#------------------------------------------------------------------------------
#$Date: 2022-05-27 01:52:31 +0300 (Fri, 27 May 2022) $
#$Revision: 275663 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/03/7710358.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7710358
loop_
_publ_author_name
'Pinto, Andrea'
'Ward, Jas S.'
'Rissanen, Kari'
'Smith, Martin'
'Rodríguez, Laura'
_publ_section_title
;
 Aggregation of gold(i) complexes: phosphorescence vs. singlet oxygen
 production
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01154A
_journal_year                    2022
_chemical_formula_moiety         'C66 H54 Au Cl6 N6 P2, 4(C H4 O), Cl'
_chemical_formula_sum            'C70 H70 Au Cl7 N6 O4 P2'
_chemical_formula_weight         1566.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-11 deposited with the CCDC.	2022-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0915(6)
_cell_length_b                   14.5770(4)
_cell_length_c                   24.3861(7)
_cell_measurement_reflns_used    10888
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.999
_cell_measurement_theta_min      0.407
_cell_volume                     6825.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.748
_exptl_absorpt_coefficient_mu    2.530
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0909 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.6745. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8486
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.278
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0465
_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/[σ²(Fo²)+(0.0438P)²+26.7836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7244
_reflns_number_total             8486
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01154a2.cif
_cod_data_source_block           5
_cod_database_code               7710358
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 C53, C54, C55, C56, C57, C58, C59, C60, C61, C62
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C33, C34, C35, C36, C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C31(H31A,H31B), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 N12(H12), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
 N32(H32), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), N52(H52),
  C54(H54), C55(H55), C58(H58), C59(H59), C60(H60), C61(H61)
3.c Idealised Me refined as rotating group:
 C102(H10A,H10B,H10C), C112(H11C,H11D,H11E)
3.d Idealised tetrahedral OH refined as rotating group:
 O101(H101), O111(H111)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.5000 0.5000 0.5000 0.03142(8) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.32642(18) 0.7500 0.1003(11) Uani 1 2 d S T P . .
P1 P 0.53415(5) 0.42450(7) 0.58603(4) 0.0273(2) Uani 1 1 d . . . . .
C11 C 0.4607(2) 0.3678(3) 0.6038(2) 0.0346(9) Uani 1 1 d . . . . .
H11A H 0.4291 0.3398 0.5688 0.042 Uiso 1 1 calc R . . . .
H11B H 0.4788 0.3183 0.6321 0.042 Uiso 1 1 calc R . . . .
N12 N 0.42253(19) 0.4329(3) 0.62727(17) 0.0372(8) Uani 1 1 d . . . . .
H12 H 0.4338 0.4389 0.6648 0.045 Uiso 1 1 calc R . . . .
C13 C 0.3692(2) 0.4861(3) 0.5938(2) 0.0316(9) Uani 1 1 d . . . . .
C14 C 0.3469(2) 0.4787(3) 0.5349(2) 0.0349(9) Uani 1 1 d . . . . .
H14 H 0.3693 0.4365 0.5164 0.042 Uiso 1 1 calc R . . . .
C15 C 0.2915(2) 0.5326(4) 0.5016(2) 0.0394(10) Uani 1 1 d . . . . .
H15 H 0.2767 0.5260 0.4610 0.047 Uiso 1 1 calc R . . . .
C16 C 0.2592(2) 0.5938(3) 0.5269(2) 0.0419(11) Uani 1 1 d . . . . .
C17 C 0.2804(2) 0.6064(3) 0.5875(2) 0.0395(10) Uani 1 1 d . . . . .
C18 C 0.2483(3) 0.6700(4) 0.6152(3) 0.0578(15) Uani 1 1 d . . . . .
H18 H 0.2111 0.7068 0.5929 0.069 Uiso 1 1 calc R . . . .
C19 C 0.2696(4) 0.6800(4) 0.6741(3) 0.0690(19) Uani 1 1 d . . . . .
H19 H 0.2469 0.7225 0.6921 0.083 Uiso 1 1 calc R . . . .
C20 C 0.3249(4) 0.6271(4) 0.7068(3) 0.0640(17) Uani 1 1 d . . . . .
