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_7244440
_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         'C4 Hg2 N4, Au2 C4 N4, C20 H16 Cu N4'
_chemical_formula_sum            'C28 H16 Au2 Cu Hg2 N12'
_chemical_formula_weight         1379.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-08 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8055(7)
_cell_length_b                   18.3374(16)
_cell_length_c                   22.0881(17)
_cell_measurement_reflns_used    2051
_cell_measurement_temperature    342.9(7)
_cell_measurement_theta_max      22.6970
_cell_measurement_theta_min      3.3920
_cell_volume                     3161.5(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 (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_environment      air
_diffrn_ambient_temperature      342.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_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    -92.00 -16.00   1.00   15.03    --  -29.89 -37.00   0.00   76
  2  \w    -56.00  43.00   1.00   15.03    --  -29.89  57.00 150.00   99
  3  \w   -103.00 -66.00   1.00   15.03    --  -29.89 -70.00  -1.41   37
  4  \w    -39.00 -13.00   1.00   15.03    --  -29.89 -70.00-170.03   26
  5  \w    -25.00   1.00   1.00   15.03    --  -29.89 -70.00  -1.41   26
  6  \w      0.00 102.00   1.00   15.03    --   31.14  70.00 -81.82  102
  7  \w     77.00 104.00   1.00   15.03    --   31.14  70.00-173.81   27
  8  \w     15.00  74.00   1.00   15.03    --   31.14  70.00-173.81   59
  9  \w     49.00  79.00   1.00   15.03    --   31.14  57.00 -90.00   30
 10  \w     58.00  84.00   1.00   15.03    --   31.14  70.00  23.30   26
 11  \w      3.00  55.00   1.00   15.03    --   31.14  70.00  23.30   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0824661000
_diffrn_orient_matrix_UB_12      0.0119655000
_diffrn_orient_matrix_UB_13      0.0091416000
_diffrn_orient_matrix_UB_21      -0.0381760000
_diffrn_orient_matrix_UB_22      -0.0263051000
_diffrn_orient_matrix_UB_23      -0.0192951000
_diffrn_orient_matrix_UB_31      0.0007202000
_diffrn_orient_matrix_UB_32      -0.0257291000
_diffrn_orient_matrix_UB_33      0.0239699000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64285
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.898
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1267
_reflns_number_total             1663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           CuAuHg343k
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244440
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.088
_shelx_estimated_absorpt_t_min   0.057
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C3(0.25) C2(0.25) C4A(0.25) C4B(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C6(H6), C8(H8)
;
_shelx_res_checksum              51795
_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 1.388
_oxdiff_exptl_absorpt_empirical_full_min 0.683