# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_Cmpd1
_audit_block_doi                 10.5517/ccdc.csd.cc2dr80g
_database_code_depnum_ccdc_archive 'CCDC 2226885'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 La N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 La N21 O6'
_chemical_formula_weight         913.03

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.473(5)
_cell_length_b                   13.830(3)
_cell_length_c                   29.778(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.898(5)
_cell_angle_gamma                90
_cell_volume                     8988(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    935
_cell_measurement_theta_min      3.492
_cell_measurement_theta_max      40.32

_exptl_crystal_description       Diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_F_000             3648

_exptl_crystal_size_max          0.996
_exptl_crystal_size_mid          0.523
_exptl_crystal_size_min          0.304
_exptl_absorpt_coefficient_mu    1.011

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62132
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.024
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9128
_reflns_number_gt                7976
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0138P)²+10.6401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9128
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0477
_refine_ls_wR_factor_gt          0.0460
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
La1 La 0.31122(2) 0.66166(2) 0.37570(2) 0.01297(3) Uani 1 1 d . . . . .
O1 O 0.08664(7) 0.86060(11) 0.40376(7) 0.0419(4) Uani 1 1 d . . . . .
O2 O 0.11684(7) 1.01052(10) 0.41437(6) 0.0363(4) Uani 1 1 d . . . . .
O3 O 0.31513(7) 0.19582(10) 0.34033(6) 0.0338(4) Uani 1 1 d . . . . .
O4 O 0.22988(7) 0.15453(9) 0.34147(5) 0.0312(3) Uani 1 1 d . . . . .
O5 O 0.54813(7) 0.92812(10) 0.41032(7) 0.0406(4) Uani 1 1 d . . . . .
O6 O 0.60125(6) 0.82129(11) 0.39307(6) 0.0353(4) Uani 1 1 d . . . . .
N1 N 0.25690(7) 0.90678(10) 0.38881(5) 0.0160(3) Uani 1 1 d . . . . .
N2 N 0.23835(7) 0.81124(10) 0.38122(6) 0.0177(3) Uani 1 1 d . . . . .
N3 N 0.32742(7) 0.90829(10) 0.34778(5) 0.0162(3) Uani 1 1 d . . . . .
N4 N 0.31548(7) 0.81763(10) 0.32670(5) 0.0171(3) Uani 1 1 d . . . . .
N5 N 0.36898(7) 0.88420(11) 0.44272(6) 0.0178(3) Uani 1 1 d . . . . .
N6 N 0.36949(7) 0.78612(10) 0.44921(5) 0.0169(3) Uani 1 1 d . . . . .
N7 N 0.12120(8) 0.92541(12) 0.40393(7) 0.0279(4) Uani 1 1 d . . . . .
N8 N 0.21043(7) 0.44708(10) 0.35235(5) 0.0168(3) Uani 1 1 d . . . . .
N9 N 0.26630(7) 0.47379(10) 0.35590(6) 0.0174(3) Uani 1 1 d . . . . .
N10 N 0.15234(7) 0.59799(11) 0.31120(6) 0.0180(3) Uani 1 1 d . . . . .
N11 N 0.19636(7) 0.64987(10) 0.30578(6) 0.0180(3) Uani 1 1 d . . . . .
N12 N 0.19537(7) 0.57139(10) 0.40633(6) 0.0168(3) Uani 1 1 d . . . . .
N13 N 0.25309(7) 0.61027(10) 0.42775(6) 0.0166(3) Uani 1 1 d . . . . .
N14 N 0.26750(8) 0.21525(11) 0.34297(6) 0.0236(4) Uani 1 1 d . . . . .
N15 N 0.46517(7) 0.63578(10) 0.38269(6) 0.0175(3) Uani 1 1 d . . . . .
N16 N 0.42834(7) 0.70361(11) 0.38931(6) 0.0178(3) Uani 1 1 d . . . . .
N17 N 0.38792(7) 0.52013(11) 0.32212(6) 0.0182(3) Uani 1 1 d . . . . .
N18 N 0.33649(7) 0.57540(10) 0.30876(6) 0.0173(3) Uani 1 1 d . . . . .
N19 N 0.43348(7) 0.49174(11) 0.41675(6) 0.0193(3) Uani 1 1 d . . . . .
N20 N 0.39420(7) 0.53430(11) 0.43217(6) 0.0193(3) Uani 1 1 d . . . . .
N21 N 0.55669(7) 0.84534(12) 0.39956(6) 0.0266(4) Uani 1 1 d . . . . .
C1 C 0.18588(8) 0.80819(13) 0.38372(7) 0.0204(4) Uani 1 1 d . . . . .
H1A H 0.162075 0.751638 0.379702 0.024 Uiso 1 1 calc R U . . .
C2 C 0.17074(8) 0.90048(13) 0.39314(7) 0.0202(4) Uani 1 1 d . . . . .
C3 C 0.21660(8) 0.96115(13) 0.39596(7) 0.0188(4) Uani 1 1 d . . . . .
H3A H 0.219105 1.028880 0.401877 0.023 Uiso 1 1 calc R U . . .
C4 C 0.32814(9) 0.82212(13) 0.28755(7) 0.0202(4) Uani 1 1 d . . . . .
H4 H 0.324174 0.769395 0.265832 0.024 Uiso 1 1 calc R U . . .
C5 C 0.34788(9) 0.91402(13) 0.28277(7) 0.0234(4) Uani 1 1 d . . . . .
H5 H 0.359561 0.935859 0.258105 0.028 Uiso 1 1 calc R U . . .
C6 C 0.34678(8) 0.96623(13) 0.32148(7) 0.0199(4) Uani 1 1 d . . . . .
H6 H 0.357843 1.032348 0.328594 0.024 Uiso 1 1 calc R U . . .
C7 C 0.41501(9) 0.76888(14) 0.49501(7) 0.0226(4) Uani 1 1 d . . . . .
H7 H 0.426150 0.706458 0.509666 0.027 Uiso 1 1 calc R U . . .
C8 C 0.44402(9) 0.85422(15) 0.51849(8) 0.0287(5) Uani 1 1 d . . . . .
H8 H 0.477494 0.861550 0.551042 0.034 Uiso 1 1 calc R U . . .
C9 C 0.41352(9) 0.92536(14) 0.48416(7) 0.0244(4) Uani 1 1 d . . . . .
H9 H 0.422310 0.992572 0.488808 0.029 Uiso 1 1 calc R U . . .
C10 C 0.29341(9) 0.39269(12) 0.35278(7) 0.0185(4) Uani 1 1 d . . . . .
H10 H 0.332622 0.388646 0.353636 0.022 Uiso 1 1 calc R U . . .
C11 C 0.25532(9) 0.31442(12) 0.34806(7) 0.0184(4) Uani 1 1 d . . . . .
C12 C 0.20310(9) 0.35154(12) 0.34795(7) 0.0188(4) Uani 1 1 d . . . . .
H12 H 0.168546 0.315957 0.345253 0.023 Uiso 1 1 calc R U . . .
C13 C 0.16682(9) 0.70179(14) 0.26380(7) 0.0232(4) Uani 1 1 d . . . . .
H13 H 0.186233 0.745160 0.250774 0.028 Uiso 1 1 calc R U . . .
C14 C 0.10455(10) 0.68454(15) 0.24171(8) 0.0315(5) Uani 1 1 d . . . . .
H14 H 0.073758 0.712142 0.211714 0.038 Uiso 1 1 calc R U . . .
C15 C 0.09722(9) 0.61826(15) 0.27302(8) 0.0288(5) Uani 1 1 d . . . . .
H15 H 0.059337 0.591250 0.268386 0.035 Uiso 1 1 calc R U . . .
C16 C 0.26290(9) 0.64076(12) 0.47344(7) 0.0190(4) Uani 1 1 d . . . . .
H16 H 0.299513 0.671126 0.496992 0.023 Uiso 1 1 calc R U . . .
C17 C 0.21243(9) 0.62213(13) 0.48192(7) 0.0215(4) Uani 1 1 d . . . . .
H17 H 0.207747 0.637058 0.511122 0.026 Uiso 1 1 calc R U . . .
C18 C 0.17091(9) 0.57741(13) 0.43873(7) 0.0202(4) Uani 1 1 d . . . . .
H18 H 0.131579 0.554553 0.432706 0.024 Uiso 1 1 calc R U . . .
C19 C 0.45781(8) 0.78703(13) 0.39672(7) 0.0193(4) Uani 1 1 d . . . . .
H19 H 0.443529 0.847303 0.402574 0.023 Uiso 1 1 calc R U . . .
C20 C 0.51285(8) 0.77281(13) 0.39461(7) 0.0199(4) Uani 1 1 d . . . . .
C21 C 0.51616(8) 0.67597(13) 0.38570(7) 0.0204(4) Uani 1 1 d . . . . .
H21 H 0.548478 0.644001 0.382336 0.024 Uiso 1 1 calc R U . . .
C22 C 0.29735(9) 0.54677(13) 0.26247(7) 0.0208(4) Uani 1 1 d . . . . .
H22 H 0.257511 0.572985 0.243561 0.025 Uiso 1 1 calc R U . . .
C23 C 0.32223(9) 0.47393(14) 0.24551(7) 0.0263(4) Uani 1 1 d . . . . .
H23 H 0.303724 0.441505 0.213994 0.032 Uiso 1 1 calc R U . . .
C24 C 0.37945(9) 0.45913(14) 0.28434(7) 0.0252(4) Uani 1 1 d . . . . .
H24 H 0.408459 0.413244 0.284563 0.030 Uiso 1 1 calc R U . . .
C25 C 0.39709(9) 0.48030(14) 0.47039(7) 0.0246(4) Uani 1 1 d . . . . .
H25 H 0.374505 0.492829 0.488631 0.029 Uiso 1 1 calc R U . . .
C26 C 0.43751(10) 0.40329(15) 0.48000(8) 0.0298(5) Uani 1 1 d . . . . .
H26 H 0.447686 0.354642 0.505038 0.036 Uiso 1 1 calc R U . . .
C27 C 0.45933(9) 0.41347(13) 0.44518(8) 0.0264(4) Uani 1 1 d . . . . .
H27 H 0.488098 0.371875 0.441730 0.032 Uiso 1 1 calc R U . . .
B1 B 0.32098(10) 0.93606(15) 0.39520(8) 0.0171(4) Uani 1 1 d . . . . .
H1 H 0.3281(9) 1.0124(15) 0.4021(7) 0.026 Uiso 1 1 d . U . . .
B2 B 0.16596(10) 0.52398(15) 0.35397(8) 0.0185(4) Uani 1 1 d . . . . .
H2 H 0.1233(9) 0.4887(14) 0.3474(7) 0.028 Uiso 1 1 d . U . . .
B3 B 0.44535(10) 0.52856(15) 0.37328(8) 0.0199(4) Uani 1 1 d . . . . .
H3 H 0.4821(10) 0.4857(15) 0.3715(7) 0.030 Uiso 1 1 d . U . . .


