12(H12), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
 N32(H32), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), N52(H52),
  C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61)
3.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C112(H11C,H11D,H11E)
3.d Idealised tetrahedral OH refined as rotating group:
 O101(H101), O111(H111)
;
_shelx_res_checksum              22135
_olex2_submission_special_instructions 'No special instructions were received'