# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_er-dbsq
_database_code_depnum_ccdc_archive 'CCDC 2287861'
loop_
_audit_author_name
_audit_author_address
'Dunstan M.A.'
;Technical University of Denmark
Denmark
;
_audit_update_record             
;
2023-08-10 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_audit_creation_date             2022-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
majad@student.unimelb.edu.au
''
''
''
''
''
richardm@ansto.gov.au
c.boskovic@unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        
erbium(III)bis(tris-pyrazolylborato)(3,5-di-tert-butylsemiquinonato)
_chemical_formula_moiety         'C32 H40 B2 Er N12 O2'
_chemical_formula_sum            'C32 H40 B2 Er N12 O2'
_chemical_formula_weight         813.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Er C32 H40 O2 N12 B2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.59650(10)
_cell_length_b                   14.87660(10)
_cell_length_c                   19.51760(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.3210(10)
_cell_angle_gamma                90
_cell_volume                     3618.96(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32510
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.8430
_cell_measurement_theta_min      3.5550
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1640
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 -13 0.0225
-2 9 -1 0.0570
2 -8 -6 0.0423
0 -8 6 0.0501
-8 0 -2 0.0339
-1 8 -7 0.0413
-2 8 7 0.0579
-2 -1 13 0.0237
2 1 -13 0.0146
8 0 1 0.0419

_exptl_crystal_preparation       
'Reactino of KTp, dbsq-, and Er(III) nitrate hexahydrate in methanol.'
_exptl_crystal_recrystallization_method 'Crystallisation from n-hexane at -18C.'
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.038
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.2103 -0.8958 -12.5145 -0.0571 -0.2448 -0.9679
-2.1437 9.2090 -1.3424 0.2266 0.9458 -0.2326
2.1979 -8.4402 -5.5698 -0.3157 -0.8954 -0.3140
0.4371 -8.3179 6.2247 -0.2655 -0.7488 0.6073
-7.7772 0.3165 -2.0987 -0.8472 0.5184 -0.1164
-0.8490 7.7509 -7.1643 0.1740 0.7231 -0.6684
-2.3263 7.6273 7.3382 0.2943 0.8354 0.4641
-1.5256 -1.4245 12.5217 0.0088 -0.0033 1.0000
1.5256 1.4245 -12.5217 -0.0088 0.0033 -1.0000
7.9972 -0.1659 0.8033 0.8530 -0.5218 0.0125