_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
La1 N18 2.6256(15) . ?
La1 N13 2.6321(15) . ?
La1 N4 2.6326(15) . ?
La1 N6 2.6389(15) . ?
La1 N20 2.6390(15) . ?
La1 N11 2.6396(16) . ?
La1 N16 2.7686(16) . ?
La1 N9 2.7786(15) . ?
La1 N2 2.7843(15) . ?
O1 N7 1.231(2) . ?
O2 N7 1.234(2) . ?
O3 N14 1.233(2) . ?
O4 N14 1.232(2) . ?
O5 N21 1.232(2) . ?
O6 N21 1.236(2) . ?
N1 C3 1.332(2) . ?
N1 N2 1.382(2) . ?
N1 B1 1.546(3) . ?
N2 C1 1.320(2) . ?
N3 C6 1.347(2) . ?
N3 N4 1.373(2) . ?
N3 B1 1.539(2) . ?
N4 C4 1.336(2) . ?
N5 C9 1.348(2) . ?
N5 N6 1.369(2) . ?
N5 B1 1.547(3) . ?
N6 C7 1.335(2) . ?
N7 C2 1.430(2) . ?
N8 C12 1.332(2) . ?
N8 N9 1.373(2) . ?
N8 B2 1.538(3) . ?
N9 C10 1.328(2) . ?
N10 C15 1.343(2) . ?
N10 N11 1.363(2) . ?
N10 B2 1.548(3) . ?
N11 C13 1.335(2) . ?
N12 C18 1.349(2) . ?
N12 N13 1.370(2) . ?
N12 B2 1.537(3) . ?
N13 C16 1.338(2) . ?
N14 C11 1.426(2) . ?
N15 C21 1.332(2) . ?
N15 N16 1.375(2) . ?
N15 B3 1.546(3) . ?
N16 C19 1.325(2) . ?
N17 C24 1.345(2) . ?
N17 N18 1.369(2) . ?
N17 B3 1.540(3) . ?
N18 C22 1.334(2) . ?
N19 C27 1.343(2) . ?
N19 N20 1.371(2) . ?
N19 B3 1.536(3) . ?
N20 C25 1.336(2) . ?
N21 C20 1.427(2) . ?
C1 C2 1.393(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.373(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.371(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.394(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.392(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.373(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.390(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.392(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.372(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.07(2) . ?
B2 H2 1.09(2) . ?
B3 H3 1.10(2) . ?

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
N18 La1 N13 134.44(5) . . ?
N18 La1 N4 82.51(5) . . ?
N13 La1 N4 135.65(4) . . ?
N18 La1 N6 134.56(5) . . ?
N13 La1 N6 85.46(5) . . ?
N4 La1 N6 77.48(5) . . ?
N18 La1 N20 78.63(5) . . ?
N13 La1 N20 84.81(5) . . ?
N4 La1 N20 133.48(5) . . ?
N6 La1 N20 86.30(5) . . ?
N18 La1 N11 84.59(5) . . ?
N13 La1 N11 77.37(5) . . ?
N4 La1 N11 84.75(5) . . ?
N6 La1 N11 132.65(4) . . ?
N20 La1 N11 134.37(5) . . ?
N18 La1 N16 67.82(4) . . ?
N13 La1 N16 140.35(5) . . ?
N4 La1 N16 67.14(5) . . ?
N6 La1 N16 66.84(4) . . ?
N20 La1 N16 66.38(5) . . ?
N11 La1 N16 142.27(5) . . ?
N18 La1 N9 67.70(4) . . ?
N13 La1 N9 66.74(4) . . ?
N4 La1 N9 139.44(4) . . ?
N6 La1 N9 143.07(4) . . ?
N20 La1 N9 68.14(5) . . ?
N11 La1 N9 66.23(4) . . ?
N16 La1 N9 120.73(4) . . ?
N18 La1 N2 139.43(4) . . ?
N13 La1 N2 68.56(4) . . ?
N4 La1 N2 67.11(5) . . ?
N6 La1 N2 65.58(5) . . ?
N20 La1 N2 141.91(5) . . ?
N11 La1 N2 67.08(4) . . ?
N16 La1 N2 118.95(4) . . ?
N9 La1 N2 120.32(5) . . ?
C3 N1 N2 110.72(14) . . ?
C3 N1 B1 128.01(15) . . ?
N2 N1 B1 120.69(14) . . ?
C1 N2 N1 106.09(14) . . ?
C1 N2 La1 130.16(12) . . ?
N1 N2 La1 123.25(10) . . ?
C6 N3 N4 109.60(14) . . ?
C6 N3 B1 126.42(15) . . ?
N4 N3 B1 123.95(14) . . ?
C4 N4 N3 105.73(14) . . ?
C4 N4 La1 127.19(11) . . ?
N3 N4 La1 123.26(10) . . ?
C9 N5 N6 109.70(15) . . ?
C9 N5 B1 127.32(16) . . ?
N6 N5 B1 122.90(14) . . ?
C7 N6 N5 105.73(15) . . ?
C7 N6 La1 128.23(12) . . ?
N5 N6 La1 124.20(11) . . ?
O1 N7 O2 123.91(17) . . ?
O1 N7 C2 118.32(16) . . ?
O2 N7 C2 117.73(17) . . ?
C12 N8 N9 111.06(15) . . ?
C12 N8 B2 128.57(16) . . ?
N9 N8 B2 120.37(14) . . ?
C10 N9 N8 106.20(14) . . ?
C10 N9 La1 129.98(12) . . ?
N8 N9 La1 123.52(10) . . ?
C15 N10 N11 109.56(15) . . ?
C15 N10 B2 126.47(16) . . ?
N11 N10 B2 123.90(15) . . ?
C13 N11 N10 105.77(15) . . ?
C13 N11 La1 129.60(12) . . ?
N10 N11 La1 123.76(11) . . ?
C18 N12 N13 109.90(14) . . ?
C18 N12 B2 126.61(15) . . ?
N13 N12 B2 123.42(14) . . ?
C16 N13 N12 105.68(14) . . ?
C16 N13 La1 128.13(12) . . ?
N12 N13 La1 123.37(10) . . ?
O4 N14 O3 124.17(16) . . ?
O4 N14 C11 118.08(17) . . ?
O3 N14 C11 117.75(16) . . ?
C21 N15 N16 111.14(14) . . ?
C21 N15 B3 128.32(15) . . ?
N16 N15 B3 120.53(14) . . ?
C19 N16 N15 105.97(14) . . ?
C19 N16 La1 131.02(12) . . ?
N15 N16 La1 122.56(10) . . ?
C24 N17 N18 109.50(15) . . ?
C24 N17 B3 126.94(16) . . ?
N18 N17 B3 123.56(14) . . ?
C22 N18 N17 105.69(14) . . ?
C22 N18 La1 127.85(12) . . ?
N17 N18 La1 122.31(11) . . ?
C27 N19 N20 109.66(16) . . ?
C27 N19 B3 125.70(16) . . ?
N20 N19 B3 124.64(14) . . ?
C25 N20 N19 105.68(15) . . ?
C25 N20 La1 130.16(13) . . ?
N19 N20 La1 121.80(11) . . ?
O5 N21 O6 123.81(16) . . ?
O5 N21 C20 118.15(16) . . ?
O6 N21 C20 118.04(16) . . ?
N2 C1 C2 109.65(16) . . ?
N2 C1 H1A 125.2 . . ?
C2 C1 H1A 125.2 . . ?
C3 C2 C1 106.72(16) . . ?
C3 C2 N7 126.27(17) . . ?
C1 C2 N7 126.60(17) . . ?
N1 C3 C2 106.81(16) . . ?
N1 C3 H3A 126.6 . . ?
C2 C3 H3A 126.6 . . ?
N4 C4 C5 111.12(16) . . ?
N4 C4 H4 124.4 . . ?
C5 C4 H4 124.4 . . ?
C6 C5 C4 104.82(16) . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
N3 C6 C5 108.74(16) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 111.22(17) . . ?
N6 C7 H7 124.4 . . ?
C8 C7 H7 124.4 . . ?
C9 C8 C7 104.60(17) . . ?
C9 C8 H8 127.7 . . ?
C7 C8 H8 127.7 . . ?
N5 C9 C8 108.75(17) . . ?
N5 C9 H9 125.6 . . ?
C8 C9 H9 125.6 . . ?
N9 C10 C11 109.31(17) . . ?
N9 C10 H10 125.3 . . ?
C11 C10 H10 125.3 . . ?
C12 C11 C10 106.77(16) . . ?
C12 C11 N14 126.67(17) . . ?
C10 C11 N14 126.53(17) . . ?
N8 C12 C11 106.65(16) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N11 C13 C14 111.50(17) . . ?
N11 C13 H13 124.3 . . ?
C14 C13 H13 124.3 . . ?
C15 C14 C13 104.28(18) . . ?
C15 C14 H14 127.9 . . ?
C13 C14 H14 127.9 . . ?
N10 C15 C14 108.89(18) . . ?
N10 C15 H15 125.6 . . ?
C14 C15 H15 125.6 . . ?
N13 C16 C17 111.11(17) . . ?
N13 C16 H16 124.4 . . ?
C17 C16 H16 124.4 . . ?
C18 C17 C16 104.76(16) . . ?
C18 C17 H17 127.6 . . ?
C16 C17 H17 127.6 . . ?
N12 C18 C17 108.53(16) . . ?
N12 C18 H18 125.7 . . ?
C17 C18 H18 125.7 . . ?
N16 C19 C20 109.56(16) . . ?
N16 C19 H19 125.2 . . ?
C20 C19 H19 125.2 . . ?
C21 C20 C19 106.82(16) . . ?
C21 C20 N21 126.69(17) . . ?
C19 C20 N21 126.47(17) . . ?
N15 C21 C20 106.51(16) . . ?
N15 C21 H21 126.7 . . ?
C20 C21 H21 126.7 . . ?
N18 C22 C23 111.35(17) . . ?
N18 C22 H22 124.3 . . ?
C23 C22 H22 124.3 . . ?
C24 C23 C22 104.54(17) . . ?
C24 C23 H23 127.7 . . ?
C22 C23 H23 127.7 . . ?
N17 C24 C23 108.91(17) . . ?
N17 C24 H24 125.5 . . ?
C23 C24 H24 125.5 . . ?
N20 C25 C26 111.20(18) . . ?
N20 C25 H25 124.4 . . ?
C26 C25 H25 124.4 . . ?
C27 C26 C25 104.44(17) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 109.01(18) . . ?
N19 C27 H27 125.5 . . ?
C26 C27 H27 125.5 . . ?
N3 B1 N1 109.93(15) . . ?
N3 B1 N5 111.91(15) . . ?
N1 B1 N5 107.42(15) . . ?
N3 B1 H1 110.1(11) . . ?
N1 B1 H1 110.5(11) . . ?
N5 B1 H1 106.9(11) . . ?
N12 B2 N8 108.28(15) . . ?
N12 B2 N10 112.35(15) . . ?
N8 B2 N10 108.86(15) . . ?
N12 B2 H2 110.2(11) . . ?
N8 B2 H2 108.7(11) . . ?
N10 B2 H2 108.4(11) . . ?
N19 B3 N17 111.86(16) . . ?
N19 B3 N15 109.19(15) . . ?
N17 B3 N15 108.85(15) . . ?
N19 B3 H3 109.4(11) . . ?
N17 B3 H3 108.2(11) . . ?
N15 B3 H3 109.3(11) . . ?

