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_7244447
_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         'Au2 C4 N4, C4 Hg2 N4, C20 H16 Cu N4'
_chemical_formula_sum            'C28 H16 Au2 Cu Hg2 N12'
_chemical_formula_weight         1379.20
_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'
_symmetry_Int_Tables_number      72
_atom_sites_solution_primary     heavy
_audit_creation_date             2021-10-09
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7631(10)
_cell_length_b                   18.2826(19)
_cell_length_c                   22.013(2)
_cell_measurement_reflns_used    2462
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      28.4290
_cell_measurement_theta_min      4.3370
_cell_volume                     3124.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2890
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_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    -25.00   1.00   1.00   35.00    --  -10.53  37.00-120.00   26
  2  \w    -28.00  64.00   1.00   35.00    --  -10.53  37.00 -90.00   92
  3  \w    -67.00  14.00   1.00   35.00    --  -10.53 -37.00  60.00   81
;
_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      0.0661768000
_diffrn_orient_matrix_UB_12      -0.0239079000
_diffrn_orient_matrix_UB_13      0.0099358000
_diffrn_orient_matrix_UB_21      -0.0516063000
_diffrn_orient_matrix_UB_22      -0.0305573000
_diffrn_orient_matrix_UB_23      -0.0080221000
_diffrn_orient_matrix_UB_31      0.0360123000
_diffrn_orient_matrix_UB_32      0.0002424000
_diffrn_orient_matrix_UB_33      -0.0295996000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7482
_diffrn_reflns_theta_full        26.3686
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.866
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.9319
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432.6736
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.0624
_refine_diff_density_min         -2.2032
_refine_diff_density_rms         0.3825
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             5.7144
_refine_ls_goodness_of_fit_ref   1.0818
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    10
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1641
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.0554
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+27.4980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                1328
_reflns_number_total             1641
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           comp11
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244447
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.56
_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. Shared sites
{N4, C4}
3. Restrained distances
 C3a-N3
 1.17 with sigma of 0.002
 N3-C3a
 1.17 with sigma of 0.02
 C3b-N3
 1.17 with sigma of 0.02
 N2-C2
 1.17 with sigma of 0.02
4. Rigid bond restraints
 Hg1, C3a, N3, C3b
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Hg1, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Hg1 \\sim C3a \\sim N3 \\sim C3b: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C2 \\sim N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Hg1 \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C3a) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C3b) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N4) = Uanis(C4)
6. Others
 Fixed Sof: C3a(0.25) C2(0.25) C3b(0.25) C2(0.25) N4(0.25) C4(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C5(H5)
;
_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 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.708