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54321
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.074
_diffrn_reflns_theta_min         3.546
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  25.00   0.50    0.41    --  -48.30  19.00-120.00  110
  2  ω    -69.00  19.00   0.50    0.41    --  -48.30  77.00 -60.00  176
  3  ω      2.00  61.00   0.50    0.41    --   48.30 -57.00 150.00  118
  4  ω     43.00  91.00   0.50    0.41    --   48.30-125.00  30.00   96
  5  ω     44.00  71.00   0.50    1.64    --  107.75 -61.00  90.00   54
  6  ω     52.00  78.00   0.50    1.64    --  107.75 -94.00  90.00   52
  7  ω     81.00 106.00   0.50    1.64    --  107.75 -94.00  90.00   50
  8  ω     83.00 110.00   0.50    1.64    --  107.75-125.00  60.00   54
  9  ω     74.00 106.00   0.50    1.64    --  107.75 -94.00  60.00   64
 10  ω     78.00 106.00   0.50    1.64    --  107.75 -94.00   0.00   56
 11  ω     81.00 107.00   0.50    1.64    --  107.75-125.00 -60.00   52
 12  ω     74.00 101.00   0.50    1.64    --  107.75 -77.00 -60.00   54
 13  ω     72.00 106.00   0.50    1.64    --  107.75 -94.00 -60.00   68
 14  ω     55.00 107.00   0.50    1.64    --  107.75-108.00 -49.52  104
 15  ω     64.00 106.00   0.50    1.64    --  107.75 -97.00  39.47   84
 16  ω     59.00  95.00   0.50    1.64    --  107.75 -77.00 -30.00   72
 17  ω     38.00  64.00   0.50    1.64    --  107.75 -77.00  30.00   52
 18  ω     36.00  63.00   0.50    1.64    --  107.75 -94.00  60.00   54
 19  ω     42.00 105.00   0.50    1.64    --  107.75 -94.00 120.00  126
 20  ω     67.00 106.00   0.50    1.64    --  107.75 -98.00 170.00   78
 21  ω     37.00  65.00   0.50    1.64    --  107.75-125.00  60.00   56
 22  ω     43.00  69.00   0.50    1.64    --  107.75 -94.00   0.00   52
 23  ω     42.00  69.00   0.50    1.64    --  107.75 -61.00 -60.00   54
 24  ω     40.00  67.00   0.50    1.64    --  107.75 -94.00 -60.00   54
 25  ω     37.00  70.00   0.50    1.64    --  107.75 -77.00 -60.00   66
 26  ω     56.00  88.00   0.50    1.64    --  107.75 -77.00-120.00   64
 27  ω     81.00 106.00   0.50    1.64    --  107.75 -94.00-150.00   50
 28  ω     78.00 105.00   0.50    1.64    --  107.75 -94.00-180.00   54
 29  ω     55.00  91.00   0.50    1.64    --  107.75 -77.00-150.00   72
 30  ω     41.00  69.00   0.50    1.64    --  107.75 -61.00-150.00   56
 31  ω     53.00  91.00   0.50    1.64    --  107.75 -77.00-180.00   76
 32  ω     39.00  74.00   0.50    1.64    --  107.75 -94.00-180.00   70
 33  ω     39.00  64.00   0.50    1.64    --  107.75 -94.00-150.00   50
 34  ω     98.00 155.00   0.50    1.64    --  107.75  15.00   0.00  114
 35  ω     98.00 153.00   0.50    1.64    --  107.75  30.00 -60.00  110
 36  ω    103.00 174.00   0.50    1.64    --  107.75  30.00-150.00  142
 37  ω    104.00 174.00   0.50    1.64    --  107.75  30.00 -90.00  140
 38  ω     97.00 163.00   0.50    1.64    --  107.75  15.00-180.00  132
 39  ω     99.00 166.00   0.50    1.64    --  107.75  30.00-120.00  134
 40  ω     97.00 164.00   0.50    1.64    --  107.75  15.00  30.00  134
 41  ω     97.00 155.00   0.50    1.64    --  107.75  15.00 150.00  116
 42  ω    100.00 150.00   0.50    1.64    --  107.75  30.00  90.00  100
 43  ω     36.00  61.00   0.50    1.64    --  107.75 -61.00  30.00   50
 44  ω     39.00  65.00   0.50    1.64    --  107.75 -61.00  60.00   52
 45  ω     36.00  69.00   0.50    1.64    --  107.75 -61.00 120.00   66
 46  ω     40.00  66.00   0.50    1.64    --  107.75 -77.00 150.00   52
 47  ω     37.00  62.00   0.50    1.64    --  107.75 -77.00  60.00   50
 48  ω     36.00  61.00   0.50    1.64    --  107.75 -61.00   0.00   50
 49  ω   -114.00 -40.00   0.50    0.41    --  -48.30 -77.00 120.00  148
 50  ω   -114.00  10.00   0.50    0.41    --  -48.30   0.00  90.00  248
 51  ω   -136.00-111.00   0.50    1.64    --  -86.25 -45.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1057828000
_diffrn_orient_matrix_UB_12      0.0520785000
_diffrn_orient_matrix_UB_13      0.0195141000
_diffrn_orient_matrix_UB_21      -0.0636144000
_diffrn_orient_matrix_UB_22      0.0881895000
_diffrn_orient_matrix_UB_23      0.0020162000
_diffrn_orient_matrix_UB_31      -0.0065223000
_diffrn_orient_matrix_UB_32      -0.0155073000
_diffrn_orient_matrix_UB_33      0.0772991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7387
_reflns_number_total             7666
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7666
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.069
_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)+(0.0326P)²+3.9293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0689
_refine_special_details          'Stucture was refined with no disorder.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Er1 Er 0.77328(2) 0.73849(2) 0.34275(2) 0.01925(5) Uani 1 1 d . . . . .
O1 O 0.59423(12) 0.76759(10) 0.33765(7) 0.0218(3) Uani 1 1 d . . . . .
O2 O 0.67896(12) 0.67076(11) 0.24640(7) 0.0245(3) Uani 1 1 d . . . . .
N1 N 0.70773(15) 0.59482(13) 0.38883(10) 0.0287(4) Uani 1 1 d . . . . .
N2 N 0.72604(15) 0.57537(14) 0.45818(10) 0.0299(4) Uani 1 1 d . . . . .
N3 N 0.92396(14) 0.66150(13) 0.41535(10) 0.0258(4) Uani 1 1 d . . . . .
N4 N 0.91674(15) 0.62935(13) 0.47985(10) 0.0265(4) Uani 1 1 d . . . . .
N5 N 0.74474(15) 0.77749(13) 0.46021(9) 0.0241(4) Uani 1 1 d . . . . .
N6 N 0.76961(15) 0.72383(14) 0.51702(10) 0.0278(4) Uani 1 1 d . . . . .
N7 N 0.73911(14) 0.86969(12) 0.26080(9) 0.0225(3) Uani 1 1 d . . . . .
N8 N 0.81980(14) 0.91539(12) 0.23594(8) 0.0217(3) Uani 1 1 d . . . . .
N9 N 0.90241(15) 0.72081(13) 0.26177(9) 0.0239(4) Uani 1 1 d . . . . .
N10 N 0.95281(14) 0.78969(12) 0.23346(9) 0.0218(3) Uani 1 1 d . . . . .
N11 N 0.91298(14) 0.85536(12) 0.37965(9) 0.0218(3) Uani 1 1 d . . . . .
N12 N 0.96996(14) 0.89697(12) 0.33408(9) 0.0214(3) Uani 1 1 d . . . . .
C1 C 0.6348(2) 0.53411(17) 0.36124(14) 0.0367(5) Uani 1 1 d . . . . .
H1 H 0.606962 0.530541 0.313405 0.044 Uiso 1 1 calc R . . . .
C2 C 0.6053(2) 0.47738(19) 0.41163(17) 0.0458(7) Uani 1 1 d . . . . .
H2 H 0.555039 0.429445 0.405525 0.055 Uiso 1 1 calc R . . . .
C3 C 0.6648(2) 0.50567(18) 0.47222(15) 0.0396(6) Uani 1 1 d . . . . .
H3 H 0.663011 0.480246 0.516686 0.048 Uiso 1 1 calc R . . . .
C4 C 1.02882(18) 0.65883(16) 0.40925(13) 0.0303(5) Uani 1 1 d . . . . .
H4 H 1.058056 0.677379 0.369317 0.036 Uiso 1 1 calc R . . . .
C5 C 1.08888(18) 0.62524(17) 0.46928(13) 0.0332(5) Uani 1 1 d . . . . .
H5 H 1.164335 0.616601 0.478257 0.040 Uiso 1 1 calc R . . . .
C6 C 1.01483(19) 0.60737(16) 0.51263(12) 0.0312(5) Uani 1 1 d . . . . .
H6 H 1.030204 0.583491 0.558134 0.037 Uiso 1 1 calc R . . . .
C7 C 0.71084(17) 0.85544(16) 0.48377(11) 0.0276(4) Uani 1 1 d . . . . .
H7 H 0.687783 0.905705 0.455459 0.033 Uiso 1 1 calc R . . . .
C8 C 0.71399(19) 0.85282(19) 0.55533(12) 0.0332(5) Uani 1 1 d . . . . .
H8 H 0.694896 0.899292 0.584626 0.040 Uiso 1 1 calc R . . . .
C9 C 0.7508(2) 0.76829(18) 0.57417(12) 0.0332(5) Uani 1 1 d . . . . .
H9 H 0.761202 0.744962 0.619960 0.040 Uiso 1 1 calc R . . . .
C10 C 0.64792(18) 0.91118(15) 0.23328(11) 0.0263(4) Uani 1 1 d . . . . .
H10 H 0.578188 0.893870 0.241331 0.032 Uiso 1 1 calc R . . . .
C11 C 0.66922(19) 0.98274(16) 0.19148(11) 0.0287(5) Uani 1 1 d . . . . .
H11 H 0.618968 1.022496 0.166268 0.034 Uiso 1 1 calc R . . . .
C12 C 0.77903(18) 0.98333(15) 0.19468(11) 0.0257(4) Uani 1 1 d . . . . .
H12 H 0.819284 1.024649 0.171675 0.031 Uiso 1 1 calc R . . . .
C13 C 0.92895(18) 0.64591(16) 0.23028(12) 0.0281(4) Uani 1 1 d . . . . .
H13 H 0.905259 0.587244 0.239924 0.034 Uiso 1 1 calc R . . . .
C14 C 0.99592(18) 0.66556(16) 0.18150(12) 0.0294(5) Uani 1 1 d . . . . .
H14 H 1.025904 0.624687 0.152171 0.035 Uiso 1 1 calc R . . . .
C15 C 1.00904(18) 0.75725(15) 0.18516(12) 0.0257(4) Uani 1 1 d . . . . .
H15 H 1.050815 0.791983 0.158138 0.031 Uiso 1 1 calc R . . . .
C16 C 0.96308(17) 0.87687(15) 0.44295(11) 0.0246(4) Uani 1 1 d . . . . .
H16 H 0.941421 0.856922 0.485049 0.029 Uiso 1 1 calc R . . . .
C17 C 1.05073(17) 0.93212(15) 0.43877(11) 0.0264(4) Uani 1 1 d . . . . .
H17 H 1.098838 0.956935 0.475943 0.032 Uiso 1 1 calc R . . . .
C18 C 1.05261(17) 0.94301(14) 0.36915(11) 0.0246(4) Uani 1 1 d . . . . .
H18 H 1.103705 0.977326 0.349017 0.029 Uiso 1 1 calc R . . . .
C19 C 0.52933(17) 0.73296(14) 0.28801(11) 0.0207(4) Uani 1 1 d . . . . .
C20 C 0.57686(16) 0.68229(14) 0.23589(10) 0.0212(4) Uani 1 1 d . . . . .
C21 C 0.41441(17) 0.74106(14) 0.28181(11) 0.0213(4) Uani 1 1 d . . . . .
C22 C 0.50968(17) 0.64911(14) 0.17655(10) 0.0222(4) Uani 1 1 d . . . . .
H22 H 0.540391 0.617683 0.141859 0.027 Uiso 1 1 calc R . . . .
C23 C 0.35541(16) 0.70646(15) 0.22318(10) 0.0226(4) Uani 1 1 d . . . . .
H23 H 0.279564 0.712208 0.218073 0.027 Uiso 1 1 calc R . . . .
C24 C 0.40121(16) 0.66206(14) 0.16898(10) 0.0211(4) Uani 1 1 d . . . . .
C25 C 0.36341(17) 0.78450(16) 0.34034(11) 0.0256(4) Uani 1 1 d . . . . .
C26 C 0.3999(2) 0.73257(17) 0.40795(12) 0.0335(5) Uani 1 1 d . . . . .
H26A H 0.379428 0.669226 0.401590 0.050 Uiso 1 1 calc GR . . . .
H26B H 0.365374 0.758291 0.445376 0.050 Uiso 1 1 calc GR . . . .
H26C H 0.477954 0.737162 0.419904 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.39723(19) 0.88346(16) 0.34877(12) 0.0301(5) Uani 1 1 d . . . . .
H27A H 0.475467 0.887210 0.360157 0.045 Uiso 1 1 calc GR . . . .
H27B H 0.363855 0.910646 0.386117 0.045 Uiso 1 1 calc GR . . . .
H27C H 0.373954 0.915706 0.305411 0.045 Uiso 1 1 calc GR . . . .
C28 C 0.2410(2) 0.7806(2) 0.32547(14) 0.0401(6) Uani 1 1 d . . . . .
H28A H 0.215904 0.814394 0.283121 0.060 Uiso 1 1 calc GR . . . .
H28B H 0.210623 0.806989 0.364358 0.060 Uiso 1 1 calc GR . . . .
H28C H 0.217830 0.717819 0.319398 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.32500(17) 0.63002(15) 0.10545(10) 0.0226(4) Uani 1 1 d . . . . .
C30 C 0.38622(18) 0.58888(15) 0.05072(10) 0.0253(4) Uani 1 1 d . . . . .
H30A H 0.434975 0.633866 0.035885 0.038 Uiso 1 1 calc GR . . . .
H30B H 0.335117 0.569496 0.010769 0.038 Uiso 1 1 calc GR . . . .
H30C H 0.427717 0.536973 0.070523 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.24895(17) 0.55899(16) 0.12815(11) 0.0260(4) Uani 1 1 d . . . . .
H31A H 0.290297 0.505891 0.145659 0.039 Uiso 1 1 calc GR . . . .
H31B H 0.195923 0.541895 0.088493 0.039 Uiso 1 1 calc GR . . . .
H31C H 0.212054 0.583799 0.164812 0.039 Uiso 1 1 calc GR . . . .
C32 C 0.25920(19) 0.71071(16) 0.07313(11) 0.0280(4) Uani 1 1 d . . . . .
H32A H 0.214602 0.734195 0.106237 0.042 Uiso 1 1 calc GR . . . .
H32B H 0.213151 0.691358 0.030894 0.042 Uiso 1 1 calc GR . . . .
H32C H 0.308009 0.757903 0.061684 0.042 Uiso 1 1 calc GR . . . .
B1 B 0.8092(2) 0.62693(19) 0.50920(13) 0.0292(5) Uani 1 1 d . . . . .
H1A H 0.820539 0.592532 0.560789 0.035 Uiso 1 1 calc R . . . .
B2 B 0.93807(19) 0.88802(16) 0.25526(12) 0.0227(4) Uani 1 1 d . . . . .
H2A H 0.989839 0.933054 0.228125 0.027 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Er1 O1 2.2846(14) . ?
Er1 O2 2.3058(14) . ?
Er1 N1 2.505(2) . ?
Er1 N3 2.4787(18) . ?
Er1 N5 2.4415(18) . ?
Er1 N7 2.5206(18) . ?
Er1 N9 2.4406(18) . ?
Er1 N11 2.5042(18) . ?
O1 C19 1.282(3) . ?
O2 C20 1.284(2) . ?
N1 N2 1.371(3) . ?
N1 C1 1.344(3) . ?
N2 C3 1.344(3) . ?
N2 B1 1.541(3) . ?
N3 N4 1.362(3) . ?
N3 C4 1.344(3) . ?
N4 C6 1.347(3) . ?
N4 B1 1.545(3) . ?
N5 N6 1.365(3) . ?
N5 C7 1.340(3) . ?
N6 C9 1.347(3) . ?
N6 B1 1.540(3) . ?
N7 N8 1.369(2) . ?
N7 C10 1.345(3) . ?
N8 C12 1.347(3) . ?
N8 B2 1.538(3) . ?
N9 N10 1.364(3) . ?
N9 C13 1.338(3) . ?
N10 C15 1.348(3) . ?
N10 B2 1.542(3) . ?
N11 N12 1.369(2) . ?
N11 C16 1.342(3) . ?
N12 C18 1.347(3) . ?
N12 B2 1.538(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.387(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(4) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.373(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.392(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.391(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.376(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C13 C14 1.391(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.375(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.388(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.372(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.462(3) . ?
C19 C21 1.440(3) . ?
C20 C22 1.420(3) . ?
C21 C23 1.371(3) . ?
C21 C25 1.532(3) . ?
C22 H22 0.9500 . ?
C22 C24 1.367(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.437(3) . ?
C24 C29 1.530(3) . ?
C25 C26 1.541(3) . ?
C25 C27 1.535(3) . ?
C25 C28 1.529(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.533(3) . ?
C29 C31 1.534(3) . ?
C29 C32 1.541(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
B1 H1A 1.1200 . ?
B2 H2A 1.1200 . ?