_refine_diff_density_max         0.310
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.055



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Cmpd8
_audit_block_doi                 10.5517/ccdc.csd.cc2dr88q
_database_code_depnum_ccdc_archive 'CCDC 2226893'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Tb N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 N21 O6 Tb'
_chemical_formula_weight         933.04

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.248(2)
_cell_length_b                   13.7248(17)
_cell_length_c                   28.843(4)
_cell_angle_alpha                90
_cell_angle_beta                 112.506(4)
_cell_angle_gamma                90
_cell_volume                     8867.9(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1536
_cell_measurement_theta_min      3.485
_cell_measurement_theta_max      47.45

_exptl_crystal_description       diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             3712

_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.376
_exptl_crystal_size_min          0.213
_exptl_absorpt_coefficient_mu    1.656

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21226
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.875
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             8999
_reflns_number_gt                7086
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8999
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

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
Tb1 Tb 0.68550(2) 0.41111(2) 0.62465(2) 0.01197(5) Uani 1 1 d . . . . .
O1 O 0.44991(11) 0.75671(18) 0.58616(10) 0.0352(7) Uani 1 1 d . . . . .
O2 O 0.43124(11) 0.60609(18) 0.59957(12) 0.0399(8) Uani 1 1 d . . . . .
O3 O 0.63970(11) -0.09837(16) 0.65740(9) 0.0286(6) Uani 1 1 d . . . . .
O4 O 0.72661(11) -0.05659(16) 0.65709(10) 0.0300(6) Uani 1 1 d . . . . .
O5 O 0.95806(11) 0.57436(18) 0.60624(10) 0.0332(7) Uani 1 1 d . . . . .
O6 O 0.88658(12) 0.68195(17) 0.58849(11) 0.0376(7) Uani 1 1 d . . . . .
N1 N 0.61694(11) 0.65303(18) 0.61101(10) 0.0138(6) Uani 1 1 d . . . . .
N2 N 0.60638(12) 0.55677(18) 0.61916(10) 0.0144(6) Uani 1 1 d . . . . .
N3 N 0.67479(11) 0.62452(18) 0.55734(10) 0.0137(6) Uani 1 1 d . . . . .
N4 N 0.66986(11) 0.52494(18) 0.55267(10) 0.0149(6) Uani 1 1 d . . . . .
N5 N 0.72869(11) 0.65121(18) 0.65147(10) 0.0149(6) Uani 1 1 d . . . . .
N6 N 0.73774(11) 0.55946(18) 0.67224(10) 0.0142(6) Uani 1 1 d . . . . .
N7 N 0.46535(13) 0.6715(2) 0.59778(11) 0.0255(7) Uani 1 1 d . . . . .
N8 N 0.60988(12) 0.19716(18) 0.64812(10) 0.0152(6) Uani 1 1 d . . . . .
N9 N 0.66232(12) 0.22387(18) 0.64390(10) 0.0161(6) Uani 1 1 d . . . . .
N10 N 0.54234(11) 0.32325(18) 0.59452(10) 0.0153(6) Uani 1 1 d . . . . .
N11 N 0.57947(12) 0.36329(18) 0.57392(10) 0.0152(6) Uani 1 1 d . . . . .
N12 N 0.59520(12) 0.35044(18) 0.68873(10) 0.0154(6) Uani 1 1 d . . . . .
N13 N 0.64487(12) 0.40272(18) 0.69234(10) 0.0154(6) Uani 1 1 d . . . . .
N14 N 0.67616(14) -0.0367(2) 0.65532(10) 0.0223(7) Uani 1 1 d . . . . .
N15 N 0.83164(12) 0.38740(18) 0.61731(10) 0.0149(6) Uani 1 1 d . . . . .
N16 N 0.78773(11) 0.45537(18) 0.61100(10) 0.0156(6) Uani 1 1 d . . . . .
N17 N 0.76325(12) 0.24564(18) 0.58332(10) 0.0159(6) Uani 1 1 d . . . . .
N18 N 0.70881(12) 0.28922(19) 0.56967(10) 0.0162(6) Uani 1 1 d . . . . .
N19 N 0.81305(11) 0.27324(18) 0.67762(10) 0.0158(6) Uani 1 1 d . . . . .
N20 N 0.77316(11) 0.32845(18) 0.68949(10) 0.0143(6) Uani 1 1 d . . . . .
N21 N 0.90650(13) 0.5988(2) 0.59965(11) 0.0243(7) Uani 1 1 d . . . . .
C1 C 0.55132(15) 0.5538(2) 0.61736(12) 0.0183(8) Uani 1 1 d . . . . .
H1A H 0.531603 0.496740 0.621706 0.022 Uiso 1 1 calc R U . . .
C2 C 0.52628(15) 0.6467(2) 0.60814(13) 0.0179(7) Uani 1 1 d . . . . .
C3 C 0.56885(14) 0.7084(2) 0.60402(12) 0.0170(7) Uani 1 1 d . . . . .
H3A H 0.564972 0.776454 0.597543 0.020 Uiso 1 1 calc R U . . .
C4 C 0.66867(14) 0.5055(2) 0.50717(12) 0.0196(8) Uani 1 1 d . . . . .
H4 H 0.665475 0.441645 0.493618 0.024 Uiso 1 1 calc R U . . .
C5 C 0.67264(15) 0.5893(2) 0.48181(13) 0.0248(8) Uani 1 1 d . . . . .
H5 H 0.672913 0.594320 0.449048 0.030 Uiso 1 1 calc R U . . .
C6 C 0.67609(15) 0.6633(2) 0.51463(12) 0.0201(8) Uani 1 1 d . . . . .
H6 H 0.678927 0.730710 0.508453 0.024 Uiso 1 1 calc R U . . .
C7 C 0.78933(14) 0.5643(2) 0.71210(12) 0.0168(7) Uani 1 1 d . . . . .
H7 H 0.806968 0.511048 0.733783 0.020 Uiso 1 1 calc R U . . .
C8 C 0.81381(15) 0.6574(2) 0.71767(12) 0.0196(8) Uani 1 1 d . . . . .
H8 H 0.849983 0.679557 0.742888 0.023 Uiso 1 1 calc R U . . .
C9 C 0.77428(15) 0.7099(2) 0.67882(12) 0.0193(8) Uani 1 1 d . . . . .
H9 H 0.778244 0.776736 0.672146 0.023 Uiso 1 1 calc R U . . .
C10 C 0.69244(15) 0.1425(2) 0.64647(12) 0.0173(7) Uani 1 1 d . . . . .
H10 H 0.730972 0.138559 0.645241 0.021 Uiso 1 1 calc R U . . .
C11 C 0.65898(14) 0.0631(2) 0.65126(12) 0.0160(7) Uani 1 1 d . . . . .
C12 C 0.60650(15) 0.1005(2) 0.65223(11) 0.0161(7) Uani 1 1 d . . . . .
H12 H 0.574475 0.064733 0.655228 0.019 Uiso 1 1 calc R U . . .
C13 C 0.54406(14) 0.3923(2) 0.52801(12) 0.0156(7) Uani 1 1 d . . . . .
H13 H 0.557657 0.423012 0.504821 0.019 Uiso 1 1 calc R U . . .
C14 C 0.48444(15) 0.3715(2) 0.51855(13) 0.0200(8) Uani 1 1 d . . . . .
H14 H 0.450668 0.384956 0.488828 0.024 Uiso 1 1 calc R U . . .
C15 C 0.48506(14) 0.3277(2) 0.56110(12) 0.0176(7) Uani 1 1 d . . . . .
H15 H 0.451107 0.304287 0.566455 0.021 Uiso 1 1 calc R U . . .
C16 C 0.65864(15) 0.4562(2) 0.73419(12) 0.0198(8) Uani 1 1 d . . . . .
H16 H 0.690907 0.501009 0.745830 0.024 Uiso 1 1 calc R U . . .
C17 C 0.62048(16) 0.4383(2) 0.75822(13) 0.0260(9) Uani 1 1 d . . . . .
H17 H 0.621563 0.465742 0.788796 0.031 Uiso 1 1 calc R U . . .
C18 C 0.58028(16) 0.3716(3) 0.72800(13) 0.0250(8) Uani 1 1 d . . . . .
H18 H 0.547419 0.344852 0.733910 0.030 Uiso 1 1 calc R U . . .
C19 C 0.80983(15) 0.5391(2) 0.60294(12) 0.0171(7) Uani 1 1 d . . . . .
H19 H 0.789288 0.599696 0.596641 0.021 Uiso 1 1 calc R U . . .
C20 C 0.86758(15) 0.5251(2) 0.60508(12) 0.0186(8) Uani 1 1 d . . . . .
C21 C 0.87988(15) 0.4281(2) 0.61423(12) 0.0177(7) Uani 1 1 d . . . . .
H21 H 0.915959 0.395932 0.617719 0.021 Uiso 1 1 calc R U . . .
C22 C 0.67166(16) 0.2372(2) 0.53102(12) 0.0207(8) Uani 1 1 d . . . . .
H22 H 0.630389 0.250813 0.513798 0.025 Uiso 1 1 calc R U . . .
C23 C 0.70199(17) 0.1602(2) 0.51950(13) 0.0262(9) Uani 1 1 d . . . . .
H23 H 0.686297 0.112899 0.493737 0.031 Uiso 1 1 calc R U . . .
C24 C 0.75937(16) 0.1684(2) 0.55373(13) 0.0221(8) Uani 1 1 d . . . . .
H24 H 0.791379 0.126171 0.556157 0.027 Uiso 1 1 calc R U . . .
C25 C 0.78100(15) 0.3017(2) 0.73626(12) 0.0183(8) Uani 1 1 d . . . . .
H25 H 0.759115 0.327995 0.754509 0.022 Uiso 1 1 calc R U . . .
C26 C 0.82493(15) 0.2311(2) 0.75484(13) 0.0224(8) Uani 1 1 d . . . . .
H26 H 0.838791 0.200761 0.786877 0.027 Uiso 1 1 calc R U . . .
C27 C 0.84363(15) 0.2153(2) 0.71645(13) 0.0219(8) Uani 1 1 d . . . . .
H27 H 0.873679 0.170306 0.717116 0.026 Uiso 1 1 calc R U . . .
B1 B 0.67501(17) 0.6802(3) 0.60419(15) 0.0166(8) Uani 1 1 d . . . . .
H1 H 0.6786(13) 0.758(2) 0.5971(12) 0.025 Uiso 1 1 d . U . . .
B2 B 0.56410(17) 0.2760(3) 0.64672(14) 0.0159(8) Uani 1 1 d . . . . .
H2 H 0.5257(14) 0.247(2) 0.6549(12) 0.024 Uiso 1 1 d . U . . .
B3 B 0.82036(18) 0.2796(3) 0.62689(15) 0.0170(8) Uani 1 1 d D . . . .
H3 H 0.8584(11) 0.235(2) 0.6284(12) 0.025 Uiso 1 1 d D U . . .