H20 H 0.3402 0.6347 0.7473 0.077 Uiso 1 1 calc R . . . .
C21 C 0.3576(3) 0.5644(4) 0.6818(2) 0.0487(12) Uani 1 1 d . . . . .
H21 H 0.3952 0.5292 0.7051 0.058 Uiso 1 1 calc R . . . .
C22 C 0.3361(2) 0.5514(3) 0.6215(2) 0.0371(10) Uani 1 1 d . . . . .
Cl23 Cl 0.18942(7) 0.65611(10) 0.48385(8) 0.0630(4) Uani 1 1 d . . . . .
C31 C 0.5958(2) 0.3282(3) 0.5894(2) 0.0353(9) Uani 1 1 d . . . . .
H31A H 0.6318 0.3475 0.5714 0.042 Uiso 1 1 calc R . . . .
H31B H 0.6196 0.3131 0.6300 0.042 Uiso 1 1 calc R . . . .
N32 N 0.5607(2) 0.2483(3) 0.56063(18) 0.0421(9) Uani 1 1 d . . . . .
H32 H 0.5549 0.2017 0.5817 0.051 Uiso 1 1 calc R . . . .
C33 C 0.5353(2) 0.2402(3) 0.50143(19) 0.0321(8) Uani 1 1 d . U . . .
C34 C 0.5581(2) 0.2976(3) 0.4658(2) 0.0405(10) Uani 1 1 d . U . . .
H34 H 0.5892 0.3462 0.4819 0.049 Uiso 1 1 calc R . . . .
C35 C 0.5358(3) 0.2852(3) 0.4056(2) 0.0408(10) Uani 1 1 d . U . . .
H35 H 0.5538 0.3230 0.3816 0.049 Uiso 1 1 calc R . . . .
C36 C 0.4885(3) 0.2190(4) 0.3826(2) 0.0484(11) Uani 1 1 d . U . . .
C37 C 0.4608(3) 0.1609(4) 0.4161(2) 0.0435(10) Uani 1 1 d . U . . .
C38 C 0.4101(4) 0.0926(5) 0.3938(3) 0.0718(18) Uani 1 1 d . U . . .
H38 H 0.3952 0.0842 0.3534 0.086 Uiso 1 1 calc R . . . .
C39 C 0.3807(4) 0.0377(5) 0.4259(3) 0.0750(19) Uani 1 1 d . U . . .
H39 H 0.3457 -0.0061 0.4089 0.090 Uiso 1 1 calc R . . . .
C40 C 0.4064(4) 0.0507(5) 0.4868(4) 0.078(2) Uani 1 1 d . U . . .
H40 H 0.3885 0.0131 0.5110 0.093 Uiso 1 1 calc R . . . .
C41 C 0.4554(3) 0.1148(4) 0.5113(3) 0.0521(13) Uani 1 1 d . U . . .
H41 H 0.4707 0.1211 0.5518 0.062 Uiso 1 1 calc R . . . .
C42 C 0.4842(2) 0.1725(3) 0.4771(2) 0.0411(10) Uani 1 1 d . U . . .
Cl43 Cl 0.46195(10) 0.20761(16) 0.30810(7) 0.0787(5) Uani 1 1 d . . . . .
C51 C 0.5759(2) 0.4910(3) 0.65271(19) 0.0348(9) Uani 1 1 d . . . . .
H51A H 0.5577 0.5545 0.6480 0.042 Uiso 1 1 calc R . . . .
H51B H 0.5634 0.4629 0.6853 0.042 Uiso 1 1 calc R . . . .
N52 N 0.6501(2) 0.4934(3) 0.66567(18) 0.0418(9) Uani 1 1 d . . . . .
H52 H 0.6746 0.4549 0.6916 0.050 Uiso 1 1 calc R . . . .
C53 C 0.6856(2) 0.5524(3) 0.64009(19) 0.0333(9) Uani 1 1 d . U . . .
C54 C 0.6535(3) 0.6261(3) 0.6077(2) 0.0402(10) Uani 1 1 d . U . . .
H54 H 0.6048 0.6346 0.6005 0.048 Uiso 1 1 calc R . . . .