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
O1 Er1 O2 70.02(5) . . ?
O1 Er1 N1 78.61(6) . . ?
O1 Er1 N3 141.43(6) . . ?
O1 Er1 N5 73.57(6) . . ?
O1 Er1 N7 75.45(6) . . ?
O1 Er1 N9 137.60(6) . . ?
O1 Er1 N11 121.95(5) . . ?
O2 Er1 N1 76.25(6) . . ?
O2 Er1 N3 121.73(6) . . ?
O2 Er1 N5 137.83(6) . . ?
O2 Er1 N7 78.48(6) . . ?
O2 Er1 N9 74.80(6) . . ?
O2 Er1 N11 142.72(5) . . ?
N1 Er1 N7 148.61(6) . . ?
N3 Er1 N1 70.45(6) . . ?
N3 Er1 N7 140.08(6) . . ?
N3 Er1 N11 73.04(6) . . ?
N5 Er1 N1 76.38(6) . . ?
N5 Er1 N3 77.15(6) . . ?
N5 Er1 N7 112.15(6) . . ?
N5 Er1 N11 75.98(6) . . ?
N9 Er1 N1 115.20(6) . . ?
N9 Er1 N3 78.08(6) . . ?
N9 Er1 N5 146.75(6) . . ?
N9 Er1 N7 75.00(6) . . ?
N9 Er1 N11 75.80(6) . . ?
N11 Er1 N1 138.04(6) . . ?
N11 Er1 N7 72.14(6) . . ?
C19 O1 Er1 118.33(13) . . ?
C20 O2 Er1 117.25(12) . . ?
N2 N1 Er1 121.18(14) . . ?
C1 N1 Er1 132.16(16) . . ?
C1 N1 N2 105.2(2) . . ?
N1 N2 B1 122.30(18) . . ?
C3 N2 N1 110.2(2) . . ?
C3 N2 B1 127.5(2) . . ?
N4 N3 Er1 122.87(13) . . ?
C4 N3 Er1 130.10(16) . . ?
C4 N3 N4 105.63(18) . . ?
N3 N4 B1 122.01(17) . . ?
C6 N4 N3 110.19(19) . . ?
C6 N4 B1 127.7(2) . . ?
N6 N5 Er1 125.17(14) . . ?
C7 N5 Er1 128.71(14) . . ?
C7 N5 N6 105.93(18) . . ?
N5 N6 B1 120.42(18) . . ?
C9 N6 N5 109.8(2) . . ?
C9 N6 B1 129.8(2) . . ?
N8 N7 Er1 122.83(12) . . ?
C10 N7 Er1 131.76(15) . . ?
C10 N7 N8 105.40(17) . . ?
N7 N8 B2 121.63(17) . . ?
C12 N8 N7 110.26(17) . . ?
C12 N8 B2 128.12(19) . . ?
N10 N9 Er1 125.05(13) . . ?
C13 N9 Er1 128.42(15) . . ?
C13 N9 N10 106.12(18) . . ?
N9 N10 B2 121.28(17) . . ?
C15 N10 N9 109.69(18) . . ?
C15 N10 B2 128.98(18) . . ?
N12 N11 Er1 122.67(12) . . ?
C16 N11 Er1 130.35(14) . . ?
C16 N11 N12 105.62(17) . . ?
N11 N12 B2 121.66(17) . . ?
C18 N12 N11 109.82(17) . . ?
C18 N12 B2 128.52(18) . . ?
N1 C1 H1 124.4 . . ?
N1 C1 C2 111.2(2) . . ?
C2 C1 H1 124.4 . . ?
C1 C2 H2 127.6 . . ?
C3 C2 C1 104.8(2) . . ?
C3 C2 H2 127.6 . . ?
N2 C3 C2 108.6(2) . . ?
N2 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
N3 C4 H4 124.5 . . ?
N3 C4 C5 110.9(2) . . ?
C5 C4 H4 124.5 . . ?
C4 C5 H5 127.7 . . ?
C6 C5 C4 104.7(2) . . ?
C6 C5 H5 127.7 . . ?
N4 C6 C5 108.6(2) . . ?
N4 C6 H6 125.7 . . ?
C5 C6 H6 125.7 . . ?
N5 C7 H7 124.6 . . ?
N5 C7 C8 110.9(2) . . ?
C8 C7 H7 124.6 . . ?
C7 C8 H8 127.6 . . ?
C9 C8 C7 104.7(2) . . ?
C9 C8 H8 127.6 . . ?
N6 C9 C8 108.7(2) . . ?
N6 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N7 C10 H10 124.5 . . ?
N7 C10 C11 111.1(2) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.6 . . ?
C12 C11 C10 104.85(19) . . ?
C12 C11 H11 127.6 . . ?
N8 C12 C11 108.4(2) . . ?
N8 C12 H12 125.8 . . ?
C11 C12 H12 125.8 . . ?
N9 C13 H13 124.6 . . ?
N9 C13 C14 110.9(2) . . ?
C14 C13 H13 124.6 . . ?
C13 C14 H14 127.7 . . ?
C15 C14 C13 104.66(19) . . ?
C15 C14 H14 127.7 . . ?
N10 C15 C14 108.7(2) . . ?
N10 C15 H15 125.7 . . ?
C14 C15 H15 125.7 . . ?
N11 C16 H16 124.5 . . ?
N11 C16 C17 111.04(19) . . ?
C17 C16 H16 124.5 . . ?
C16 C17 H17 127.6 . . ?
C18 C17 C16 104.83(18) . . ?
C18 C17 H17 127.6 . . ?
N12 C18 C17 108.69(19) . . ?
N12 C18 H18 125.7 . . ?
C17 C18 H18 125.7 . . ?
O1 C19 C20 116.90(18) . . ?
O1 C19 C21 123.59(19) . . ?
C21 C19 C20 119.51(18) . . ?
O2 C20 C19 117.33(18) . . ?
O2 C20 C22 123.27(18) . . ?
C22 C20 C19 119.39(18) . . ?
C19 C21 C25 119.83(18) . . ?
C23 C21 C19 117.09(19) . . ?
C23 C21 C25 123.06(19) . . ?
C20 C22 H22 119.7 . . ?
C24 C22 C20 120.51(18) . . ?
C24 C22 H22 119.7 . . ?
C21 C23 H23 118.0 . . ?
C21 C23 C24 124.06(19) . . ?
C24 C23 H23 118.0 . . ?
C22 C24 C23 119.13(18) . . ?
C22 C24 C29 122.95(18) . . ?
C23 C24 C29 117.91(18) . . ?
C21 C25 C26 108.79(18) . . ?
C21 C25 C27 110.16(18) . . ?
C27 C25 C26 110.21(19) . . ?
C28 C25 C21 111.26(18) . . ?
C28 C25 C26 108.1(2) . . ?
C28 C25 C27 108.3(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 C30 111.67(17) . . ?
C24 C29 C31 108.98(16) . . ?
C24 C29 C32 109.05(18) . . ?
C30 C29 C31 108.93(18) . . ?
C30 C29 C32 108.71(17) . . ?
C31 C29 C32 109.48(18) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 B1 N4 108.80(19) . . ?
N2 B1 H1A 109.8 . . ?
N4 B1 H1A 109.8 . . ?
N6 B1 N2 109.27(19) . . ?
N6 B1 N4 109.19(19) . . ?
N6 B1 H1A 109.8 . . ?
N8 B2 N10 109.55(17) . . ?
N8 B2 N12 109.01(17) . . ?
N8 B2 H2A 109.6 . . ?
N10 B2 H2A 109.6 . . ?
N12 B2 N10 109.48(17) . . ?
N12 B2 H2A 109.6 . . ?