_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
Tb1 N20 2.502(3) . ?
Tb1 N13 2.504(3) . ?
Tb1 N4 2.508(3) . ?
Tb1 N11 2.510(3) . ?
Tb1 N6 2.511(2) . ?
Tb1 N18 2.514(3) . ?
Tb1 N16 2.723(3) . ?
Tb1 N9 2.733(3) . ?
Tb1 N2 2.733(3) . ?
O1 N7 1.235(3) . ?
O2 N7 1.235(4) . ?
O3 N14 1.242(3) . ?
O4 N14 1.235(3) . ?
O5 N21 1.237(4) . ?
O6 N21 1.232(3) . ?
N1 C3 1.341(4) . ?
N1 N2 1.383(3) . ?
N1 B1 1.540(4) . ?
N2 C1 1.317(4) . ?
N3 C6 1.353(4) . ?
N3 N4 1.374(3) . ?
N3 B1 1.550(5) . ?
N4 C4 1.329(4) . ?
N5 C9 1.351(4) . ?
N5 N6 1.375(3) . ?
N5 B1 1.534(5) . ?
N6 C7 1.338(4) . ?
N7 C2 1.432(4) . ?
N8 C12 1.337(4) . ?
N8 N9 1.373(3) . ?
N8 B2 1.540(4) . ?
N9 C10 1.321(4) . ?
N10 C15 1.355(4) . ?
N10 N11 1.370(3) . ?
N10 B2 1.535(4) . ?
N11 C13 1.334(4) . ?
N12 C18 1.346(4) . ?
N12 N13 1.371(3) . ?
N12 B2 1.543(4) . ?
N13 C16 1.341(4) . ?
N14 C11 1.423(4) . ?
N15 C21 1.329(4) . ?
N15 N16 1.374(3) . ?
N15 B3 1.548(4) . ?
N16 C19 1.326(4) . ?
N17 C24 1.341(4) . ?
N17 N18 1.363(3) . ?
N17 B3 1.543(5) . ?
N18 C22 1.340(4) . ?
N19 C27 1.341(4) . ?
N19 N20 1.371(3) . ?
N19 B3 1.542(5) . ?
N20 C25 1.339(4) . ?
N21 C20 1.432(4) . ?
C1 C2 1.393(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.375(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.387(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.392(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.397(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.361(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.374(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.369(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.398(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.368(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.365(5) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.09(3) . ?
B2 H2 1.12(3) . ?
B3 H3 1.092(17) . ?

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
N20 Tb1 N13 82.62(8) . . ?
N20 Tb1 N4 135.82(8) . . ?
N13 Tb1 N4 133.96(8) . . ?
N20 Tb1 N11 134.80(8) . . ?
N13 Tb1 N11 79.72(9) . . ?
N4 Tb1 N11 83.33(8) . . ?
N20 Tb1 N6 81.52(8) . . ?
N13 Tb1 N6 82.98(8) . . ?
N4 Tb1 N6 80.34(8) . . ?
N11 Tb1 N6 136.10(8) . . ?
N20 Tb1 N18 80.67(8) . . ?
N13 Tb1 N18 135.39(8) . . ?
N4 Tb1 N18 83.78(8) . . ?
N11 Tb1 N18 83.44(8) . . ?
N6 Tb1 N18 134.14(8) . . ?
N20 Tb1 N16 69.47(8) . . ?
N13 Tb1 N16 140.78(8) . . ?
N4 Tb1 N16 66.36(8) . . ?
N11 Tb1 N16 139.46(8) . . ?
N6 Tb1 N16 66.51(8) . . ?
N18 Tb1 N16 67.69(8) . . ?
N20 Tb1 N9 66.65(8) . . ?
N13 Tb1 N9 68.00(8) . . ?
N4 Tb1 N9 140.91(8) . . ?
N11 Tb1 N9 68.17(8) . . ?
N6 Tb1 N9 138.73(8) . . ?
N18 Tb1 N9 67.40(8) . . ?
N16 Tb1 N9 120.57(8) . . ?
N20 Tb1 N2 138.74(8) . . ?
N13 Tb1 N2 66.53(8) . . ?
N4 Tb1 N2 67.42(8) . . ?
N11 Tb1 N2 67.53(8) . . ?
N6 Tb1 N2 68.57(8) . . ?
N18 Tb1 N2 140.59(8) . . ?
N16 Tb1 N2 119.08(8) . . ?
N9 Tb1 N2 120.35(8) . . ?
C3 N1 N2 111.1(3) . . ?
C3 N1 B1 128.9(3) . . ?
N2 N1 B1 119.4(2) . . ?
C1 N2 N1 105.9(3) . . ?
C1 N2 Tb1 131.1(2) . . ?
N1 N2 Tb1 122.48(18) . . ?
C6 N3 N4 109.5(3) . . ?
C6 N3 B1 127.3(3) . . ?
N4 N3 B1 123.1(3) . . ?
C4 N4 N3 105.4(3) . . ?
C4 N4 Tb1 129.1(2) . . ?
N3 N4 Tb1 123.96(18) . . ?
C9 N5 N6 109.4(3) . . ?
C9 N5 B1 126.2(3) . . ?
N6 N5 B1 124.3(3) . . ?
C7 N6 N5 105.7(2) . . ?
C7 N6 Tb1 128.3(2) . . ?
N5 N6 Tb1 122.77(19) . . ?
O1 N7 O2 124.2(3) . . ?
O1 N7 C2 117.6(3) . . ?
O2 N7 C2 118.2(3) . . ?
C12 N8 N9 111.3(3) . . ?
C12 N8 B2 129.2(3) . . ?
N9 N8 B2 119.5(2) . . ?
C10 N9 N8 106.3(3) . . ?
C10 N9 Tb1 130.9(2) . . ?
N8 N9 Tb1 122.59(18) . . ?
C15 N10 N11 109.8(3) . . ?
C15 N10 B2 126.2(3) . . ?
N11 N10 B2 124.0(3) . . ?
C13 N11 N10 105.7(3) . . ?
C13 N11 Tb1 128.8(2) . . ?
N10 N11 Tb1 123.29(19) . . ?
C18 N12 N13 109.5(3) . . ?
C18 N12 B2 126.6(3) . . ?
N13 N12 B2 123.9(3) . . ?
C16 N13 N12 105.3(3) . . ?
C16 N13 Tb1 129.8(2) . . ?
N12 N13 Tb1 124.15(19) . . ?
O4 N14 O3 124.0(3) . . ?
O4 N14 C11 118.1(3) . . ?
O3 N14 C11 117.9(3) . . ?
C21 N15 N16 111.3(2) . . ?
C21 N15 B3 129.3(3) . . ?
N16 N15 B3 119.4(3) . . ?
C19 N16 N15 105.5(3) . . ?
C19 N16 Tb1 132.1(2) . . ?
N15 N16 Tb1 122.10(18) . . ?
C24 N17 N18 109.8(3) . . ?
C24 N17 B3 125.4(3) . . ?
N18 N17 B3 124.8(3) . . ?
C22 N18 N17 106.0(3) . . ?
C22 N18 Tb1 129.6(2) . . ?
N17 N18 Tb1 122.46(19) . . ?
C27 N19 N20 109.7(3) . . ?
C27 N19 B3 126.7(3) . . ?
N20 N19 B3 123.6(3) . . ?
C25 N20 N19 105.0(3) . . ?
C25 N20 Tb1 129.0(2) . . ?
N19 N20 Tb1 122.86(19) . . ?
O6 N21 O5 124.3(3) . . ?
O6 N21 C20 118.3(3) . . ?
O5 N21 C20 117.4(3) . . ?
N2 C1 C2 109.9(3) . . ?
N2 C1 H1A 125.1 . . ?
C2 C1 H1A 125.1 . . ?
C3 C2 C1 107.1(3) . . ?
C3 C2 N7 125.7(3) . . ?
C1 C2 N7 126.6(3) . . ?
N1 C3 C2 106.0(3) . . ?
N1 C3 H3A 127.0 . . ?
C2 C3 H3A 127.0 . . ?
N4 C4 C5 112.0(3) . . ?
N4 C4 H4 124.0 . . ?
C5 C4 H4 124.0 . . ?
C6 C5 C4 104.4(3) . . ?
C6 C5 H5 127.8 . . ?
C4 C5 H5 127.8 . . ?
N3 C6 C5 108.8(3) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 111.2(3) . . ?
N6 C7 H7 124.4 . . ?
C8 C7 H7 124.4 . . ?
C9 C8 C7 104.8(3) . . ?
C9 C8 H8 127.6 . . ?
C7 C8 H8 127.6 . . ?
N5 C9 C8 108.9(3) . . ?
N5 C9 H9 125.5 . . ?
C8 C9 H9 125.5 . . ?
N9 C10 C11 109.6(3) . . ?
N9 C10 H10 125.2 . . ?
C11 C10 H10 125.2 . . ?
C12 C11 C10 106.6(3) . . ?
C12 C11 N14 126.8(3) . . ?
C10 C11 N14 126.6(3) . . ?
N8 C12 C11 106.2(3) . . ?
N8 C12 H12 126.9 . . ?
C11 C12 H12 126.9 . . ?
N11 C13 C14 111.0(3) . . ?
N11 C13 H13 124.5 . . ?
C14 C13 H13 124.5 . . ?
C15 C14 C13 105.1(3) . . ?
C15 C14 H14 127.4 . . ?
C13 C14 H14 127.4 . . ?
N10 C15 C14 108.4(3) . . ?
N10 C15 H15 125.8 . . ?
C14 C15 H15 125.8 . . ?
N13 C16 C17 111.9(3) . . ?
N13 C16 H16 124.1 . . ?
C17 C16 H16 124.1 . . ?
C16 C17 C18 104.4(3) . . ?
C16 C17 H17 127.8 . . ?
C18 C17 H17 127.8 . . ?
N12 C18 C17 108.8(3) . . ?
N12 C18 H18 125.6 . . ?
C17 C18 H18 125.6 . . ?
N16 C19 C20 109.9(3) . . ?
N16 C19 H19 125.1 . . ?
C20 C19 H19 125.1 . . ?
C21 C20 C19 106.5(3) . . ?
C21 C20 N21 127.2(3) . . ?
C19 C20 N21 126.3(3) . . ?
N15 C21 C20 106.8(3) . . ?
N15 C21 H21 126.6 . . ?
C20 C21 H21 126.6 . . ?
N18 C22 C23 110.7(3) . . ?
N18 C22 H22 124.7 . . ?
C23 C22 H22 124.7 . . ?
C24 C23 C22 104.4(3) . . ?
C24 C23 H23 127.8 . . ?
C22 C23 H23 127.8 . . ?
N17 C24 C23 109.2(3) . . ?
N17 C24 H24 125.4 . . ?
C23 C24 H24 125.4 . . ?
N20 C25 C26 111.9(3) . . ?
N20 C25 H25 124.1 . . ?
C26 C25 H25 124.1 . . ?
C27 C26 C25 104.0(3) . . ?
C27 C26 H26 128.0 . . ?
C25 C26 H26 128.0 . . ?
N19 C27 C26 109.5(3) . . ?
N19 C27 H27 125.2 . . ?
C26 C27 H27 125.2 . . ?
N5 B1 N1 109.3(3) . . ?
N5 B1 N3 111.5(3) . . ?
N1 B1 N3 107.1(3) . . ?
N5 B1 H1 108.6(17) . . ?
N1 B1 H1 113.6(16) . . ?
N3 B1 H1 106.9(17) . . ?
N10 B2 N8 107.2(3) . . ?
N10 B2 N12 111.8(3) . . ?
N8 B2 N12 108.3(3) . . ?
N10 B2 H2 110.8(16) . . ?
N8 B2 H2 113.4(16) . . ?
N12 B2 H2 105.4(16) . . ?
N19 B3 N17 111.2(3) . . ?
N19 B3 N15 108.4(3) . . ?
N17 B3 N15 108.0(3) . . ?
N19 B3 H3 109.5(17) . . ?
N17 B3 H3 110.2(17) . . ?
N15 B3 H3 109.5(17) . . ?