C55 C 0.6917(3) 0.6894(4) 0.5848(2) 0.0505(12) Uani 1 1 d . U . . .
H55 H 0.6693 0.7408 0.5632 0.061 Uiso 1 1 calc R . . . .
C56 C 0.7612(3) 0.6750(5) 0.5944(3) 0.0578(13) Uani 1 1 d . U . . .
C57 C 0.7970(3) 0.5991(4) 0.6242(2) 0.0505(11) Uani 1 1 d . U . . .
C58 C 0.8681(3) 0.5783(6) 0.6315(3) 0.0736(17) Uani 1 1 d . U . . .
H58 H 0.8948 0.6222 0.6183 0.088 Uiso 1 1 calc R . . . .
C59 C 0.9002(4) 0.5030(6) 0.6553(3) 0.0796(19) Uani 1 1 d . U . . .
H59 H 0.9476 0.4922 0.6578 0.096 Uiso 1 1 calc R . . . .
C60 C 0.8607(3) 0.4373(6) 0.6774(3) 0.0805(19) Uani 1 1 d . U . . .
H60 H 0.8821 0.3822 0.6948 0.097 Uiso 1 1 calc R . . . .
C61 C 0.7918(3) 0.4548(5) 0.6731(3) 0.0552(13) Uani 1 1 d . U . . .
H61 H 0.7665 0.4111 0.6879 0.066 Uiso 1 1 calc R . . . .
C62 C 0.7579(2) 0.5352(4) 0.6475(2) 0.0423(10) Uani 1 1 d . U . . .
Cl63 Cl 0.80714(12) 0.75746(18) 0.56835(10) 0.1039(8) Uani 1 1 d . . . . .
O101 O 0.6761(3) 0.3390(4) 0.7421(2) 0.0864(16) Uani 1 1 d . . . . .
H101 H 0.6363 0.3370 0.7466 0.130 Uiso 1 1 calc GR . . . .
C102 C 0.7261(6) 0.3368(9) 0.7951(3) 0.125(4) Uani 1 1 d . . . . .
H10A H 0.7654 0.3760 0.7943 0.187 Uiso 1 1 calc GR . . . .
H10B H 0.7424 0.2737 0.8041 0.187 Uiso 1 1 calc GR . . . .
H10C H 0.7059 0.3592 0.8246 0.187 Uiso 1 1 calc GR . . . .
O111 O 0.5464(4) 0.1744(5) 0.6723(3) 0.119(3) Uani 1 1 d . . . . .
H111 H 0.5488 0.2232 0.6911 0.178 Uiso 1 1 calc GR . . . .
C112 C 0.5931(4) 0.1128(5) 0.7036(4) 0.085(2) Uani 1 1 d . . . . .
H11C H 0.6167 0.1390 0.7413 0.128 Uiso 1 1 calc GR . . . .
H11D H 0.6275 0.0984 0.6836 0.128 Uiso 1 1 calc GR . . . .
H11E H 0.5687 0.0566 0.7085 0.128 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au1 P1 180.0 5_666 . ?
C11 P1 Au1 112.66(15) . . ?
C11 P1 C31 102.7(2) . . ?
C11 P1 C51 102.3(2) . . ?
C31 P1 Au1 114.82(15) . . ?
C31 P1 C51 103.3(2) . . ?
C51 P1 Au1 119.03(15) . . ?
N12 C11 P1 110.7(3) . . ?
C13 N12 C11 123.2(4) . . ?
N12 C13 C14 122.0(4) . . ?
N12 C13 C22 118.8(4) . . ?
C14 C13 C22 119.3(4) . . ?
C13 C14 C15 121.1(4) . . ?
C16 C15 C14 120.5(5) . . ?
C15 C16 C17 121.5(4) . . ?
C15 C16 Cl23 118.5(4) . . ?
C17 C16 Cl23 120.0(4) . . ?
C16 C17 C22 118.2(4) . . ?
C18 C17 C16 122.9(5) . . ?
C18 C17 C22 118.9(5) . . ?
C19 C18 C17 121.5(6) . . ?
C18 C19 C20 119.2(6) . . ?
C21 C20 C19 121.4(6) . . ?
C20 C21 C22 120.7(6) . . ?
