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_7244451
_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         'C30 H18 Au2 Cu2 N10, C2 H3 N'
_chemical_formula_sum            'C32 H21 Au2 Cu2 N11'
_chemical_formula_weight         1080.61
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-02-15 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                87.894(10)
_cell_angle_beta                 75.657(9)
_cell_angle_gamma                64.038(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7397(11)
_cell_length_b                   12.2661(14)
_cell_length_c                   13.3343(17)
_cell_measurement_reflns_used    3874
_cell_measurement_temperature    295(5)
_cell_measurement_theta_max      25.3760
_cell_measurement_theta_min      3.3570
_cell_volume                     1666.9(4)
_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      295(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2890
_diffrn_detector_type            Ruby
_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     19.00  63.00   1.00    7.50    --  -22.62  19.00-180.00   44
  2  \w     45.00  70.00   1.00    7.50    --   22.47 -70.00-107.00   25
  3  \w    -12.00  26.00   1.00    7.50    --  -22.62 -67.00 -45.80   38
  4  \w    -24.00  11.00   1.00    7.50    --  -22.62  19.00-180.00   35
  5  \w    -84.00  69.00   1.00    7.50    --   22.47 -69.00 -82.00  153
  6  \w    -27.00  63.00   1.00    7.50    --   22.47 -69.00 169.29   90
  7  \w    -85.00  69.00   1.00    7.50    --   22.47 -70.00  43.88  154
  8  \w    -59.00 -34.00   1.00    7.50    --   22.47 -69.00 169.29   25
  9  \w    -79.00  68.00   1.00    7.50    --   22.47 -70.00 125.36  147
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0210553000
_diffrn_orient_matrix_UB_12      0.0463885000
_diffrn_orient_matrix_UB_13      -0.0093769000
_diffrn_orient_matrix_UB_21      0.0020148000
_diffrn_orient_matrix_UB_22      0.0023106000
_diffrn_orient_matrix_UB_23      0.0525756000
_diffrn_orient_matrix_UB_31      0.0662576000
_diffrn_orient_matrix_UB_32      -0.0448067000
_diffrn_orient_matrix_UB_33      -0.0135287000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17920
_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         26.372
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24921
_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            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             1012
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4309
_reflns_number_total             6808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           preex1
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C1AA(H1AA), C3AA(H3AA), C2AA(H2AA), C4AA(H4AA), C5AA(H5AA),
 C20(H20), C8AA(H8AA), C6AA(H6AA), C5(H5), C6(H6), C9AA(H9AA), C2BA(H2BA),
 C0BA(H0BA), C1BA(H1BA), C11(H11), C3BA(H3BA)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.517
_oxdiff_exptl_absorpt_empirical_full_min 0.593