Noncovalent interactions in gold(iii) tetrakis(4-butoxyphenyl)porphyrinate structures
Bardina, Elena E.; Makotchenko, Eugeniya V.; Birin, Kirill P.; Baidina, Iraida A.; Sukhikh, Taisiya S.; Novikov, Alexander S.; Gorbunova, Yulia G.; Tsivadze, Aslan Yu.; Gushchin, Artem L.; CrystEngComm 25 (2023) 4755–4767; doi:10.1039/D3CE00428G

data_7247090
_publ_section_title
;
 Noncovalent interactions in gold(iii)
 tetrakis(4-butoxyphenyl)porphyrinate structures
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4755
_journal_page_last               4767
_journal_paper_doi               10.1039/D3CE00428G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C60 H60 Au N4 O4, Au Cl4'
_chemical_formula_sum            'C60 H60 Au2 Cl4 N4 O4'
_chemical_formula_weight         1436.85
_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             2022-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-12 deposited with the CCDC.	2023-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                77.941(3)
_cell_angle_beta                 82.828(3)
_cell_angle_gamma                75.258(3)
_cell_formula_units_Z            4
_cell_length_a                   16.7951(17)
_cell_length_b                   17.6474(17)
_cell_length_c                   19.8427(18)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.27
_cell_volume                     5546.1(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77263
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.710
_diffrn_reflns_theta_min         1.665
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1149 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.8916. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.725
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1410
_refine_ls_number_reflns         21056
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0353P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15533
_reflns_number_total             21056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00428g7.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7247089--7247091.cif.'
_cod_database_code               7247090
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C24 = O2A-C24
 1.37 with sigma of 0.02
 O2-C2B1 = O2A-C2B5
 1.42 with sigma of 0.02
 C2B2-C2B1 = C2B5-C2B6 = C2B7-C2B6 = C2B8-C2B7 = C2B3-C2B2 = C2B3-C2B4
 1.54 with sigma of 0.02
 C4B2-C4B1 = C4B1-C4B5 = C4B3-C4B2 = C4B6-C4B5 = C4B7-C4B6 = C4B4-C4B3
 1.54 with sigma of 0.02
 C7B6-C7B5 = C7B2-C7B1 = C7B3-C7B2 = C7B7-C7B6 = C7B8-C7B7 = C7B4-C7B3
 1.54 with sigma of 0.02
 O7-C7B5 = O7-C7B1
 1.42 with sigma of 0.02
 C2B6-C2B8
 2.5 with sigma of 0.04
 C2B2-C2B4
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C7B5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7B6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C2B7) = Uiso(C2B3) = Uiso(C2B8) = Uiso(C2B4)