C17 C22 C13 119.4(4) . . ?
C21 C22 C13 122.2(5) . . ?
C21 C22 C17 118.3(5) . . ?
N32 C31 P1 111.5(3) . . ?
C33 N32 C31 123.7(4) . . ?
N32 C33 C42 119.5(4) . . ?
C34 C33 N32 121.1(4) . . ?
C34 C33 C42 119.4(5) . . ?
C33 C34 C35 121.0(5) . . ?
C36 C35 C34 119.4(5) . . ?
C35 C36 C37 122.6(5) . . ?
C35 C36 Cl43 117.6(4) . . ?
C37 C36 Cl43 119.8(4) . . ?
C36 C37 C38 124.6(6) . . ?
C36 C37 C42 118.0(5) . . ?
C38 C37 C42 117.4(5) . . ?
C39 C38 C37 125.2(7) . . ?
C38 C39 C40 115.5(6) . . ?
C41 C40 C39 122.5(7) . . ?
C40 C41 C42 121.0(6) . . ?
C33 C42 C37 119.5(5) . . ?
C41 C42 C33 122.2(5) . . ?
C41 C42 C37 118.3(5) . . ?
N52 C51 P1 112.2(3) . . ?
C53 N52 C51 124.0(4) . . ?
N52 C53 C62 118.3(4) . . ?
C54 C53 N52 122.1(4) . . ?
C54 C53 C62 119.7(4) . . ?
C53 C54 C55 121.3(5) . . ?
C56 C55 C54 118.6(6) . . ?
C55 C56 C57 123.6(5) . . ?
C55 C56 Cl63 117.2(5) . . ?
C57 C56 Cl63 119.2(4) . . ?
C56 C57 C58 125.3(6) . . ?
C56 C57 C62 117.4(5) . . ?
C58 C57 C62 117.3(6) . . ?
C59 C58 C57 125.2(7) . . ?
C58 C59 C60 117.8(7) . . ?
C61 C60 C59 119.8(8) . . ?
C60 C61 C62 122.1(7) . . ?
C53 C62 C57 119.2(5) . . ?
C61 C62 C53 122.9(5) . . ?
C61 C62 C57 117.8(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.2881(10) 5_666 ?
Au1 P1 2.2881(10) . ?
P1 C11 1.851(4) . ?
P1 C31 1.858(4) . ?
P1 C51 1.867(4) . ?
C11 N12 1.440(6) . ?
N12 C13 1.379(6) . ?
C13 C14 1.379(7) . ?
C13 C22 1.438(6) . ?
C14 C15 1.408(7) . ?
C15 C16 1.356(7) . ?
C16 C17 1.424(7) . ?
C16 Cl23 1.740(5) . ?
C17 C18 1.410(7) . ?
C17 C22 1.428(7) . ?
C18 C19 1.379(10) . ?
C19 C20 1.394(10) . ?
C20 C21 1.370(8) . ?
C21 C22 1.417(7) . ?
C31 N32 1.434(6) . ?
N32 C33 1.387(6) . ?
C33 C34 1.378(6) . ?
C33 C42 1.423(7) . ?
C34 C35 1.413(7) . ?
C35 C36 1.355(7) . ?
C36 C37 1.401(8) . ?
C36 Cl43 1.743(6) . ?
C37 C38 1.413(8) . ?
C37 C42 1.432(7) . ?
C38 C39 1.367(10) . ?
C39 C40 1.434(11) . ?
C40 C41 1.362(8) . ?
C41 C42 1.421(7) . ?
C51 N52 1.430(6) . ?
N52 C53 1.377(6) . ?
C53 C54 1.375(7) . ?
C53 C62 1.434(6) . ?
C54 C55 1.415(7) . ?
C55 C56 1.363(8) . ?
C56 C57 1.401(9) . ?
C56 Cl63 1.745(6) . ?
C57 C58 1.420(8) . ?
C57 C62 1.439(7) . ?
C58 C59 1.318(11) . ?
C59 C60 1.444(12) . ?
C60 C61 1.381(8) . ?
C61 C62 1.405(9) . ?
O101 C102 1.385(9) . ?
O111 C112 1.359(9) . ?