_refine_diff_density_max         0.612
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.097



_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Cmpd4
_audit_block_doi                 10.5517/ccdc.csd.cc2dr83k
_database_code_depnum_ccdc_archive 'CCDC 2226888'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Nd N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 N21 Nd O6'
_chemical_formula_weight         918.36

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'
B B 0.0013 0.0007 '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'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.3443(7)
_cell_length_b                   13.7711(3)
_cell_length_c                   28.8113(11)
_cell_angle_alpha                90
_cell_angle_beta                 112.5370(10)
_cell_angle_gamma                90
_cell_volume                     8921.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    424
_cell_measurement_theta_min      3.494
_cell_measurement_theta_max      39.30

_exptl_crystal_description       diamond
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_F_000             3672

_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    1.224

_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8192
_exptl_absorpt_correction_T_max  0.9318
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
 Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination" J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41569
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.031
_diffrn_reflns_theta_max         25.692
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8463
_reflns_number_gt                6813
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8463
_refine_ls_number_parameters     533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Nd1 Nd 0.68563(2) 0.58871(2) 0.62448(2) 0.01212(5) Uani 1 1 d . . . . .
O1 O 0.43196(10) 0.39152(16) 0.59741(10) 0.0380(6) Uani 1 1 d . . . . .
O2 O 0.45124(10) 0.24125(16) 0.58568(9) 0.0347(6) Uani 1 1 d . . . . .
O3 O 0.72579(10) 1.05513(14) 0.65837(8) 0.0297(6) Uani 1 1 d . . . . .
O4 O 0.63907(10) 1.09689(14) 0.65792(8) 0.0282(5) Uani 1 1 d . . . . .
O5 O 0.95830(10) 0.42788(16) 0.60679(9) 0.0333(6) Uani 1 1 d . . . . .
O6 O 0.88746(11) 0.32009(16) 0.58990(10) 0.0386(6) Uani 1 1 d . . . . .
N1 N 0.61764(10) 0.34531(16) 0.61110(8) 0.0140(5) Uani 1 1 d . . . . .
N2 N 0.60693(11) 0.44148(16) 0.61900(9) 0.0167(6) Uani 1 1 d . . . . .
N3 N 0.72967(10) 0.34532(15) 0.65208(9) 0.0148(5) Uani 1 1 d . . . . .
N4 N 0.73846(10) 0.43638(16) 0.67324(9) 0.0150(5) Uani 1 1 d . . . . .
N5 N 0.67587(10) 0.37067(16) 0.55761(9) 0.0152(5) Uani 1 1 d . . . . .
N6 N 0.67025(10) 0.46937(16) 0.55182(9) 0.0160(5) Uani 1 1 d . . . . .
N7 N 0.46644(12) 0.32645(19) 0.59649(10) 0.0262(6) Uani 1 1 d . . . . .
N8 N 0.60899(10) 0.80245(16) 0.64772(9) 0.0145(5) Uani 1 1 d . . . . .
N9 N 0.66140(10) 0.77630(16) 0.64368(9) 0.0158(5) Uani 1 1 d . . . . .
N10 N 0.59297(11) 0.65076(16) 0.68858(9) 0.0165(6) Uani 1 1 d . . . . .
N11 N 0.64268(10) 0.59877(16) 0.69345(9) 0.0160(5) Uani 1 1 d . . . . .
N12 N 0.54042(10) 0.67761(16) 0.59370(9) 0.0144(5) Uani 1 1 d . . . . .
N13 N 0.57716(10) 0.63808(16) 0.57263(9) 0.0155(5) Uani 1 1 d . . . . .
N14 N 0.67528(12) 1.03592(18) 0.65630(9) 0.0223(6) Uani 1 1 d . . . . .
N15 N 0.83228(10) 0.61379(16) 0.61779(9) 0.0149(5) Uani 1 1 d . . . . .
N16 N 0.78846(10) 0.54555(16) 0.61121(9) 0.0160(5) Uani 1 1 d . . . . .
N17 N 0.81453(10) 0.72870(16) 0.67787(9) 0.0153(5) Uani 1 1 d . . . . .
N18 N 0.77573(10) 0.67316(16) 0.69045(9) 0.0141(5) Uani 1 1 d . . . . .
N19 N 0.76522(11) 0.75682(16) 0.58335(9) 0.0165(5) Uani 1 1 d . . . . .
N20 N 0.71039(11) 0.71309(16) 0.56862(9) 0.0169(6) Uani 1 1 d . . . . .
N21 N 0.90700(12) 0.40310(19) 0.60043(10) 0.0257(6) Uani 1 1 d . . . . .
C1 C 0.55176(13) 0.4441(2) 0.61652(11) 0.0183(7) Uani 1 1 d . . . . .
H1A H 0.531815 0.500866 0.620503 0.022 Uiso 1 1 calc R U . . .
C2 C 0.52697(13) 0.3513(2) 0.60719(11) 0.0184(7) Uani 1 1 d . . . . .
C3 C 0.56994(13) 0.2912(2) 0.60420(11) 0.0188(7) Uani 1 1 d . . . . .
H3A H 0.566451 0.223186 0.598276 0.023 Uiso 1 1 calc R U . . .
C4 C 0.79019(13) 0.4313(2) 0.71274(11) 0.0180(7) Uani 1 1 d . . . . .
H4 H 0.807797 0.484087 0.734635 0.022 Uiso 1 1 calc R U . . .
C5 C 0.81481(14) 0.3395(2) 0.71769(11) 0.0214(7) Uani 1 1 d . . . . .
H5 H 0.851247 0.317623 0.742506 0.026 Uiso 1 1 calc R U . . .
C6 C 0.77512(13) 0.2871(2) 0.67897(11) 0.0190(7) Uani 1 1 d . . . . .
H6 H 0.779019 0.220501 0.672188 0.023 Uiso 1 1 calc R U . . .
C7 C 0.66944(13) 0.4875(2) 0.50623(11) 0.0195(7) Uani 1 1 d . . . . .
H7 H 0.665735 0.550471 0.491915 0.023 Uiso 1 1 calc R U . . .
C8 C 0.67472(14) 0.4022(2) 0.48204(12) 0.0255(7) Uani 1 1 d . . . . .
H8 H 0.675449 0.395905 0.449445 0.031 Uiso 1 1 calc R U . . .
C9 C 0.67860(14) 0.3300(2) 0.51555(11) 0.0210(7) Uani 1 1 d . . . . .
H9 H 0.682548 0.262617 0.510377 0.025 Uiso 1 1 calc R U . . .
C10 C 0.69172(13) 0.8572(2) 0.64649(11) 0.0171(7) Uani 1 1 d . . . . .
H10 H 0.730153 0.861005 0.645351 0.021 Uiso 1 1 calc R U . . .
C11 C 0.65817(13) 0.93642(19) 0.65140(10) 0.0171(7) Uani 1 1 d . . . . .
C12 C 0.60575(13) 0.89872(19) 0.65201(10) 0.0165(7) Uani 1 1 d . . . . .
H12 H 0.573770 0.934267 0.654901 0.020 Uiso 1 1 calc R U . . .
C13 C 0.65587(14) 0.5465(2) 0.73490(11) 0.0202(7) Uani 1 1 d . . . . .
H13 H 0.688363 0.502565 0.747196 0.024 Uiso 1 1 calc R U . . .
C14 C 0.61623(15) 0.5639(2) 0.75820(12) 0.0268(8) Uani 1 1 d . . . . .
H14 H 0.616286 0.536319 0.788452 0.032 Uiso 1 1 calc R U . . .
C15 C 0.57692(15) 0.6302(2) 0.72723(12) 0.0258(8) Uani 1 1 d . . . . .
H15 H 0.543767 0.657220 0.732342 0.031 Uiso 1 1 calc R U . . .
C16 C 0.54157(13) 0.60851(19) 0.52691(11) 0.0170(7) Uani 1 1 d . . . . .
H16 H 0.554938 0.578071 0.503549 0.020 Uiso 1 1 calc R U . . .
C17 C 0.48216(14) 0.6281(2) 0.51787(11) 0.0194(7) Uani 1 1 d . . . . .
H17 H 0.448270 0.613853 0.488419 0.023 Uiso 1 1 calc R U . . .
C18 C 0.48348(13) 0.67248(19) 0.56089(11) 0.0185(7) Uani 1 1 d . . . . .
H18 H 0.449863 0.695723 0.566605 0.022 Uiso 1 1 calc R U . . .
C19 C 0.81064(13) 0.4617(2) 0.60352(11) 0.0172(7) Uani 1 1 d . . . . .
H19 H 0.790367 0.401207 0.597511 0.021 Uiso 1 1 calc R U . . .
C20 C 0.86811(13) 0.4761(2) 0.60562(11) 0.0177(7) Uani 1 1 d . . . . .
C21 C 0.88034(13) 0.57316(19) 0.61458(11) 0.0168(7) Uani 1 1 d . . . . .
H21 H 0.916201 0.605212 0.617868 0.020 Uiso 1 1 calc R U . . .
C22 C 0.78319(13) 0.7010(2) 0.73710(10) 0.0171(7) Uani 1 1 d . . . . .
H22 H 0.761948 0.674527 0.755747 0.021 Uiso 1 1 calc R U . . .
C23 C 0.82562(14) 0.7731(2) 0.75460(11) 0.0228(7) Uani 1 1 d . . . . .
H23 H 0.838914 0.804769 0.786296 0.027 Uiso 1 1 calc R U . . .
C24 C 0.84421(14) 0.7885(2) 0.71599(11) 0.0228(7) Uani 1 1 d . . . . .
H24 H 0.873467 0.834314 0.716173 0.027 Uiso 1 1 calc R U . . .
C25 C 0.67452(14) 0.7663(2) 0.53013(11) 0.0207(7) Uani 1 1 d . . . . .
H25 H 0.633434 0.753329 0.512277 0.025 Uiso 1 1 calc R U . . .
C26 C 0.70502(15) 0.8431(2) 0.51954(12) 0.0266(8) Uani 1 1 d . . . . .
H26 H 0.689781 0.890805 0.493985 0.032 Uiso 1 1 calc R U . . .
C27 C 0.76228(15) 0.8342(2) 0.55446(12) 0.0243(8) Uani 1 1 d . . . . .
H27 H 0.794449 0.876168 0.557533 0.029 Uiso 1 1 calc R U . . .
B1 B 0.67590(15) 0.3169(2) 0.60479(13) 0.0161(7) Uani 1 1 d . . . . .
B2 B 0.56266(16) 0.7252(2) 0.64596(13) 0.0180(8) Uani 1 1 d . . . . .
H2 H 0.5287(13) 0.760(2) 0.6537(11) 0.027 Uiso 1 1 d . U . . .
B3 B 0.82105(16) 0.7212(2) 0.62705(13) 0.0186(8) Uani 1 1 d . . . . .
H3 H 0.8595(13) 0.766(2) 0.6274(10) 0.028 Uiso 1 1 d . U . . .
H1 H 0.6739(12) 0.239(2) 0.5981(10) 0.025(8) Uiso 1 1 d . . . . .


