#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:39:33 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286104 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/70/7247021.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_7247021
loop_
_publ_author_name
'Brown, Matthew L.'
'Karpiuk, Thomas E.'
'Leznoff, Daniel B.'
_publ_section_title
;
 Emissive lanthanide dicyanoaurate coordination polymers with
 2,2′-bipyridine dioxide antenna groups and their hydration states
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4658
_journal_page_last               4668
_journal_paper_doi               10.1039/D3CE00583F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
;
0.5(C52 H32 Au6 Tb2 N20 O8), 2(C2 H6 O), 2(H2 O)
;
_chemical_formula_sum            'C30 H32 Au3 N10 O8 Tb'
_chemical_formula_weight         1410.47
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-01 deposited with the CCDC.	2023-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.626(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8870(7)
_cell_length_b                   18.0157(13)
_cell_length_c                   19.5884(14)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.948
_cell_measurement_theta_min      2.307
_cell_volume                     3787.9(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 & ShelxLE'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67387
_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         26.372
_diffrn_reflns_theta_min         2.109
_diffrn_source                   'Sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.487
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.3665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1635 before and 0.0828 after correction. 
The Ratio of minimum to maximum transmission is 0.4904. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2592
_exptl_crystal_preparation
'Slow evaporation from 50:50 EtOH:H2O,Luminescent'
_exptl_crystal_recrystallization_method 'Slow evaporation from 50:50 EtOH:H2O'
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.124
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3878
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0362
_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/[σ²(Fo²)+(0.0737P)²+196.4647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3432
_reflns_number_total             3878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           TbEW
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247021
_shelx_shelxl_version_number     2018/3
_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   0.552
_shelx_estimated_absorpt_t_min   0.032
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H2-N3
 2.18 with sigma of 0.02
 H1A-H1B
 1.31 with sigma of 0.02
 O1-H1A = O1-H1B
 0.82 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
3.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_date_sample_data_collection 2018-04-09
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMount using parabar oil'
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 0.14937(3) 0.34063(2) 0.03029(2) 0.01883(14) Uani 1 1 d . . . . .
Tb1 Tb 0.500000 0.44716(4) 0.250000 0.01126(17) Uani 1 2 d S T P . .
O1 O 0.4142(7) 0.3463(4) 0.3037(4) 0.0180(15) Uani 1 1 d D . . . .
H1A H 0.445(9) 0.310(5) 0.326(6) 0.027 Uiso 1 1 d DR . . . .
H1B H 0.340(3) 0.345(6) 0.307(7) 0.027 Uiso 1 1 d DR . . . .
N1 N 0.3291(8) 0.4020(5) 0.1587(4) 0.0196(18) Uani 1 1 d . . . . .
C1 C 0.2601(9) 0.3824(6) 0.1130(5) 0.021(2) Uani 1 1 d . . . . .
Au2 Au 0.000000 0.500000 0.500000 0.02882(19) Uani 1 2 d S T P . .
O2 O 0.1668(9) 0.3449(6) 0.3020(6) 0.048(3) Uani 1 1 d . . . . .
H2 H 0.157893 0.386868 0.319211 0.073 Uiso 1 1 calc DGR . . . .
N2 N 0.0032(10) 0.2636(6) -0.1014(5) 0.030(2) Uani 1 1 d . . . . .
C2 C 0.0527(10) 0.2938(7) -0.0529(5) 0.023(2) Uani 1 1 d . . . . .
N3 N 0.0580(11) 0.4823(9) 0.3498(7) 0.050(3) Uani 1 1 d D . . . .
C3 C 0.0351(11) 0.4927(8) 0.4046(7) 0.034(3) Uani 1 1 d . . . . .
O10 O 0.3427(6) 0.4869(4) 0.3092(4) 0.0169(14) Uani 1 1 d . . . . .
N10 N 0.2985(7) 0.5544(5) 0.3000(4) 0.0162(17) Uani 1 1 d . . . . .
C10 C 0.2008(9) 0.5681(7) 0.2489(5) 0.021(2) Uani 1 1 d . . . . .
H10 H 0.165408 0.528965 0.219561 0.025 Uiso 1 1 calc R . . . .
O11 O 0.5719(6) 0.5542(4) 0.3165(3) 0.0177(15) Uani 1 1 d . . . . .
N11 N 0.5628(7) 0.5653(5) 0.3827(4) 0.0157(17) Uani 1 1 d . . . . .
C11 C 0.1532(10) 0.6384(7) 0.2395(6) 0.025(2) Uani 1 1 d . . . . .
H11 H 0.086979 0.647986 0.202385 0.030 Uiso 1 1 calc R . . . .
C12 C 0.2002(11) 0.6958(7) 0.2832(6) 0.028(2) Uani 1 1 d . . . . .
H12 H 0.165899 0.744386 0.277731 0.034 Uiso 1 1 calc R . . . .
C13 C 0.2990(11) 0.6796(7) 0.3353(6) 0.026(2) Uani 1 1 d . . . . .