_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 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.763
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_y-trop
_database_code_depnum_ccdc_archive 'CCDC 2287862'
loop_
_audit_author_name
_audit_author_address
'Dunstan M.A.'
;Technical University of Denmark
Denmark
;
_audit_update_record             
;
2023-08-10 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_audit_creation_date             2022-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
majad@student.unimelb.edu.au
''
''
''
''
''
richardm@ansto.gov.au
c.boskovic@unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        
yttrium(III)bis(tris-pyrazolylborato)(tropolonato)
_chemical_formula_moiety         'C25 H25 B2 N12 O2 Y'
_chemical_formula_sum            'C25 H25 B2 N12 O2 Y'
_chemical_formula_weight         636.10
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25 H25 O2 N12 Y B2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   9.33650(10)
_cell_length_b                   9.33650(10)
_cell_length_c                   31.9312(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2783.45(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.7470
_cell_measurement_theta_min      4.9150
_shelx_estimated_absorpt_T_max   0.850
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    3.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -2 0.0536
0 -1 2 0.0184
-2 1 2 0.0412
-2 -1 1 0.0339
1 0 -2 0.0128
0 -1 0 0.0265
1 1 -2 0.0235
-1 -1 2 0.0313
0 0 1 0.0483
1 0 -1 0.0073
1 0 1 0.0101
0 0 -1 0.0520
1 -1 1 0.0135
-1 1 -1 0.0599
0 1 2 0.0656
0 -1 -2 0.0399

_exptl_crystal_preparation       
'Reaction of KTp, Y(III) nitrate hexahydrate and tropolonate in methanol.'
_exptl_crystal_recrystallization_method 
'Hot recrystallisation in methanol/ethyl acetate.'
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0004 0.9995 -1.9995 0.0922 0.0483 -0.1603
0.0004 -0.9995 1.9995 -0.0922 -0.0483 0.1603
-2.0016 0.9997 1.9989 0.0457 -0.3309 -0.1847
-2.0009 -1.0001 0.9980 0.0828 -0.3324 0.1465
1.0006 -0.0001 -1.9992 0.0232 0.1896 0.0122
0.0004 -0.9998 -0.0004 -0.0036 -0.0103 0.1645
1.0002 0.9997 -1.9987 0.0268 0.1999 -0.1523
-1.0002 -0.9997 1.9987 -0.0268 -0.1999 0.1523
0.0000 0.0001 1.0000 -0.0443 -0.0190 -0.0021
1.0006 0.0001 -0.9992 -0.0211 0.1706 0.0101
1.0007 0.0004 1.0007 -0.1096 0.1325 0.0058
-0.0000 -0.0001 -1.0000 0.0443 0.0190 0.0021
1.0010 -0.9995 1.0003 -0.1132 0.1222 0.1704
-1.0010 0.9995 -1.0003 0.1132 -0.1222 -0.1704
-0.0003 1.0001 2.0004 -0.0849 -0.0278 -0.1688
0.0003 -1.0001 -2.0004 0.0849 0.0278 0.1688

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9108
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.388
_diffrn_reflns_theta_min         4.935
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     97.00 154.00   0.50    1.89    --  105.86 128.00 -29.00  114
  2  ω     78.00 106.00   0.50    1.89    --  105.86 -94.00-180.00   56
  3  ω     34.00  69.00   0.50    1.89    --  105.86 -94.00-180.00   70
  4  ω     33.00  66.00   0.50    1.89    --  105.86 -61.00-150.00   66
  5  ω     37.00  99.00   0.50    1.89    --  105.86-129.00 166.00  124
  6  ω     36.00 105.00   0.50    1.89    --  105.86 -94.00 150.00  138
  7  ω    -42.00 -15.00   0.50    1.89    --  -86.25   5.00 158.00   54
  8  ω    -28.00  10.00   0.50    0.47    --  -47.45  19.00  90.00   76
  9  ω   -101.00 -74.00   0.50    1.89    --  -86.25-128.00-103.00   54
 10  ω   -114.00 -74.00   0.50    0.47    --  -47.45-125.00   0.00   80
 11  ω    -30.00  16.00   0.50    0.47    --  -47.45  19.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0652583000
_diffrn_orient_matrix_UB_12      0.0036075000
_diffrn_orient_matrix_UB_13      -0.0442780000
_diffrn_orient_matrix_UB_21      0.1514575000
_diffrn_orient_matrix_UB_22      0.0103372000
_diffrn_orient_matrix_UB_23      -0.0190293000
_diffrn_orient_matrix_UB_31      0.0079930000
_diffrn_orient_matrix_UB_32      -0.1645561000
_diffrn_orient_matrix_UB_33      -0.0020937000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                2669
_reflns_number_total             2827
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 
;
 Flack x determined using 987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2827
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.066
_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)+(0.0237P)²+1.8557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0747
_refine_special_details          'Stucture was refined with no disorder.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Y1 Y 0.39439(3) 0.39439(3) 0.500000 0.02125(13) Uani 1 2 d S T P . .
O1 O 0.1737(3) 0.3275(3) 0.47566(8) 0.0255(6) Uani 1 1 d . . . . .
N1 N 0.2288(3) 0.4715(4) 0.55727(11) 0.0278(7) Uani 1 1 d . . . . .
N2 N 0.2699(4) 0.5503(4) 0.59110(11) 0.0287(7) Uani 1 1 d . . . . .
N3 N 0.4504(4) 0.6504(4) 0.51940(10) 0.0277(7) Uani 1 1 d . . . . .
N4 N 0.4684(4) 0.6933(3) 0.56001(10) 0.0269(7) Uani 1 1 d . . . . .
N5 N 0.5301(4) 0.3685(3) 0.56525(10) 0.0263(7) Uani 1 1 d . . . . .
N6 N 0.5257(4) 0.4632(4) 0.59771(10) 0.0288(7) Uani 1 1 d . . . . .
C1 C 0.0856(4) 0.4587(4) 0.56063(13) 0.0288(8) Uani 1 1 d . . . . .
H1 H 0.026893 0.407251 0.541541 0.035 Uiso 1 1 calc R . . . .
C2 C 0.0352(4) 0.5307(5) 0.59577(14) 0.0310(9) Uani 1 1 d . . . . .
H2 H -0.061307 0.538747 0.604918 0.037 Uiso 1 1 calc R . . . .
C3 C 0.1544(4) 0.5876(5) 0.61434(13) 0.0313(9) Uani 1 1 d . . . . .
H3 H 0.155904 0.643518 0.639189 0.038 Uiso 1 1 calc R . . . .
C4 C 0.5018(4) 0.7585(4) 0.49614(15) 0.0314(8) Uani 1 1 d . . . . .
H4 H 0.504053 0.758413 0.466395 0.038 Uiso 1 1 calc R . . . .
C5 C 0.5512(5) 0.8704(4) 0.52080(15) 0.0342(9) Uani 1 1 d . . . . .
H5 H 0.592071 0.958412 0.511833 0.041 Uiso 1 1 calc R . . . .
C6 C 0.5275(5) 0.8252(5) 0.56106(15) 0.0311(9) Uani 1 1 d . . . . .
H6 H 0.549189 0.878026 0.585676 0.037 Uiso 1 1 calc R . . . .
C7 C 0.6269(4) 0.2684(4) 0.57574(14) 0.0320(9) Uani 1 1 d . . . . .
H7 H 0.651264 0.188024 0.558940 0.038 Uiso 1 1 calc R . . . .
C8 C 0.6867(5) 0.2989(5) 0.61473(14) 0.0371(9) Uani 1 1 d . . . . .
H8 H 0.758161 0.246170 0.629242 0.045 Uiso 1 1 calc R . . . .
C9 C 0.6192(4) 0.4226(4) 0.62754(13) 0.0337(9) Uani 1 1 d . . . . .
H9 H 0.635941 0.471292 0.653210 0.040 Uiso 1 1 calc R . . . .
C10 C 0.1187(4) 0.2071(4) 0.48596(12) 0.0260(8) Uani 1 1 d . . . . .
C11 C -0.0201(4) 0.1715(5) 0.47094(14) 0.0305(8) Uani 1 1 d . . . . .
H11 H -0.063091 0.242268 0.453659 0.037 Uiso 1 1 calc R . . . .
C12 C -0.1027(5) 0.0507(4) 0.47737(14) 0.0357(9) Uani 1 1 d . . . . .
H12 H -0.194008 0.052481 0.464272 0.043 Uiso 1 1 calc R . . . .
C13 C -0.0732(4) -0.0732(4) 0.500000 0.0381(13) Uani 1 2 d S T P . .
H13 H -0.145103 -0.145103 0.500000 0.046 Uiso 1 2 calc RS T P . .
B1 B 0.4258(4) 0.5965(5) 0.59717(13) 0.0299(9) Uani 1 1 d . . . . .
H1A H 0.436874 0.657111 0.627256 0.036 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Y1 O1 2.289(3) 7_556 ?
Y1 O1 2.289(3) . ?
Y1 N1 2.500(3) . ?
Y1 N1 2.500(3) 7_556 ?
Y1 N3 2.524(3) . ?
Y1 N3 2.524(3) 7_556 ?
Y1 N5 2.450(3) 7_556 ?
Y1 N5 2.450(3) . ?
O1 C10 1.279(5) . ?
N1 N2 1.361(5) . ?
N1 C1 1.347(5) . ?
N2 C3 1.354(5) . ?
N2 B1 1.530(5) . ?
N3 N4 1.367(4) . ?
N3 C4 1.342(5) . ?
N4 C6 1.350(5) . ?
N4 B1 1.544(6) . ?
N5 N6 1.363(5) . ?
N5 C7 1.343(5) . ?
N6 C9 1.347(5) . ?
N6 B1 1.555(6) . ?
C1 C2 1.390(6) . ?
C2 C3 1.368(6) . ?
C4 C5 1.387(6) . ?
C5 C6 1.371(7) . ?
C7 C8 1.394(6) . ?
C8 C9 1.378(6) . ?
C10 C10 1.472(8) 7_556 ?
C10 C11 1.421(6) . ?
C11 C12 1.382(6) . ?
C12 C13 1.391(5) . ?