_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
Nd1 N18 2.565(2) . ?
Nd1 N6 2.573(2) . ?
Nd1 N20 2.575(2) . ?
Nd1 N13 2.577(2) . ?
Nd1 N4 2.577(2) . ?
Nd1 N11 2.579(2) . ?
Nd1 N16 2.738(2) . ?
Nd1 N2 2.752(2) . ?
Nd1 N9 2.753(2) . ?
O1 N7 1.235(3) . ?
O2 N7 1.234(3) . ?
O3 N14 1.237(3) . ?
O4 N14 1.231(3) . ?
O5 N21 1.239(3) . ?
O6 N21 1.231(3) . ?
N1 C3 1.329(3) . ?
N1 N2 1.385(3) . ?
N1 B1 1.548(4) . ?
N2 C1 1.318(4) . ?
N3 C6 1.345(3) . ?
N3 N4 1.375(3) . ?
N3 B1 1.535(4) . ?
N4 C4 1.337(4) . ?
N5 C9 1.360(4) . ?
N5 N6 1.370(3) . ?
N5 B1 1.548(4) . ?
N6 C7 1.330(3) . ?
N7 C2 1.427(4) . ?
N8 C12 1.337(3) . ?
N8 N9 1.373(3) . ?
N8 B2 1.537(4) . ?
N9 C10 1.321(3) . ?
N10 C15 1.344(4) . ?
N10 N11 1.366(3) . ?
N10 B2 1.552(4) . ?
N11 C13 1.324(4) . ?
N12 C18 1.348(4) . ?
N12 N13 1.371(3) . ?
N12 B2 1.538(4) . ?
N13 C16 1.333(3) . ?
N14 C11 1.423(3) . ?
N15 C21 1.332(3) . ?
N15 N16 1.379(3) . ?
N15 B3 1.545(4) . ?
N16 C19 1.329(3) . ?
N17 C24 1.341(4) . ?
N17 N18 1.368(3) . ?
N17 B3 1.535(4) . ?
N18 C22 1.341(3) . ?
N19 C27 1.337(3) . ?
N19 N20 1.375(3) . ?
N19 B3 1.537(4) . ?
N20 C25 1.337(3) . ?
N21 C20 1.428(4) . ?
C1 C2 1.395(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.362(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.396(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.364(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.403(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.394(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.372(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.391(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.377(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.09(3) . ?
B2 H2 1.05(3) . ?
B3 H3 1.12(3) . ?

