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_7244448
_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         '2(Au C2 N2), C24 H26 Cu N4 O, 2(H2 O)'
_chemical_formula_sum            'C28 H30 Au2 Cu N8 O3'
_chemical_formula_weight         984.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                98.846(5)
_cell_angle_beta                 101.818(5)
_cell_angle_gamma                97.377(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1876(7)
_cell_length_b                   11.8612(8)
_cell_length_c                   12.4954(7)
_cell_measurement_reflns_used    4158
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      31.5220
_cell_measurement_theta_min      3.7010
_cell_volume                     1581.60(18)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.974
_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    -10.00  16.00   1.00   30.00    --  -17.99  40.00 106.00   26
  2  \w    -33.00  44.00   1.00   30.00    --   19.55 -40.00 -47.00   77
  3  \w     18.00  44.00   1.00   30.00    --   19.55  40.00 106.00   26
  4  \w    -33.00  -1.00   1.00   30.00    --  -17.99 -70.00 128.56   32
  5  \w    -87.00   0.00   1.00   30.00    --  -17.99 -68.00  37.74   87
  6  \w    -49.00  13.00   1.00   30.00    --  -17.99 -70.00 -55.21   62
  7  \w    -55.00  37.00   1.00   30.00    --   19.55 -37.00  90.00   92
  8  \w     -9.00  59.00   1.00   30.00    --   19.55  62.00 -33.64   68
  9  \w     -8.00  42.00   1.00   30.00    --   19.55  66.00-138.89   50
;
_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  0.0592
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18507
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.390
_exptl_absorpt_coefficient_mu    9.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56609
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ammonia soutions'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0036P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4363
_reflns_number_total             6290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           comp4
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244448
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.407
_shelx_estimated_absorpt_t_min   0.046
_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, All O(H,H) groups
2.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B)
2.b Rotating group:
 O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C19(H19), C26(H26), C20(H20), C14(H14), C12(H12), C8(H8),
 C11(H11), C7(H7), C24(H24), C23(H23)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C27(H27A,H27B,
 H27C)
;
_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
;