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
O1 Y1 O1 67.93(14) 7_556 . ?
O1 Y1 N1 80.93(11) . 7_556 ?
O1 Y1 N1 76.73(10) . . ?
O1 Y1 N1 76.73(10) 7_556 7_556 ?
O1 Y1 N1 80.93(11) 7_556 . ?
O1 Y1 N3 145.65(10) 7_556 . ?
O1 Y1 N3 145.65(10) . 7_556 ?
O1 Y1 N3 121.87(11) 7_556 7_556 ?
O1 Y1 N3 121.87(11) . . ?
O1 Y1 N5 76.33(10) 7_556 . ?
O1 Y1 N5 76.33(10) . 7_556 ?
O1 Y1 N5 136.66(10) . . ?
O1 Y1 N5 136.66(10) 7_556 7_556 ?
N1 Y1 N1 153.00(15) 7_556 . ?
N1 Y1 N3 134.85(11) . 7_556 ?
N1 Y1 N3 71.07(11) 7_556 7_556 ?
N1 Y1 N3 134.85(11) 7_556 . ?
N1 Y1 N3 71.07(11) . . ?
N3 Y1 N3 70.62(16) . 7_556 ?
N5 Y1 N1 74.11(11) . . ?
N5 Y1 N1 114.33(11) 7_556 . ?
N5 Y1 N1 74.11(11) 7_556 7_556 ?
N5 Y1 N1 114.33(11) . 7_556 ?
N5 Y1 N3 77.15(11) 7_556 7_556 ?
N5 Y1 N3 74.89(11) 7_556 . ?
N5 Y1 N3 77.15(11) . . ?
N5 Y1 N3 74.89(11) . 7_556 ?
N5 Y1 N5 145.56(15) 7_556 . ?
C10 O1 Y1 120.9(2) . . ?
N2 N1 Y1 124.2(2) . . ?
C1 N1 Y1 130.3(3) . . ?
C1 N1 N2 105.3(3) . . ?
N1 N2 B1 121.4(3) . . ?
C3 N2 N1 110.5(3) . . ?
C3 N2 B1 128.0(4) . . ?
N4 N3 Y1 122.4(2) . . ?
C4 N3 Y1 130.6(3) . . ?
C4 N3 N4 105.1(3) . . ?
N3 N4 B1 121.7(3) . . ?
C6 N4 N3 109.9(3) . . ?
C6 N4 B1 128.4(4) . . ?
N6 N5 Y1 124.5(2) . . ?
C7 N5 Y1 129.0(3) . . ?
C7 N5 N6 106.4(3) . . ?
N5 N6 B1 121.9(3) . . ?
C9 N6 N5 109.6(3) . . ?
C9 N6 B1 128.5(4) . . ?
N1 C1 C2 110.9(4) . . ?
C3 C2 C1 105.2(4) . . ?
N2 C3 C2 108.1(4) . . ?
N3 C4 C5 111.8(4) . . ?
C6 C5 C4 104.3(4) . . ?
N4 C6 C5 108.9(4) . . ?
N5 C7 C8 110.5(4) . . ?
C9 C8 C7 104.7(4) . . ?
N6 C9 C8 108.8(4) . . ?
O1 C10 C10 115.1(2) . 7_556 ?
O1 C10 C11 119.0(4) . . ?
C11 C10 C10 125.8(2) . 7_556 ?
C12 C11 C10 130.5(4) . . ?
C11 C12 C13 130.2(4) . . ?
C12 C13 C12 126.8(5) 7_556 . ?
N2 B1 N4 108.2(3) . . ?
N2 B1 N6 110.3(4) . . ?
N4 B1 N6 108.8(3) . . ?

_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 2.140
_oxdiff_exptl_absorpt_empirical_full_min 0.655
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_er-trop
_database_code_depnum_ccdc_archive 'CCDC 2287863'
loop_
_audit_author_name
_audit_author_address
'Dunstan M.A.'
;Technical University of Denmark
Denmark
;
_audit_update_record             
;
2023-08-10 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_audit_creation_date             2022-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
majad@student.unimelb.edu.au
''
''
''
''
''
richardm@ansto.gov.au
c.boskovic@unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        
erbium(III)bis(tris-pyrazolylborato)(tropolonato)
_chemical_formula_moiety         'C25 H25 B2 Er N12 O2'
_chemical_formula_sum            'C25 H25 B2 Er N12 O2'
_chemical_formula_weight         714.45
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25 H25 Er O2 N12 B2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   9.32610(10)
_cell_length_b                   9.32610(10)
_cell_length_c                   31.8683(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2771.78(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6335
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7610
_cell_measurement_theta_min      4.9360
_shelx_estimated_absorpt_T_max   0.604
_shelx_estimated_absorpt_T_min   0.314
_exptl_absorpt_coefficient_mu    6.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.321
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 -1 0.0799
-1 -1 1 0.0342
0 0 -1 0.0925
1 2 2 0.0342
-1 -2 1 0.0306
1 -1 -2 0.0848
-1 2 1 0.0636
-1 2 -1 0.0680
0 -1 2 0.0826
-2 1 -2 0.0867
-1 -1 2 0.0487
-2 -1 2 0.0421
2 2 -1 0.0505
0 1 2 0.0476
0 1 1 0.0435
0 -1 -1 0.0665
0 -1 0 0.0599
-1 0 2 0.0545

_exptl_crystal_preparation       
'Reaction of KTp, Er(III) nitrate hexahydrate and tropolonate in methanol.'
_exptl_crystal_recrystallization_method 
'Hot recrystallisation in methanol/ethyl acetate.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.093
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.0006 0.9991 -0.9995 0.2328 -0.1086 -0.2699
-1.0004 -0.9993 1.0003 -0.1133 0.0117 0.2096
-0.0003 -0.0000 -1.0004 -0.0325 -0.0230 -0.0275
1.0018 1.9988 2.0001 0.2371 0.1656 -0.2489
-1.0010 -1.9987 1.0011 -0.1396 -0.0966 0.3313
0.9991 -0.9997 -1.9993 0.0282 -0.2512 0.0064
-0.9988 1.9992 0.9981 -0.0343 0.3365 -0.1556
-0.9993 1.9992 -1.0026 -0.0993 0.2905 -0.2105
-0.0000 -0.9995 2.0015 0.0387 -0.0623 0.1767
-2.0002 0.9999 -2.0031 -0.2776 0.2561 -0.0559
-1.0002 -0.9993 2.0007 -0.0808 0.0347 0.2370
-2.0003 -0.9991 1.9999 -0.2003 0.1316 0.2974
2.0011 1.9985 -1.0003 0.2591 -0.0003 -0.3916
0.0011 0.9995 2.0000 0.0913 0.1543 -0.0668
0.0008 0.9995 0.9997 0.0588 0.1313 -0.0942
-0.0008 -0.9995 -0.9997 -0.0588 -0.1313 0.0942
-0.0006 -0.9995 0.0007 -0.0263 -0.1083 0.1217
-0.9996 0.0002 2.0000 -0.0545 0.1429 0.1153

