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_7244449
_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(C2 Hg N2), C20 H16 Cu N4, 2(C2 Au N2)'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-14
_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                   7.7326(2)
_cell_length_b                   18.2993(6)
_cell_length_c                   22.0376(6)
_cell_measurement_reflns_used    7187
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      31.5060
_cell_measurement_theta_min      1.8270
_cell_volume                     3118.35(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      4.21 185.82   0.30   25.00    --   30.00  73.87 -25.79  606
  2  \w      4.21 185.82   0.30   25.00    --   30.00  73.87  64.21  606
  3  \w      4.21 185.82   0.30   25.00    --   30.00  73.87 154.21  606
  4  \w      4.21 185.82   0.30   25.00    --   30.00  73.87-115.79  606
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16425
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         1.848
_exptl_absorpt_coefficient_mu    19.901
_exptl_absorpt_correction_T_max  0.88652
_exptl_absorpt_correction_T_min  0.88652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.938
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_recrystallization_method 'recristallization from Ethyl acetate'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1641
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0271P)^2^+81.0322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1425
_reflns_number_total             1641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00964h2.cif
_cod_data_source_block           CuAuHg200k
_cod_depositor_comments
'Adding full bibliography for 7244437--7244451.cif.'
_cod_database_code               7244449
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N4, C0AA}
3. Restrained distances
 C3-N3
 1.16 with sigma of 0.02
 N3-C4
 1.16 with sigma of 0.02
 N2-C2
 1.16 with sigma of 0.02
4. Rigid bond restraints
 N2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N3, C3, Hg1, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Hg1, C2, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C4 \\sim N3 \\sim C3 \\sim Hg1 \\sim C0AA: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N2 \\sim C2 \\sim Hg1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(Hg1) \\sim
Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq: with
sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C0AA) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) = Uanis(C0AA)
6. Others
 Fixed Sof: C0AA(0.25) C2(0.25) C4(0.25) C3(0.25) N4(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9)
;
_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
- Detector area scaling
;