H13 H 0.332542 0.717768 0.366405 0.031 Uiso 1 1 calc R . . . .
C14 C 0.3494(9) 0.6100(6) 0.3430(5) 0.0161(19) Uani 1 1 d . . . . .
C15 C 0.4534(9) 0.5917(6) 0.3995(5) 0.017(2) Uani 1 1 d . . . . .
C16 C 0.4465(10) 0.6078(6) 0.4676(5) 0.021(2) Uani 1 1 d . . . . .
H16 H 0.372008 0.628053 0.479161 0.025 Uiso 1 1 calc R . . . .
C17 C 0.5478(11) 0.5946(7) 0.5193(6) 0.028(2) Uani 1 1 d . . . . .
H17 H 0.542707 0.604614 0.566355 0.034 Uiso 1 1 calc R . . . .
C18 C 0.6573(11) 0.5663(7) 0.5012(6) 0.030(3) Uani 1 1 d . . . . .
H18 H 0.726879 0.555483 0.535937 0.036 Uiso 1 1 calc R . . . .
C19 C 0.6635(10) 0.5543(6) 0.4321(6) 0.022(2) Uani 1 1 d . . . . .
H19 H 0.739483 0.538091 0.419257 0.027 Uiso 1 1 calc R . . . .
C21 C 0.0998(14) 0.2920(12) 0.3333(10) 0.062(5) Uani 1 1 d . . . . .
H21A H 0.091362 0.246574 0.304427 0.075 Uiso 1 1 calc R . . . .
H21B H 0.014968 0.311484 0.333810 0.075 Uiso 1 1 calc R . . . .
C22 C 0.1543(17) 0.2720(13) 0.4027(11) 0.073(6) Uani 1 1 d . . . . .
H22A H 0.237309 0.250882 0.402784 0.110 Uiso 1 1 calc GR . . . .
H22B H 0.101462 0.235182 0.420571 0.110 Uiso 1 1 calc GR . . . .
H22C H 0.161407 0.316248 0.432206 0.110 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'
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'
Tb Tb -0.1723 4.1537 '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
C1 Au1 Au2 91.8(3) . 2 ?
C2 Au1 C1 174.8(4) . . ?
C2 Au1 Au2 92.6(3) . 2 ?
O1 Tb1 O1 79.8(4) . 2_655 ?
O1 Tb1 N1 74.5(3) . 2_655 ?
O1 Tb1 N1 76.4(3) 2_655 2_655 ?
O1 Tb1 N1 76.4(3) . . ?
O1 Tb1 N1 74.5(3) 2_655 . ?
O1 Tb1 O11 119.7(2) . . ?
O1 Tb1 O11 138.2(2) . 2_655 ?
O1 Tb1 O11 138.2(2) 2_655 . ?
O1 Tb1 O11 119.7(2) 2_655 2_655 ?
N1 Tb1 N1 141.9(4) . 2_655 ?
O10 Tb1 O1 146.3(3) 2_655 . ?
O10 Tb1 O1 68.8(3) 2_655 2_655 ?
O10 Tb1 O1 68.8(3) . . ?
O10 Tb1 O1 146.3(3) . 2_655 ?
O10 Tb1 N1 105.4(3) . 2_655 ?
O10 Tb1 N1 86.3(3) . . ?
O10 Tb1 N1 86.3(3) 2_655 2_655 ?
O10 Tb1 N1 105.4(3) 2_655 . ?
O10 Tb1 O10 144.3(4) 2_655 . ?
O10 Tb1 O11 71.4(2) . . ?
O10 Tb1 O11 79.8(2) . 2_655 ?
O10 Tb1 O11 79.8(2) 2_655 . ?
O10 Tb1 O11 71.4(2) 2_655 2_655 ?
O11 Tb1 N1 74.6(3) . 2_655 ?
O11 Tb1 N1 142.5(3) 2_655 2_655 ?
O11 Tb1 N1 74.6(3) 2_655 . ?
O11 Tb1 N1 142.5(3) . . ?
O11 Tb1 O11 72.1(4) . 2_655 ?
Tb1 O1 H1A 133(7) . . ?
Tb1 O1 H1B 121(7) . . ?
H1A O1 H1B 105(3) . . ?
C1 N1 Tb1 173.1(8) . . ?
N1 C1 Au1 174.7(10) . . ?
Au1 Au2 Au1 180.000(13) 2 6_566 ?
C3 Au2 Au1 86.5(4) 5_566 6_566 ?
C3 Au2 Au1 93.5(4) . 6_566 ?
C3 Au2 Au1 93.5(4) 5_566 2 ?
C3 Au2 Au1 86.5(4) . 2 ?
C3 Au2 C3 180.00(15) . 5_566 ?
C21 O2 H2 109.5 . . ?
N2 C2 Au1 175.5(10) . . ?
N3 C3 Au2 174.3(13) . . ?
N10 O10 Tb1 120.0(5) . . ?
