Crystal engineering of aurophilic supramolecular architectures and coordination polymers based on butterfly-like copper–dicyanoaurate complexes: vapochromism, P–T behaviour and multi-metallic cocrystal formation
Priola, Emanuele; Curetti, Nadia; Marabello, Domenica; Andreo, Jacopo; Giordana, Alessia; Andreo, Luca; Benna, Piera; Freire, Paulo Tarso Cavalcante; Benzi, Paola; Operti, Lorenza; Diana, Eliano; CrystEngComm 24 (2022) 2336–2348; doi:10.1039/D1CE00964H

data_7244443
_publ_section_title
;
 Crystal engineering of aurophilic supramolecular architectures and
 coordination polymers based on butterfly-like copper--dicyanoaurate
 complexes: vapochromism, P--T behaviour and multi-metallic cocrystal
 formation
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2336
_journal_page_last               2348
_journal_paper_doi               10.1039/D1CE00964H
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C42 H24 Au2 Cu F6 N10, C2 H6 O S'
_chemical_formula_sum            'C44 H30 Au2 Cu F6 N10 O S'
_chemical_formula_weight         1318.31
_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
_audit_creation_date             2021-10-21
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2022-01-23 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.178(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8380(15)
_cell_length_b                   13.0922(5)
_cell_length_c                   16.6160(10)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      23.0800
_cell_measurement_theta_min      3.7820
_cell_volume                     4413.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     31.00  57.00   1.00   25.00    --  -10.13  37.00 -30.00   26
  2  \w    -12.00  86.00   1.00   25.00    --   11.30  37.00 120.00   98
  3  \w    -41.00 -15.00   1.00   25.00    --   11.30 -37.00  60.00   26
  4  \w    -56.00  39.00   1.00   25.00    --   11.30 -57.00  30.00   95
  5  \w     11.00  64.00   1.00   25.00    --   11.30  57.00 -90.00   53
  6  \w    -60.00 -34.00   1.00   25.00    --   11.30 -37.00-120.00   26
  7  \w     -5.00  83.00   1.00   25.00    --   11.30  57.00-180.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.305
_exptl_absorpt_coefficient_mu    7.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_preparation       'recristallization from DMSO'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4518
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0280P)^2^+6.5468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3206
_reflns_number_total             4518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           comp8
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244443
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.186
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1A-O1 \\sim O1-C22
 with sigma of 0.001
 C21-C18 \\sim C21-F2A \\sim C21-F1A \\sim C21-F3A
 with sigma of 0.001
 F2A-F1A \\sim F2A-F3A \\sim F1A-F3A
 with sigma of 0.002
 C18-F2A \\sim C18-F2B
 with sigma of 0.04
 F2A-F1A \\sim F2B-F1B
 with sigma of 0.04
 C18-F3A \\sim C18-F3B
 with sigma of 0.04
 C18-F1A \\sim C18-F1B
 with sigma of 0.04
 F1A-F3A \\sim F1B-F3B
 with sigma of 0.04
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
3. Rigid bond restraints
 F3A, C21, F1A, F2A, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N1, Cu1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu1, N1, C1, Au1, C2, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F3A \\sim C21 \\sim F2A \\sim F1A \\sim C18: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
C1 \\sim N1 \\sim Cu1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Cu1 \\sim N1 \\sim C1 \\sim Au1 \\sim C2 \\sim N2: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(F3A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(F1A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cu1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(Au1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 S1, O1, C22, C1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F2A, F3A, F1A, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, F2A, F1A, F3A, F2B, F1B, F3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: F2A(0.55) F1A(0.55) F3A(0.55) S1(0.5) O1(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) F2B(0.45) F1B(0.45)
 F3B(0.45)
7.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C10(H10), C19(H19), C16(H16), C13(H13), C12(H12), C11(H11),
 C17(H17), C3(H3), C6(H6), C4(H4), C5(H5)
7.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              72560
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;