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9357
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.493
_diffrn_reflns_theta_min         4.941
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     86.00 178.00   0.50    0.09    --  105.86  75.00 -81.00  184
  2  ω     36.00  61.00   0.50    0.09    --  105.86 -61.00 -60.00   50
  3  ω     40.00  69.00   0.50    0.09    --  105.86 -61.00 -30.00   58
  4  ω     35.00  60.00   0.50    0.09    --  105.86 -56.00   5.00   50
  5  ω     39.00 101.00   0.50    0.09    --  105.86 -77.00  60.00  124
  6  ω     79.00 108.00   0.50    0.09    --  105.86-125.00 150.00   58
  7  ω   -109.00 -84.00   0.50    0.05    --  -47.57-125.00  60.00   50
  8  ω   -105.00 -79.00   0.50    0.05    --  -47.57-125.00 -60.00   52
  9  ω   -138.00 -86.00   0.50    0.09    --  -86.25 -95.00 -94.00  104
 10  ω    -50.00  20.00   0.50    0.05    --  -47.57  56.00 147.00  140
 11  ω     38.00  64.00   0.50    0.09    --  105.86-125.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1194382000
_diffrn_orient_matrix_UB_12      0.0262976000
_diffrn_orient_matrix_UB_13      0.0324522000
_diffrn_orient_matrix_UB_21      -0.0969156000
_diffrn_orient_matrix_UB_22      0.1083957000
_diffrn_orient_matrix_UB_23      0.0230093000
_diffrn_orient_matrix_UB_31      -0.0604079000
_diffrn_orient_matrix_UB_32      -0.1217290000
_diffrn_orient_matrix_UB_33      0.0274771000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.614
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                2716
_reflns_number_total             2822
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 
;
 Flack x determined using 1005 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.071
_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)+(0.0335P)²+1.6068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          'Stucture was refined with no disorder.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Er1 Er 0.39407(3) 0.60593(3) 0.250000 0.02197(12) Uani 1 2 d S T P . .
O1 O 0.1740(4) 0.6719(4) 0.27447(9) 0.0253(7) Uani 1 1 d . . . . .
N1 N 0.4702(5) 0.7714(4) 0.30706(12) 0.0266(9) Uani 1 1 d . . . . .
N2 N 0.5490(5) 0.7293(5) 0.34121(12) 0.0291(9) Uani 1 1 d . . . . .
N3 N 0.6488(4) 0.5495(5) 0.26925(12) 0.0278(8) Uani 1 1 d . . . . .
N4 N 0.6921(5) 0.5311(4) 0.30999(11) 0.0272(8) Uani 1 1 d . . . . .
N5 N 0.3662(4) 0.4706(4) 0.31479(12) 0.0255(9) Uani 1 1 d . . . . .
N6 N 0.4610(5) 0.4740(5) 0.34749(11) 0.0278(8) Uani 1 1 d . . . . .
C1 C 0.4576(5) 0.9131(6) 0.31033(15) 0.0296(10) Uani 1 1 d . . . . .
H1 H 0.407313 0.970305 0.291503 0.036 Uiso 1 1 calc R . . . .
C2 C 0.5298(6) 0.9650(6) 0.34569(15) 0.0325(11) Uani 1 1 d . . . . .
H2 H 0.537926 1.059645 0.354567 0.039 Uiso 1 1 calc R . . . .
C3 C 0.5861(6) 0.8443(5) 0.36441(14) 0.0313(11) Uani 1 1 d . . . . .
H3 H 0.640408 0.842447 0.388882 0.038 Uiso 1 1 calc R . . . .
C4 C 0.7573(5) 0.4990(5) 0.24604(16) 0.0313(10) Uani 1 1 d . . . . .
H4 H 0.757883 0.497716 0.216860 0.038 Uiso 1 1 calc R . . . .
C5 C 0.8684(5) 0.4488(6) 0.27078(15) 0.0309(10) Uani 1 1 d . . . . .
H5 H 0.954464 0.408461 0.261964 0.037 Uiso 1 1 calc R . . . .
C6 C 0.8235(6) 0.4719(6) 0.31114(16) 0.0307(11) Uani 1 1 d . . . . .
H6 H 0.875196 0.450291 0.335276 0.037 Uiso 1 1 calc R . . . .
C7 C 0.2661(5) 0.3747(6) 0.32489(16) 0.0312(10) Uani 1 1 d . . . . .
H7 H 0.187160 0.352052 0.308325 0.037 Uiso 1 1 calc R . . . .
C8 C 0.2963(6) 0.3126(6) 0.36396(15) 0.0352(11) Uani 1 1 d . . . . .
H8 H 0.244390 0.241952 0.377872 0.042 Uiso 1 1 calc R . . . .
C9 C 0.4198(5) 0.3795(5) 0.37715(14) 0.0322(11) Uani 1 1 d . . . . .
H9 H 0.467101 0.362348 0.402355 0.039 Uiso 1 1 calc R . . . .
C10 C 0.1186(6) 0.7934(5) 0.26394(13) 0.0262(9) Uani 1 1 d . . . . .
C11 C -0.0209(5) 0.8287(6) 0.27886(14) 0.0306(10) Uani 1 1 d . . . . .
H11 H -0.063772 0.758907 0.295503 0.037 Uiso 1 1 calc R . . . .
C12 C -0.1025(6) 0.9501(6) 0.27251(16) 0.0355(11) Uani 1 1 d . . . . .
H12 H -0.191734 0.948847 0.285509 0.043 Uiso 1 1 calc R . . . .
C13 C -0.0732(5) 1.0732(5) 0.250000 0.0363(16) Uani 1 2 d S T P . .
H13 H -0.143740 1.143734 0.249998 0.044 Uiso 1 2 calc RS T P . .
B1 B 0.5945(6) 0.5730(6) 0.34735(14) 0.0284(11) Uani 1 1 d . . . . .
H1A H 0.654658 0.561209 0.377567 0.034 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Er1 O1 2.280(3) 8_665 ?
Er1 O1 2.280(3) . ?
Er1 N1 2.489(4) 8_665 ?
Er1 N1 2.489(4) . ?
Er1 N3 2.510(4) 8_665 ?
Er1 N3 2.510(4) . ?
Er1 N5 2.434(4) 8_665 ?
Er1 N5 2.434(4) . ?
O1 C10 1.290(6) . ?
N1 N2 1.371(5) . ?
N1 C1 1.331(7) . ?
N2 C3 1.348(6) . ?
N2 B1 1.531(7) . ?
N3 N4 1.371(5) . ?
N3 C4 1.339(6) . ?
N4 C6 1.344(7) . ?
N4 B1 1.549(6) . ?
N5 N6 1.367(6) . ?
N5 C7 1.332(6) . ?
N6 C9 1.348(6) . ?
N6 B1 1.550(7) . ?
C1 C2 1.399(7) . ?
C2 C3 1.378(8) . ?
C4 C5 1.383(7) . ?
C5 C6 1.370(7) . ?
C7 C8 1.402(7) . ?
C8 C9 1.376(8) . ?
C10 C10 1.461(10) 8_665 ?
C10 C11 1.424(7) . ?
C11 C12 1.379(8) . ?
C12 C13 1.381(6) . ?

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
O1 Er1 O1 68.37(17) 8_665 . ?
O1 Er1 N1 80.77(13) . . ?
O1 Er1 N1 76.63(12) . 8_665 ?
O1 Er1 N1 76.63(12) 8_665 . ?
O1 Er1 N1 80.77(13) 8_665 8_665 ?
O1 Er1 N3 145.60(12) 8_665 8_665 ?
O1 Er1 N3 145.60(12) . . ?
O1 Er1 N3 121.85(14) 8_665 . ?
O1 Er1 N3 121.85(14) . 8_665 ?
O1 Er1 N5 136.74(12) 8_665 . ?
O1 Er1 N5 136.74(12) . 8_665 ?
O1 Er1 N5 75.73(12) . . ?
O1 Er1 N5 75.73(12) 8_665 8_665 ?
N1 Er1 N1 152.62(19) . 8_665 ?
N1 Er1 N3 134.90(13) 8_665 . ?
N1 Er1 N3 71.41(13) . . ?
N1 Er1 N3 134.90(13) . 8_665 ?
N1 Er1 N3 71.41(13) 8_665 8_665 ?
N3 Er1 N3 70.29(19) 8_665 . ?
N5 Er1 N1 113.92(13) . 8_665 ?
N5 Er1 N1 74.47(13) 8_665 8_665 ?
N5 Er1 N1 113.92(13) 8_665 . ?
N5 Er1 N1 74.47(13) . . ?
N5 Er1 N3 74.85(13) 8_665 . ?
N5 Er1 N3 77.59(13) 8_665 8_665 ?
N5 Er1 N3 74.85(13) . 8_665 ?
N5 Er1 N3 77.59(13) . . ?
N5 Er1 N5 146.14(19) 8_665 . ?
C10 O1 Er1 120.6(3) . . ?
N2 N1 Er1 123.7(3) . . ?
C1 N1 Er1 130.4(3) . . ?
C1 N1 N2 105.7(4) . . ?
N1 N2 B1 121.5(4) . . ?
C3 N2 N1 110.2(4) . . ?
C3 N2 B1 128.1(4) . . ?
N4 N3 Er1 122.5(3) . . ?
C4 N3 Er1 130.9(3) . . ?
C4 N3 N4 104.9(4) . . ?
N3 N4 B1 121.6(4) . . ?
C6 N4 N3 110.2(4) . . ?
C6 N4 B1 128.2(4) . . ?
N6 N5 Er1 124.4(3) . . ?
C7 N5 Er1 128.9(3) . . ?
C7 N5 N6 106.5(4) . . ?
N5 N6 B1 122.1(4) . . ?
C9 N6 N5 109.6(4) . . ?
C9 N6 B1 128.3(4) . . ?
N1 C1 C2 111.4(5) . . ?
C3 C2 C1 104.4(5) . . ?
N2 C3 C2 108.4(4) . . ?
N3 C4 C5 111.7(4) . . ?
C6 C5 C4 104.7(5) . . ?
N4 C6 C5 108.5(4) . . ?
N5 C7 C8 110.5(5) . . ?
C9 C8 C7 104.6(4) . . ?
N6 C9 C8 108.7(4) . . ?
O1 C10 C10 115.2(3) . 8_665 ?
O1 C10 C11 118.8(4) . . ?
C11 C10 C10 125.9(3) . 8_665 ?
C12 C11 C10 130.2(5) . . ?
C11 C12 C13 130.5(5) . . ?
C12 C13 C12 126.7(7) 8_665 . ?
N2 B1 N4 107.7(4) . . ?
N2 B1 N6 110.2(4) . . ?
N4 B1 N6 108.9(4) . . ?