O10 N10 C10 119.8(9) . . ?
O10 N10 C14 119.7(8) . . ?
C10 N10 C14 120.5(9) . . ?
N10 C10 H10 120.0 . . ?
N10 C10 C11 120.1(10) . . ?
C11 C10 H10 120.0 . . ?
N11 O11 Tb1 125.7(6) . . ?
O11 N11 C15 119.6(8) . . ?
O11 N11 C19 119.5(8) . . ?
C19 N11 C15 120.8(8) . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.0(10) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 121.3 . . ?
C13 C12 C11 117.3(11) . . ?
C13 C12 H12 121.3 . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.5(11) . . ?
C14 C13 H13 119.2 . . ?
N10 C14 C15 118.5(9) . . ?
C13 C14 N10 119.4(9) . . ?
C13 C14 C15 122.0(10) . . ?
N11 C15 C14 118.9(8) . . ?
N11 C15 C16 119.7(9) . . ?
C16 C15 C14 121.1(9) . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.3(10) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.5 . . ?
C16 C17 C18 119.1(10) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.3(10) . . ?
C19 C18 H18 120.4 . . ?
N11 C19 C18 120.8(10) . . ?
N11 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
O2 C21 H21A 108.5 . . ?
O2 C21 H21B 108.5 . . ?
O2 C21 C22 114.9(15) . . ?
H21A C21 H21B 107.5 . . ?
C22 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
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 C1 1.997(11) . ?
Au1 Au2 3.3042(5) 2 ?
Au1 C2 1.975(10) . ?
Tb1 O1 2.367(7) 2_655 ?
Tb1 O1 2.367(7) . ?
Tb1 N1 2.492(8) . ?
Tb1 N1 2.492(8) 2_655 ?
Tb1 O10 2.335(7) 2_655 ?
Tb1 O10 2.335(7) . ?
Tb1 O11 2.385(7) 2_655 ?
Tb1 O11 2.385(7) . ?
O1 H1A 0.82(2) . ?
O1 H1B 0.82(2) . ?
N1 C1 1.125(14) . ?
Au2 C3 1.974(13) 5_566 ?
Au2 C3 1.974(13) . ?
O2 H2 0.8400 . ?
O2 C21 1.402(18) . ?
N2 C2 1.147(14) . ?
N3 C3 1.158(18) . ?
O10 N10 1.308(11) . ?
N10 C10 1.356(13) . ?
N10 C14 1.366(13) . ?
C10 H10 0.9500 . ?
C10 C11 1.369(16) . ?
O11 N11 1.331(10) . ?
N11 C15 1.372(13) . ?
N11 C19 1.350(13) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(18) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(17) . ?
C13 H13 0.9500 . ?
C13 C14 1.367(16) . ?
C14 C15 1.482(13) . ?
C15 C16 1.380(14) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(16) . ?
C17 H17 0.9500 . ?
C17 C18 1.396(17) . ?
C18 H18 0.9500 . ?
C18 C19 1.383(16) . ?
C19 H19 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.44(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O10 N10 C10 89.3(9) . . . . ?
Tb1 O10 N10 C14 -92.2(9) . . . . ?
Tb1 O11 N11 C15 -82.1(10) . . . . ?
Tb1 O11 N11 C19 101.3(9) . . . . ?
O10 N10 C10 C11 179.3(9) . . . . ?
O10 N10 C14 C13 -176.9(9) . . . . ?
O10 N10 C14 C15 -0.4(13) . . . . ?
N10 C10 C11 C12 -2.5(16) . . . . ?
N10 C14 C15 N11 62.6(13) . . . . ?
N10 C14 C15 C16 -124.2(11) . . . . ?
C10 N10 C14 C13 1.6(14) . . . . ?
C10 N10 C14 C15 178.1(9) . . . . ?
C10 C11 C12 C13 1.8(16) . . . . ?
O11 N11 C15 C14 -2.5(14) . . . . ?
O11 N11 C15 C16 -175.8(9) . . . . ?
O11 N11 C19 C18 179.2(10) . . . . ?
N11 C15 C16 C17 -2.7(16) . . . . ?
C11 C12 C13 C14 0.6(17) . . . . ?
C12 C13 C14 N10 -2.3(16) . . . . ?
C12 C13 C14 C15 -178.7(10) . . . . ?
C13 C14 C15 N11 -121.1(11) . . . . ?
C13 C14 C15 C16 52.2(15) . . . . ?
C14 N10 C10 C11 0.8(14) . . . . ?
C14 C15 C16 C17 -175.9(10) . . . . ?
C15 N11 C19 C18 2.7(16) . . . . ?
C15 C16 C17 C18 1.4(17) . . . . ?
C16 C17 C18 C19 1.9(18) . . . . ?
C17 C18 C19 N11 -4.0(18) . . . . ?
C19 N11 C15 C14 174.0(10) . . . . ?
C19 N11 C15 C16 0.7(15) . . . . ?