4. Others
 Sof(H5BG)=Sof(H5BH)=Sof(C5B5)=Sof(H5BL)=Sof(H5BM)=Sof(H5BN)=Sof(C7B5)=
 Sof(H7BJ)=Sof(H7BK)=Sof(C7B6)=Sof(H7BL)=Sof(H7BM)=Sof(C7B7)=Sof(H7BN)=
 Sof(H7BO)=Sof(C7B8)=Sof(H7BP)=Sof(H7BQ)=Sof(H7BR)=1-FVAR(1)
 Sof(H5BE)=Sof(H5BF)=Sof(C5B4)=Sof(H5BI)=Sof(H5BJ)=Sof(H5BK)=Sof(C7B1)=
 Sof(H7BA)=Sof(H7BB)=Sof(C7B2)=Sof(H7BC)=Sof(H7BD)=Sof(C7B3)=Sof(H7BE)=
 Sof(H7BF)=Sof(C7B4)=Sof(H7BG)=Sof(H7BH)=Sof(H7BI)=FVAR(1)
 Fixed Sof: O2(0.5) O2A(0.5) H4BA(0.5) H4BB(0.5) H4BC(0.5) H4BD(0.5) C2B1(0.5)
 H2BA(0.5) H2BB(0.5) C2B2(0.5) H2BC(0.5) H2BD(0.5) C2B3(0.5) H2BE(0.5)
 H2BF(0.5) C2B4(0.5) H2BG(0.5) H2BH(0.5) H2BI(0.5) C4B2(0.5) H4BE(0.5)
 H4BF(0.5) C4B3(0.5) H4BG(0.5) H4BH(0.5) C4B4(0.5) H4BI(0.5) H4BJ(0.5)
 H4BK(0.5) C2B5(0.5) H2BJ(0.5) H2BK(0.5) C2B6(0.5) H2BL(0.5) H2BM(0.5)
 C2B7(0.5) H2BN(0.5) H2BO(0.5) C2B8(0.5) H2BP(0.5) H2BQ(0.5) H2BR(0.5)
 C4B5(0.5) H4BL(0.5) H4BM(0.5) C4B6(0.5) H4BN(0.5) H4BO(0.5) C4B7(0.5)
 H4BP(0.5) H4BQ(0.5) H4BR(0.5) H8BG(0.5) H8BH(0.5) H8BE(0.5) H8BF(0.5)
 C8B4(0.5) H8BI(0.5) H8BJ(0.5) H8BK(0.5) C8B5(0.5) H8BL(0.5) H8BM(0.5) H8BN(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1B1(H1BA,H1BB), C1B2(H1BC,H1BD), C1B3(H1BE,H1BF), C3B1(H3BA,H3BB), C3B2(H3BC,
 H3BD), C3B3(H3BE,H3BF), C4B1(H4BA,H4BB), C4B1(H4BC,H4BD), C2B1(H2BA,H2BB),
 C2B2(H2BC,H2BD), C2B3(H2BE,H2BF), C4B2(H4BE,H4BF), C4B3(H4BG,H4BH), C2B5(H2BJ,
 H2BK), C2B6(H2BL,H2BM), C2B7(H2BN,H2BO), C4B5(H4BL,H4BM), C4B6(H4BN,H4BO),
 C5B1(H5BA,H5BB), C5B2(H5BC,H5BD), C5B3(H5BG,H5BH), C5B3(H5BE,H5BF), C6B1(H6BA,
 H6BB), C6B2(H6BC,H6BD), C6B3(H6BE,H6BF), C8B1(H8BA,H8BB), C8B2(H8BC,H8BD),
 C8B3(H8BG,H8BH), C8B3(H8BE,H8BF), C7B1(H7BA,H7BB), C7B2(H7BC,H7BD), C7B3(H7BE,
 H7BF), C7B5(H7BJ,H7BK), C7B6(H7BL,H7BM), C7B7(H7BN,H7BO)
5.b Me refined with riding coordinates:
 C2B4(H2BG,H2BH,H2BI), C4B4(H4BI,H4BJ,H4BK), C2B8(H2BP,H2BQ,H2BR), C4B7(H4BP,
 H4BQ,H4BR), C7B4(H7BG,H7BH,H7BI), C8B4(H8BI,H8BJ,H8BK), C7B8(H7BP,H7BQ,H7BR),
 C8B5(H8BL,H8BM,H8BN)
5.c Aromatic/amide H refined with riding coordinates:
 C1C(H1C), C1D(H1D), C2C(H2C), C2D(H2D), C3C(H3C), C3D(H3D), C4C(H4C),
 C4D(H4D), C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
  C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
 C45(H45), C46(H46), C5C(H5C), C5D(H5D), C6C(H6C), C6D(H6D), C7C(H7C), C7D(H7D),
  C8C(H8C), C8D(H8D), C52(H52), C53(H53), C55(H55), C56(H56), C62(H62),
 C63(H63), C65(H65), C66(H66), C72(H72), C73(H73), C75(H75), C76(H76), C82(H82),
  C83(H83), C85(H85), C86(H86)
5.d Idealised Me refined as rotating group:
 C1B4(H1BG,H1BH,H1BI), C3B4(H3BG,H3BH,H3BI), C6B4(H6BG,H6BH,H6BI), C5B4(H5BI,
 H5BJ,H5BK), C5B5(H5BL,H5BM,H5BN)
;
_shelx_res_checksum              89198
_olex2_submission_special_instructions 'No special instructions were received'