_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 1.182
_oxdiff_exptl_absorpt_empirical_full_min 0.860
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_er-y-trop
_database_code_depnum_ccdc_archive 'CCDC 2287864'
loop_
_audit_author_name
_audit_author_address
'Dunstan M.A.'
;Technical University of Denmark
Denmark
;
_audit_update_record             
;
2023-08-10 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_audit_creation_date             2022-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
majad@student.unimelb.edu.au
''
''
''
''
''
richardm@ansto.gov.au
c.boskovic@unimelb.edu.au
_chemical_name_common            ?
_chemical_name_systematic        
erbium(III)@yttrium(III)bis(tris-pyrazolylborato)(tropolonato)
_chemical_formula_moiety         'C25 H25 B2 Er0.04 N12 O2 Y0.96'
_chemical_formula_sum            'C25 H25 B2 Er0.04 N12 O2 Y0.96'
_chemical_formula_weight         639.23
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Y0.9 Er0.1 C25 H25 N12 O2 B2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   9.33390(10)
_cell_length_b                   9.33390(10)
_cell_length_c                   31.9618(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2784.57(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7020
_cell_measurement_theta_min      4.9270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1301
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0312
-1 -1 -2 0.0341
0 1 1 0.0211
1 0 -2 0.0306
1 0 2 0.0409
0 -1 -2 0.0247
-1 1 2 0.0412
0 -2 -1 0.0247
-2 -2 -1 0.0344
2 -2 -1 0.0297
-1 2 -2 0.0412
1 -2 2 0.0352
0 -1 2 0.0393
1 -1 2 0.0374
0 0 -1 0.0538
0 0 1 0.0556
0 1 -2 0.0348
-1 0 1 0.0398
-1 0 -1 0.0389
1 1 -2 0.0281
-1 -1 2 0.0346

_exptl_crystal_preparation       
'Reaction of Y(III) nitrate hexahydrate or Er(III) nitrate hexahydrate with trispyrazolylborate and tropolonate. Crude compounds combined in 1:19 ratio before recrystallisation.'
_exptl_crystal_recrystallization_method 
'Recrystallisation from hot methanol/ethyl acetate.'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.046
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0002 0.0004 -0.0010 -0.0047 0.0196 -0.1638
-1.0002 -1.0015 -1.9967 -0.0094 -0.2091 0.1417
-0.0003 1.0006 0.9979 -0.0292 0.1683 0.0209
0.9998 -0.0006 -2.0005 -0.0912 -0.0228 -0.1664
1.0006 0.0014 1.9985 0.0818 0.0621 -0.1612
0.0001 -1.0011 -1.9976 -0.0140 -0.1895 -0.0222
-1.0003 1.0007 1.9986 0.0187 0.1699 0.1860
0.0007 -2.0007 -0.9960 0.1017 -0.3153 -0.0404
-1.9997 -2.0015 -0.9940 0.1110 -0.3546 0.2872
2.0012 -1.9998 -0.9980 0.0924 -0.2761 -0.3681
-1.0016 1.9987 -2.0023 -0.2268 0.2320 0.2004
1.0016 -1.9987 2.0023 0.2268 -0.2320 -0.2004
0.0009 -0.9991 2.0014 0.1590 -0.1046 -0.0170
1.0011 -0.9987 2.0004 0.1543 -0.0850 -0.1808
-0.0002 -0.0005 -0.9998 -0.0433 -0.0212 -0.0013
0.0002 0.0005 0.9998 0.0433 0.0212 0.0013
-0.0009 0.9991 -2.0014 -0.1590 0.1046 0.0170
-1.0000 0.0001 1.0007 0.0479 0.0016 0.1651
-1.0004 -0.0009 -0.9988 -0.0386 -0.0408 0.1625
0.9994 0.9995 -2.0024 -0.1636 0.1242 -0.1468
-0.9994 -0.9995 2.0024 0.1636 -0.1242 0.1468