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
N18 Nd1 N6 135.14(7) . . ?
N18 Nd1 N20 79.81(7) . . ?
N6 Nd1 N20 84.97(7) . . ?
N18 Nd1 N13 134.83(7) . . ?
N6 Nd1 N13 84.24(7) . . ?
N20 Nd1 N13 84.01(7) . . ?
N18 Nd1 N4 81.88(7) . . ?
N6 Nd1 N4 79.06(7) . . ?
N20 Nd1 N4 134.00(7) . . ?
N13 Nd1 N4 135.80(7) . . ?
N18 Nd1 N11 83.61(7) . . ?
N6 Nd1 N11 133.27(7) . . ?
N20 Nd1 N11 134.98(7) . . ?
N13 Nd1 N11 78.73(7) . . ?
N4 Nd1 N11 83.61(7) . . ?
N18 Nd1 N16 68.53(7) . . ?
N6 Nd1 N16 66.65(7) . . ?
N20 Nd1 N16 67.15(7) . . ?
N13 Nd1 N16 139.88(7) . . ?
N4 Nd1 N16 66.90(7) . . ?
N11 Nd1 N16 141.38(7) . . ?
N18 Nd1 N2 139.05(7) . . ?
N6 Nd1 N2 66.54(7) . . ?
N20 Nd1 N2 141.15(7) . . ?
N13 Nd1 N2 67.98(7) . . ?
N4 Nd1 N2 67.83(7) . . ?
N11 Nd1 N2 66.73(7) . . ?
N16 Nd1 N2 119.05(7) . . ?
N18 Nd1 N9 67.28(7) . . ?
N6 Nd1 N9 141.93(7) . . ?
N20 Nd1 N9 67.72(7) . . ?
N13 Nd1 N9 67.55(7) . . ?
N4 Nd1 N9 139.01(7) . . ?
N11 Nd1 N9 67.26(7) . . ?
N16 Nd1 N9 120.63(7) . . ?
N2 Nd1 N9 120.32(7) . . ?
C3 N1 N2 110.6(2) . . ?
C3 N1 B1 128.9(2) . . ?
N2 N1 B1 120.0(2) . . ?
C1 N2 N1 105.6(2) . . ?
C1 N2 Nd1 130.95(18) . . ?
N1 N2 Nd1 122.88(16) . . ?
C6 N3 N4 109.5(2) . . ?
C6 N3 B1 126.3(2) . . ?
N4 N3 B1 124.1(2) . . ?
C4 N4 N3 105.4(2) . . ?
C4 N4 Nd1 128.09(18) . . ?
N3 N4 Nd1 122.70(16) . . ?
C9 N5 N6 109.7(2) . . ?
C9 N5 B1 127.0(2) . . ?
N6 N5 B1 123.2(2) . . ?
C7 N6 N5 105.6(2) . . ?
C7 N6 Nd1 128.78(19) . . ?
N5 N6 Nd1 123.93(17) . . ?
O2 N7 O1 123.7(3) . . ?
O2 N7 C2 117.9(3) . . ?
O1 N7 C2 118.4(3) . . ?
C12 N8 N9 111.0(2) . . ?
C12 N8 B2 128.4(3) . . ?
N9 N8 B2 120.7(2) . . ?
C10 N9 N8 106.8(2) . . ?
C10 N9 Nd1 130.2(2) . . ?
N8 N9 Nd1 122.74(16) . . ?
C15 N10 N11 109.4(2) . . ?
C15 N10 B2 126.4(3) . . ?
N11 N10 B2 124.1(2) . . ?
C13 N11 N10 106.0(2) . . ?
C13 N11 Nd1 129.5(2) . . ?
N10 N11 Nd1 123.62(17) . . ?
C18 N12 N13 109.8(2) . . ?
C18 N12 B2 126.2(3) . . ?
N13 N12 B2 123.9(2) . . ?
C16 N13 N12 105.8(2) . . ?
C16 N13 Nd1 128.73(19) . . ?
N12 N13 Nd1 123.04(16) . . ?
O4 N14 O3 124.4(3) . . ?
O4 N14 C11 118.3(3) . . ?
O3 N14 C11 117.3(3) . . ?
C21 N15 N16 111.0(2) . . ?
C21 N15 B3 129.2(2) . . ?
N16 N15 B3 119.8(2) . . ?
C19 N16 N15 105.8(2) . . ?
C19 N16 Nd1 131.58(19) . . ?
N15 N16 Nd1 122.23(16) . . ?
C24 N17 N18 109.6(2) . . ?
C24 N17 B3 127.0(2) . . ?
N18 N17 B3 123.3(2) . . ?
C22 N18 N17 105.3(2) . . ?
C22 N18 Nd1 128.40(19) . . ?
N17 N18 Nd1 122.57(16) . . ?
C27 N19 N20 110.1(2) . . ?
C27 N19 B3 125.7(3) . . ?
N20 N19 B3 124.2(2) . . ?
C25 N20 N19 105.3(2) . . ?
C25 N20 Nd1 130.4(2) . . ?
N19 N20 Nd1 122.04(16) . . ?
O6 N21 O5 124.4(3) . . ?
O6 N21 C20 118.1(3) . . ?
O5 N21 C20 117.5(3) . . ?
N2 C1 C2 110.0(3) . . ?
N2 C1 H1A 125.0 . . ?
C2 C1 H1A 125.0 . . ?
C3 C2 C1 106.4(3) . . ?
C3 C2 N7 126.5(3) . . ?
C1 C2 N7 126.6(3) . . ?
N1 C3 C2 107.3(3) . . ?
N1 C3 H3A 126.3 . . ?
C2 C3 H3A 126.3 . . ?
N4 C4 C5 111.4(3) . . ?
N4 C4 H4 124.3 . . ?
C5 C4 H4 124.3 . . ?
C6 C5 C4 104.8(3) . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
N3 C6 C5 108.8(3) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 111.5(3) . . ?
N6 C7 H7 124.3 . . ?
C8 C7 H7 124.3 . . ?
C9 C8 C7 104.8(3) . . ?
C9 C8 H8 127.6 . . ?
C7 C8 H8 127.6 . . ?
N5 C9 C8 108.4(3) . . ?
N5 C9 H9 125.8 . . ?
C8 C9 H9 125.8 . . ?
N9 C10 C11 109.2(3) . . ?
N9 C10 H10 125.4 . . ?
C11 C10 H10 125.4 . . ?
C12 C11 C10 106.5(2) . . ?
C12 C11 N14 126.6(3) . . ?
C10 C11 N14 126.8(3) . . ?
N8 C12 C11 106.5(2) . . ?
N8 C12 H12 126.8 . . ?
C11 C12 H12 126.8 . . ?
N11 C13 C14 111.6(3) . . ?
N11 C13 H13 124.2 . . ?
C14 C13 H13 124.2 . . ?
C15 C14 C13 103.9(3) . . ?
C15 C14 H14 128.1 . . ?
C13 C14 H14 128.1 . . ?
N10 C15 C14 109.1(3) . . ?
N10 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
N13 C16 C17 111.1(3) . . ?
N13 C16 H16 124.4 . . ?
C17 C16 H16 124.4 . . ?
C18 C17 C16 104.7(3) . . ?
C18 C17 H17 127.6 . . ?
C16 C17 H17 127.6 . . ?
N12 C18 C17 108.6(3) . . ?
N12 C18 H18 125.7 . . ?
C17 C18 H18 125.7 . . ?
N16 C19 C20 109.6(3) . . ?
N16 C19 H19 125.2 . . ?
C20 C19 H19 125.2 . . ?
C21 C20 C19 106.8(3) . . ?
C21 C20 N21 126.9(3) . . ?
C19 C20 N21 126.2(3) . . ?
N15 C21 C20 106.8(3) . . ?
N15 C21 H21 126.6 . . ?
C20 C21 H21 126.6 . . ?
N18 C22 C23 111.5(3) . . ?
N18 C22 H22 124.2 . . ?
C23 C22 H22 124.2 . . ?
C24 C23 C22 104.4(3) . . ?
C24 C23 H23 127.8 . . ?
C22 C23 H23 127.8 . . ?
N17 C24 C23 109.2(3) . . ?
N17 C24 H24 125.4 . . ?
C23 C24 H24 125.4 . . ?
N20 C25 C26 111.4(3) . . ?
N20 C25 H25 124.3 . . ?
C26 C25 H25 124.3 . . ?
C27 C26 C25 104.4(3) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 108.9(3) . . ?
N19 C27 H27 125.6 . . ?
C26 C27 H27 125.6 . . ?
N3 B1 N5 111.8(2) . . ?
N3 B1 N1 109.8(2) . . ?
N5 B1 N1 106.9(2) . . ?
N3 B1 H1 112.0(15) . . ?
N5 B1 H1 109.3(15) . . ?
N1 B1 H1 106.9(15) . . ?
N8 B2 N12 107.8(2) . . ?
N8 B2 N10 108.1(2) . . ?
N12 B2 N10 112.0(2) . . ?
N8 B2 H2 107.9(16) . . ?
N12 B2 H2 113.0(16) . . ?
N10 B2 H2 107.9(16) . . ?
N17 B3 N19 112.2(3) . . ?
N17 B3 N15 108.6(2) . . ?
N19 B3 N15 108.9(2) . . ?
N17 B3 H3 110.2(15) . . ?
N19 B3 H3 107.8(15) . . ?
N15 B3 H3 109.1(15) . . ?

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.080



_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Cmpd8b
_audit_block_doi                 10.5517/ccdc.csd.cc2drdzk
_database_code_depnum_ccdc_archive 'CCDC 2227039'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-16 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 N21 O6 Tb, 7(C6 H6)'
_chemical_formula_sum            'C69 H69 B3 N21 O6 Tb'
_chemical_formula_weight         1479.80

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'
B B 0.0013 0.0007 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   21.6423(9)
_cell_length_b                   21.6423(9)
_cell_length_c                   25.7873(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10460.3(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1485
_cell_measurement_theta_min      3.757
_cell_measurement_theta_max      48.14

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             4548

_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.141
_exptl_absorpt_coefficient_mu    1.082

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5023
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41716
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.312
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4765
_reflns_number_gt                4292
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          
;
;

_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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+44.8034P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4765
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Tb1 Tb 0.333333 0.666667 0.42126(2) 0.01061(7) Uani 1 3 d S T P . .
O1 O 0.66716(11) 0.74753(12) 0.41079(9) 0.0310(5) Uani 1 1 d . . . . .
O2 O 0.65394(12) 0.64296(13) 0.42722(9) 0.0313(6) Uani 1 1 d . . . . .
N1 N 0.44053(13) 0.57953(12) 0.42663(9) 0.0159(5) Uani 1 1 d . . . . .
N2 N 0.44807(12) 0.64634(12) 0.42101(9) 0.0155(5) Uani 1 1 d . . . . .
N3 N 0.32366(12) 0.51471(12) 0.47242(9) 0.0159(5) Uani 1 1 d . . . . .
N4 N 0.31583(12) 0.57222(12) 0.48475(9) 0.0150(5) Uani 1 1 d . . . . .
N5 N 0.33108(12) 0.51584(12) 0.37333(9) 0.0160(5) Uani 1 1 d . . . . .
N6 N 0.31971(12) 0.57097(12) 0.35977(9) 0.0160(5) Uani 1 1 d . . . . .
N7 N 0.62980(13) 0.68332(15) 0.42026(10) 0.0232(6) Uani 1 1 d . . . . .
C1 C 0.51786(15) 0.69163(16) 0.41891(11) 0.0172(6) Uani 1 1 d . . . . .
H1A H 0.539444 0.741866 0.414974 0.021 Uiso 1 1 calc R U . . .
C2 C 0.55457(15) 0.65430(16) 0.42337(11) 0.0170(6) Uani 1 1 d . . . . .
C3 C 0.50384(15) 0.58298(16) 0.42805(11) 0.0182(6) Uani 1 1 d . . . . .
H3 H 0.512306 0.544141 0.431566 0.022 Uiso 1 1 calc R U . . .
C4 C 0.27935(15) 0.55430(16) 0.52964(11) 0.0184(6) Uani 1 1 d . . . . .
H4 H 0.266200 0.584138 0.547865 0.022 Uiso 1 1 calc R U . . .
C5 C 0.26326(16) 0.48673(16) 0.54606(12) 0.0216(7) Uani 1 1 d . . . . .
H5 H 0.237792 0.462087 0.576304 0.026 Uiso 1 1 calc R U . . .
C6 C 0.29232(15) 0.46345(16) 0.50889(12) 0.0203(6) Uani 1 1 d . . . . .
H6 H 0.290653 0.418744 0.508844 0.024 Uiso 1 1 calc R U . . .
C7 C 0.29429(16) 0.55648(16) 0.31129(11) 0.0210(6) Uani 1 1 d . . . . .
H7 H 0.281152 0.585423 0.291848 0.025 Uiso 1 1 calc R U . . .
C8 C 0.28949(16) 0.49393(16) 0.29295(12) 0.0232(7) Uani 1 1 d . . . . .
H8 H 0.273390 0.472472 0.259877 0.028 Uiso 1 1 calc R U . . .
C9 C 0.31318(16) 0.47016(16) 0.33324(12) 0.0224(7) Uani 1 1 d . . . . .
H9 H 0.316478 0.428005 0.332990 0.027 Uiso 1 1 calc R U . . .
C10 C 0.10149(19) 0.3982(2) 0.23600(15) 0.0411(9) Uani 1 1 d . . . . .
H10 H 0.106381 0.356982 0.234670 0.049 Uiso 1 1 calc R U . . .
C11 C 0.11340(19) 0.4355(2) 0.28192(15) 0.0413(10) Uani 1 1 d . . . . .
H11 H 0.126394 0.419855 0.312290 0.050 Uiso 1 1 calc R U . . .
C12 C 0.1064(2) 0.4955(2) 0.28368(15) 0.0455(11) Uani 1 1 d . . . . .
H12 H 0.114989 0.521320 0.315170 0.055 Uiso 1 1 calc R U . . .
C13 C 0.0872(2) 0.5179(2) 0.23988(15) 0.0454(10) Uani 1 1 d . . . . .
H13 H 0.082264 0.559066 0.241184 0.054 Uiso 1 1 calc R U . . .
C14 C 0.0748(2) 0.4804(2) 0.19361(15) 0.0438(10) Uani 1 1 d . . . . .
H14 H 0.061110 0.495707 0.163379 0.053 Uiso 1 1 calc R U . . .
C15 C 0.0824(2) 0.4213(2) 0.19198(15) 0.0442(10) Uani 1 1 d . . . . .
H15 H 0.074482 0.395948 0.160346 0.053 Uiso 1 1 calc R U . . .
C16 C 0.4587(2) 0.3720(2) 0.42187(16) 0.0431(10) Uani 1 1 d . . . . .
H16 H 0.433874 0.339101 0.448998 0.052 Uiso 1 1 calc R U . . .
C17 C 0.5303(2) 0.4218(2) 0.42744(14) 0.0379(9) Uani 1 1 d . . . . .
H17 H 0.554788 0.423150 0.458379 0.046 Uiso 1 1 calc R U . . .
C18 C 0.56571(19) 0.46899(19) 0.38851(14) 0.0311(8) Uani 1 1 d . . . . .
H18 H 0.614920 0.503000 0.392435 0.037 Uiso 1 1 calc R U . . .
C19 C 0.53110(17) 0.46793(17) 0.34372(13) 0.0265(7) Uani 1 1 d . . . . .
H19 H 0.556338 0.501494 0.317044 0.032 Uiso 1 1 calc R U . . .
C20 C 0.45976(18) 0.41836(18) 0.33713(13) 0.0288(8) Uani 1 1 d . . . . .
H20 H 0.436098 0.417407 0.305853 0.035 Uiso 1 1 calc R U . . .
C21 C 0.42299(19) 0.37017(18) 0.37624(16) 0.0367(9) Uani 1 1 d . . . . .
H21 H 0.373831 0.336075 0.372151 0.044 Uiso 1 1 calc R U . . .
C22 C 0.2785(2) 0.59674(19) 0.16654(15) 0.0386(9) Uani 1 1 d . . . . .
H22 H 0.240801 0.548570 0.166196 0.046 Uiso 1 1 calc R U . . .
C23 C 0.67237(17) 0.40016(16) 0.33339(12) 0.0217(7) Uani 1 1 d . . . . .
H23 H 0.676271 0.445878 0.333544 0.026 Uiso 1 1 calc R U . . .
B1 B 0.36565(19) 0.51357(18) 0.42511(14) 0.0189(7) Uani 1 1 d . . . . .
H1 H 0.3705(17) 0.4639(17) 0.4257(12) 0.028 Uiso 1 1 d . U . . .


