Homo- and hetero-metallophilicity-driven synthesis of highly emissive and stimuli-responsive Au(I)-Cu(I) double salts.
Kobayashi, Ryosuke; Yumura, Takashi; Imoto, Hiroaki; Naka, Kensuke; Chemical communications (Cambridge, England) 57 (2021) 5382–5385; doi:10.1039/d1cc01316e

data_7128373
_publ_section_title
;
 Homo- and hetero-metallophilicity-driven synthesis of highly emissive and
 stimuli-responsive Au(I)-Cu(I) double salts.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5382
_journal_page_last               5385
_journal_paper_doi               10.1039/d1cc01316e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C50 H44 As4 Au2 Cl4 Cu2'
_chemical_formula_sum            'C50 H44 As4 Au2 Cl4 Cu2'
_chemical_formula_weight         1607.34
_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     iterative
_audit_creation_date             2020-12-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.380(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.036(4)
_cell_length_b                   15.6209(18)
_cell_length_c                   16.343(3)
_cell_measurement_reflns_used    4514
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      54.971
_cell_measurement_theta_min      6.133
_cell_volume                     5124.0(15)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'XtaLAB mini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26763
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.067
_exptl_absorpt_coefficient_mu    9.333
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS(Rigaku, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and methanol by solvent layering.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.384
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5856
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0618P)^2^+13.5666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3803
_reflns_number_total             5856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01316e2.cif
_cod_data_source_block           As-AuCuCl_c
_cod_depositor_comments
'Adding full bibliography for 7128370--7128375.cif.'
_cod_original_cell_volume        5124.0(13)
_cod_database_code               7128373
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.257
_shelx_estimated_absorpt_t_min   0.257
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C24B-C19B \\sim C24A-C19A
 with sigma of 0.02
 C24B-C23B \\sim C24A-C23A
 with sigma of 0.02
 C19B-C20B \\sim C19A-C20A
 with sigma of 0.02
 As2-C19B \\sim As2-C19A
 with sigma of 0.02
 C19B-C21B \\sim C19A-C21A
 with sigma of 0.04
 C20B-C21B \\sim C20A-C21A
 with sigma of 0.02
 C21B-C22B \\sim C21A-C22A
 with sigma of 0.02
 C21B-C23B \\sim C21A-C23A
 with sigma of 0.04
 C19B-C23B \\sim C19A-C23A
 with sigma of 0.04
 C22B-C23B \\sim C22A-C23A
 with sigma of 0.02
 C20B-C22B \\sim C20A-C22A
 with sigma of 0.04
 As2-C24B \\sim As2-C24A
 with sigma of 0.04
 As2-C20B \\sim As2-C20A
 with sigma of 0.04
 C24B-C20B \\sim C24A-C20A
 with sigma of 0.04
 C24B-C22B \\sim C24A-C22A
 with sigma of 0.04
3. Restrained planarity
 C20A, C19A, C24A, C23A, C22A, C21A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C20B \\sim C20A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Rigid body (RIGU) restrains
 C19B, C22B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19B, C24B, C23B, C22B, C21B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C9A, C8A, C10A, C12A, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7B, C8B, C9B, C10B, C11B, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24B, C19B, C22B, C20B, C23B, C21B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19A, C20A, C23A, C21A, C24A, C22A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=
 Sof(H11B)=Sof(C12B)=Sof(H12B)=1-FVAR(1)
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=FVAR(1)
 Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=1-FVAR(2)
 Sof(C24B)=Sof(H24B)=Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
7.b Aromatic/amide H refined with riding coordinates:
 C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2),
 C24B(H24B), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C8A(H8A), C9A(H9A),
  C10A(H10A), C11A(H11A), C12A(H12A), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A), C24A(H24A)
7.c Fitted hexagon refined as free rotating group:
 C7B(C8B,C9B,C10B,C11B,C12B), C13(C14,C15,C16,C17,C18), C24B(C19B,C20B,C21B,
 C22B,C23B), C7A(C8A,C9A,C10A,C11A,C12A), C19A(C20A,C21A,C22A,C23A,C24A)
;
_shelx_res_checksum              51382
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre.'
_olex2_submission_special_instructions 'No special instructions were received'