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            9327
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.699
_diffrn_reflns_theta_min         4.936
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00 109.00   0.50    0.85    --  105.86-120.00-105.00  152
  2  ω     35.00  70.00   0.50    0.85    --  105.86 -61.00 150.00   70
  3  ω     36.00  71.00   0.50    0.85    --  105.86 -61.00 120.00   70
  4  ω     92.00 124.00   0.50    0.85    --  105.86  15.00   0.00   64
  5  ω    148.00 174.00   0.50    0.85    --  105.86  15.00   0.00   52
  6  ω    -33.00  10.00   0.50    0.21    --  -47.57  38.00  90.00   86
  7  ω    -92.00 -67.00   0.50    0.85    --  -86.25 155.00 135.00   50
  8  ω    -50.00 -23.00   0.50    0.85    --  -86.25  45.00 -90.00   54
  9  ω   -117.00 -75.00   0.50    0.21    --  -47.57-125.00  60.00   84
 10  ω   -115.00 -84.00   0.50    0.21    --  -47.57-125.00  30.00   62
 11  ω   -154.00 -96.00   0.50    0.85    --  -86.25-138.00  -4.00  116
 12  ω    -90.00 -65.00   0.50    0.85    --  -86.25-138.00  -4.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0045855000
_diffrn_orient_matrix_UB_12      -0.0723774000
_diffrn_orient_matrix_UB_13      0.0432974000
_diffrn_orient_matrix_UB_21      0.0195811000
_diffrn_orient_matrix_UB_22      0.1470872000
_diffrn_orient_matrix_UB_23      0.0211475000
_diffrn_orient_matrix_UB_31      -0.1637733000
_diffrn_orient_matrix_UB_32      0.0195038000
_diffrn_orient_matrix_UB_33      0.0013083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.603
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2673
_reflns_number_total             2772
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Flack x determined using 1000 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.037(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.078
_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/[σ²(Fo²)+(0.0283P)²+1.5955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0672
_refine_special_details          
'The structure was refined with the rare earth centre in two parts, one an Er(III) ion and one an Y(III) ion. The rare earth center occupancies were freely refined, with the overall occupancy summing to 1. The rare earth ions were refined to have the same position and equivalent atomic displacement parameters.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Shared sites
{Y1, Er1}
3. Uiso/Uaniso restraints and constraints
Uanis(Y1) = Uanis(Er1)
4. Others
 Sof(Er1)=0.5*(1-FVAR(2))
 Sof(Y1)=0.5*FVAR(2)
5.a Ternary CH refined with riding coordinates:
 B1(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Er1 Er 0.39403(3) 0.60597(3) 0.750000 0.01877(11) Uani 0.041(6) 2 d S T P A 2
Y1 Y 0.39403(3) 0.60597(3) 0.750000 0.01877(11) Uani 0.959(6) 2 d S T P A 1
O1 O 0.1733(3) 0.6724(3) 0.72562(7) 0.0233(5) Uani 1 1 d . . . . .
N1 N 0.4706(3) 0.7719(3) 0.69268(9) 0.0248(6) Uani 1 1 d . . . . .
N2 N 0.5497(3) 0.7303(3) 0.65894(9) 0.0263(7) Uani 1 1 d . . . . .
N3 N 0.6495(3) 0.5500(3) 0.73062(9) 0.0248(6) Uani 1 1 d . . . . .
N4 N 0.6930(3) 0.5320(3) 0.69007(8) 0.0247(6) Uani 1 1 d . . . . .
N5 N 0.3680(3) 0.4712(3) 0.68472(9) 0.0245(7) Uani 1 1 d . . . . .
N6 N 0.4628(3) 0.4747(3) 0.65252(8) 0.0245(6) Uani 1 1 d . . . . .
C1 C 0.4579(4) 0.9143(4) 0.68932(11) 0.0264(7) Uani 1 1 d . . . . .
H1 H 0.407424 0.971700 0.707984 0.032 Uiso 1 1 calc R . . . .
C2 C 0.5300(4) 0.9651(4) 0.65435(11) 0.0291(8) Uani 1 1 d . . . . .
H2 H 0.538279 1.059719 0.645533 0.035 Uiso 1 1 calc R . . . .
C3 C 0.5863(4) 0.8458(4) 0.63568(11) 0.0285(8) Uani 1 1 d . . . . .
H3 H 0.640294 0.844345 0.611235 0.034 Uiso 1 1 calc R . . . .
C4 C 0.7583(4) 0.4991(4) 0.75406(11) 0.0273(7) Uani 1 1 d . . . . .
H4 H 0.758584 0.497357 0.783149 0.033 Uiso 1 1 calc R . . . .
C5 C 0.8702(4) 0.4495(4) 0.72916(11) 0.0291(8) Uani 1 1 d . . . . .
H5 H 0.956507 0.409543 0.737839 0.035 Uiso 1 1 calc R . . . .
C6 C 0.8245(4) 0.4729(4) 0.68894(12) 0.0281(8) Uani 1 1 d . . . . .
H6 H 0.875937 0.451414 0.664830 0.034 Uiso 1 1 calc R . . . .
C7 C 0.2676(4) 0.3740(4) 0.67422(11) 0.0280(8) Uani 1 1 d . . . . .
H7 H 0.188776 0.350606 0.690664 0.034 Uiso 1 1 calc R . . . .
C8 C 0.2977(4) 0.3134(4) 0.63545(11) 0.0318(8) Uani 1 1 d . . . . .
H8 H 0.245783 0.243526 0.621323 0.038 Uiso 1 1 calc R . . . .
C9 C 0.4221(4) 0.3804(4) 0.62264(10) 0.0295(8) Uani 1 1 d . . . . .
H9 H 0.470013 0.363458 0.597611 0.035 Uiso 1 1 calc R . . . .
C10 C 0.1177(4) 0.7936(4) 0.73600(10) 0.0235(7) Uani 1 1 d . . . . .
C11 C -0.0198(4) 0.8286(4) 0.72101(11) 0.0273(8) Uani 1 1 d . . . . .
H11 H -0.061708 0.759227 0.704081 0.033 Uiso 1 1 calc R . . . .
C12 C -0.1027(4) 0.9498(4) 0.72745(12) 0.0323(8) Uani 1 1 d . . . . .
H12 H -0.192109 0.948035 0.714636 0.039 Uiso 1 1 calc R . . . .
C13 C -0.0732(4) 1.0732(4) 0.750000 0.0327(11) Uani 1 2 d S T P . .
H13 H -0.143688 1.143694 0.749998 0.039 Uiso 1 2 calc RS T P . .
B1 B 0.5954(5) 0.5737(4) 0.65283(11) 0.0262(8) Uani 1 1 d . . . . .
H1A H 0.655771 0.562233 0.622727 0.031 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Er1 O1 2.288(2) . ?
Er1 O1 2.288(2) 8_666 ?
Er1 N1 2.503(3) . ?
Er1 N1 2.503(3) 8_666 ?
Er1 N3 2.519(3) 8_666 ?
Er1 N3 2.519(3) . ?
Er1 N5 2.448(3) . ?
Er1 N5 2.448(3) 8_666 ?
Y1 O1 2.288(2) . ?
Y1 O1 2.288(2) 8_666 ?
Y1 N1 2.503(3) 8_666 ?
Y1 N1 2.503(3) . ?
Y1 N3 2.519(3) 8_666 ?
Y1 N3 2.519(3) . ?
Y1 N5 2.448(3) 8_666 ?
Y1 N5 2.448(3) . ?
O1 C10 1.289(4) . ?
N1 N2 1.363(4) . ?
N1 C1 1.339(5) . ?
N2 C3 1.354(5) . ?
N2 B1 1.535(5) . ?
N3 N4 1.368(4) . ?
N3 C4 1.348(4) . ?
N4 C6 1.346(5) . ?
N4 B1 1.549(5) . ?
N5 N6 1.357(4) . ?
N5 C7 1.347(5) . ?
N6 C9 1.353(4) . ?
N6 B1 1.545(5) . ?
C1 C2 1.388(5) . ?
C2 C3 1.368(5) . ?
C4 C5 1.392(5) . ?
C5 C6 1.372(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.380(5) . ?
C10 C10 1.474(7) 8_666 ?
C10 C11 1.408(5) . ?
C11 C12 1.386(5) . ?
C12 C13 1.387(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
O1 Er1 O1 68.17(12) . 8_666 ?
O1 Er1 N1 80.81(9) 8_666 8_666 ?
O1 Er1 N1 80.81(9) . . ?
O1 Er1 N1 76.68(9) . 8_666 ?
O1 Er1 N1 76.68(9) 8_666 . ?
O1 Er1 N3 121.80(10) . 8_666 ?
O1 Er1 N3 121.81(10) 8_666 . ?
O1 Er1 N3 145.58(9) . . ?
O1 Er1 N3 145.58(9) 8_666 8_666 ?
O1 Er1 N5 76.09(9) 8_666 8_666 ?
O1 Er1 N5 136.55(9) . 8_666 ?
O1 Er1 N5 76.09(9) . . ?
O1 Er1 N5 136.55(9) 8_666 . ?
N1 Er1 N1 152.76(13) 8_666 . ?
N1 Er1 N3 134.95(9) . 8_666 ?
N1 Er1 N3 71.21(10) 8_666 8_666 ?
N1 Er1 N3 134.95(9) 8_666 . ?
N1 Er1 N3 71.21(10) . . ?
N3 Er1 N3 70.58(14) . 8_666 ?
N5 Er1 N1 114.55(10) . 8_666 ?
N5 Er1 N1 114.55(10) 8_666 . ?
N5 Er1 N1 73.90(10) 8_666 8_666 ?
N5 Er1 N1 73.90(10) . . ?
N5 Er1 N3 77.17(9) . . ?
N5 Er1 N3 75.14(9) . 8_666 ?
N5 Er1 N3 77.17(9) 8_666 8_666 ?
N5 Er1 N3 75.14(9) 8_666 . ?
N5 Er1 N5 145.90(14) 8_666 . ?
O1 Y1 O1 68.17(12) . 8_666 ?
O1 Y1 N1 76.68(9) 8_666 . ?
O1 Y1 N1 76.68(9) . 8_666 ?
O1 Y1 N1 80.81(9) 8_666 8_666 ?
O1 Y1 N1 80.81(9) . . ?
O1 Y1 N3 145.58(9) . . ?
O1 Y1 N3 145.58(9) 8_666 8_666 ?
O1 Y1 N3 121.81(10) 8_666 . ?
O1 Y1 N3 121.80(10) . 8_666 ?
O1 Y1 N5 76.09(9) . . ?
O1 Y1 N5 76.09(9) 8_666 8_666 ?
O1 Y1 N5 136.55(9) 8_666 . ?
O1 Y1 N5 136.55(9) . 8_666 ?
N1 Y1 N1 152.76(13) 8_666 . ?
N1 Y1 N3 134.95(9) 8_666 . ?
N1 Y1 N3 71.21(10) 8_666 8_666 ?
N1 Y1 N3 134.95(9) . 8_666 ?
N1 Y1 N3 71.21(10) . . ?
N3 Y1 N3 70.58(14) . 8_666 ?
N5 Y1 N1 73.90(10) . . ?
N5 Y1 N1 73.90(10) 8_666 8_666 ?
N5 Y1 N1 114.55(10) . 8_666 ?
N5 Y1 N1 114.55(10) 8_666 . ?
N5 Y1 N3 75.14(9) 8_666 . ?
N5 Y1 N3 77.17(9) 8_666 8_666 ?
N5 Y1 N3 77.17(9) . . ?
N5 Y1 N3 75.14(9) . 8_666 ?
N5 Y1 N5 145.90(14) 8_666 . ?
C10 O1 Er1 120.9(2) . . ?
C10 O1 Y1 120.9(2) . . ?
N2 N1 Er1 123.9(2) . . ?
N2 N1 Y1 123.9(2) . . ?
C1 N1 Er1 130.4(2) . . ?
C1 N1 Y1 130.4(2) . . ?
C1 N1 N2 105.5(3) . . ?
N1 N2 B1 121.5(3) . . ?
C3 N2 N1 110.1(3) . . ?
C3 N2 B1 128.2(3) . . ?
N4 N3 Er1 122.6(2) . . ?
N4 N3 Y1 122.6(2) . . ?
C4 N3 Er1 130.5(2) . . ?
C4 N3 Y1 130.5(2) . . ?
C4 N3 N4 105.1(3) . . ?
N3 N4 B1 121.5(3) . . ?
C6 N4 N3 110.2(3) . . ?
C6 N4 B1 128.2(3) . . ?
N6 N5 Er1 124.7(2) . . ?
N6 N5 Y1 124.7(2) . . ?
C7 N5 Er1 128.9(2) . . ?
C7 N5 Y1 128.9(2) . . ?
C7 N5 N6 106.3(3) . . ?
N5 N6 B1 122.1(3) . . ?
C9 N6 N5 109.7(3) . . ?
C9 N6 B1 128.2(3) . . ?
N1 C1 C2 111.1(3) . . ?
C3 C2 C1 105.0(3) . . ?
N2 C3 C2 108.2(3) . . ?
N3 C4 C5 111.4(3) . . ?
C6 C5 C4 104.4(3) . . ?
N4 C6 C5 108.9(3) . . ?
N5 C7 C8 110.8(3) . . ?
C9 C8 C7 104.5(3) . . ?
N6 C9 C8 108.7(3) . . ?
O1 C10 C10 115.03(18) . 8_666 ?
O1 C10 C11 118.9(3) . . ?
C11 C10 C10 126.0(2) . 8_666 ?
C12 C11 C10 130.3(4) . . ?
C11 C12 C13 130.2(4) . . ?
C12 C13 C12 126.8(5) . 8_666 ?
N2 B1 N4 107.8(3) . . ?
N2 B1 N6 110.3(3) . . ?
N6 B1 N4 109.0(3) . . ?

_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.875