_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
Tb1 N4 2.495(2) 3_565 ?
Tb1 N4 2.495(2) 2_665 ?
Tb1 N4 2.496(2) . ?
Tb1 N6 2.506(2) 3_565 ?
Tb1 N6 2.506(2) . ?
Tb1 N6 2.506(2) 2_665 ?
Tb1 N2 2.730(2) 2_665 ?
Tb1 N2 2.730(2) 3_565 ?
Tb1 N2 2.730(2) . ?
O1 N7 1.233(3) . ?
O2 N7 1.235(3) . ?
N1 C3 1.335(4) . ?
N1 N2 1.379(3) . ?
N1 B1 1.534(4) . ?
N2 C1 1.328(4) . ?
N3 C6 1.350(4) . ?
N3 N4 1.375(3) . ?
N3 B1 1.529(4) . ?
N4 C4 1.345(4) . ?
N5 C9 1.346(4) . ?
N5 N6 1.378(3) . ?
N5 B1 1.544(4) . ?
N6 C7 1.338(4) . ?
N7 C2 1.424(4) . ?
C1 C2 1.393(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.388(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.383(5) . ?
C10 C15 1.384(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.369(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.384(6) . ?
C16 C21 1.398(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.362(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.370(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.381(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C22 1.379(4) 15 ?
C22 C22 1.379(4) 14_455 ?
C22 H22 0.9500 . ?
C23 C23 1.389(3) 18_545 ?
C23 C23 1.389(3) 17 ?
C23 H23 0.9500 . ?
B1 H1 1.13(3) . ?

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
N4 Tb1 N4 81.63(8) 3_565 2_665 ?
N4 Tb1 N4 81.63(8) 3_565 . ?
N4 Tb1 N4 81.63(8) 2_665 . ?
N4 Tb1 N6 80.28(7) 3_565 3_565 ?
N4 Tb1 N6 136.79(7) 2_665 3_565 ?
N4 Tb1 N6 133.26(8) . 3_565 ?
N4 Tb1 N6 136.79(8) 3_565 . ?
N4 Tb1 N6 133.26(7) 2_665 . ?
N4 Tb1 N6 80.28(7) . . ?
N6 Tb1 N6 84.23(8) 3_565 . ?
N4 Tb1 N6 133.26(7) 3_565 2_665 ?
N4 Tb1 N6 80.28(8) 2_665 2_665 ?
N4 Tb1 N6 136.79(7) . 2_665 ?
N6 Tb1 N6 84.23(8) 3_565 2_665 ?
N6 Tb1 N6 84.23(8) . 2_665 ?
N4 Tb1 N2 66.52(7) 3_565 2_665 ?
N4 Tb1 N2 69.35(7) 2_665 2_665 ?
N4 Tb1 N2 139.10(7) . 2_665 ?
N6 Tb1 N2 67.46(7) 3_565 2_665 ?
N6 Tb1 N2 140.60(7) . 2_665 ?
N6 Tb1 N2 66.79(7) 2_665 2_665 ?
N4 Tb1 N2 69.35(7) 3_565 3_565 ?
N4 Tb1 N2 139.10(7) 2_665 3_565 ?
N4 Tb1 N2 66.52(7) . 3_565 ?
N6 Tb1 N2 66.79(7) 3_565 3_565 ?
N6 Tb1 N2 67.46(7) . 3_565 ?
N6 Tb1 N2 140.60(7) 2_665 3_565 ?
N2 Tb1 N2 119.999(1) 2_665 3_565 ?
N4 Tb1 N2 139.10(7) 3_565 . ?
N4 Tb1 N2 66.52(7) 2_665 . ?
N4 Tb1 N2 69.35(7) . . ?
N6 Tb1 N2 140.60(7) 3_565 . ?
N6 Tb1 N2 66.79(7) . . ?
N6 Tb1 N2 67.46(7) 2_665 . ?
N2 Tb1 N2 119.999(1) 2_665 . ?
N2 Tb1 N2 120.000(1) 3_565 . ?
C3 N1 N2 111.3(2) . . ?
C3 N1 B1 129.1(2) . . ?
N2 N1 B1 119.3(2) . . ?
C1 N2 N1 105.8(2) . . ?
C1 N2 Tb1 132.18(19) . . ?
N1 N2 Tb1 121.89(16) . . ?
C6 N3 N4 110.1(2) . . ?
C6 N3 B1 127.0(3) . . ?
N4 N3 B1 122.9(2) . . ?
C4 N4 N3 105.0(2) . . ?
C4 N4 Tb1 128.89(19) . . ?
N3 N4 Tb1 123.57(17) . . ?
C9 N5 N6 109.3(2) . . ?
C9 N5 B1 127.4(3) . . ?
N6 N5 B1 123.1(2) . . ?
C7 N6 N5 105.3(2) . . ?
C7 N6 Tb1 130.49(19) . . ?
N5 N6 Tb1 123.83(17) . . ?
O1 N7 O2 123.7(3) . . ?
O1 N7 C2 118.0(3) . . ?
O2 N7 C2 118.3(3) . . ?
N2 C1 C2 109.7(3) . . ?
N2 C1 H1A 125.2 . . ?
C2 C1 H1A 125.2 . . ?
C3 C2 C1 106.9(3) . . ?
C3 C2 N7 126.3(3) . . ?
C1 C2 N7 126.7(3) . . ?
N1 C3 C2 106.3(3) . . ?
N1 C3 H3 126.9 . . ?
C2 C3 H3 126.9 . . ?
N4 C4 C5 111.6(3) . . ?
N4 C4 H4 124.2 . . ?
C5 C4 H4 124.2 . . ?
C6 C5 C4 104.7(3) . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
N3 C6 C5 108.6(3) . . ?
N3 C6 H6 125.7 . . ?
C5 C6 H6 125.7 . . ?
N6 C7 C8 111.6(3) . . ?
N6 C7 H7 124.2 . . ?
C8 C7 H7 124.2 . . ?
C9 C8 C7 104.4(3) . . ?
C9 C8 H8 127.8 . . ?
C7 C8 H8 127.8 . . ?
N5 C9 C8 109.3(3) . . ?
N5 C9 H9 125.3 . . ?
C8 C9 H9 125.3 . . ?
C11 C10 C15 119.5(4) . . ?
C11 C10 H10 120.2 . . ?
C15 C10 H10 120.2 . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 119.5(4) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C10 120.6(4) . . ?
C14 C15 H15 119.7 . . ?
C10 C15 H15 119.7 . . ?
C17 C16 C21 119.8(4) . . ?
C17 C16 H16 120.1 . . ?
C21 C16 H16 120.1 . . ?
C18 C17 C16 119.9(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C21 119.7(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C20 C21 C16 119.5(3) . . ?
C20 C21 H21 120.3 . . ?
C16 C21 H21 120.3 . . ?
C22 C22 C22 119.994(8) 15 14_455 ?
C22 C22 H22 120.0 15 . ?
C22 C22 H22 120.0 14_455 . ?
C23 C23 C23 119.991(3) 18_545 17 ?
C23 C23 H23 120.0 18_545 . ?
C23 C23 H23 120.0 17 . ?
N3 B1 N1 108.9(2) . . ?
N3 B1 N5 112.9(3) . . ?
N1 B1 N5 107.2(2) . . ?
N3 B1 H1 110.1(16) . . ?
N1 B1 H1 109.1(16) . . ?
N5 B1 H1 108.5(16) . . ?

_refine_diff_density_max         0.641
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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_Cmpd6
_audit_block_doi                 10.5517/ccdc.csd.cc2dr86n
_database_code_depnum_ccdc_archive 'CCDC 2226891'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Eu N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 Eu N21 O6'
_chemical_formula_weight         926.08

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.313(16)
_cell_length_b                   13.724(10)
_cell_length_c                   29.722(15)
_cell_angle_alpha                90
_cell_angle_beta                 115.893(13)
_cell_angle_gamma                90
_cell_volume                     8922(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    123
_cell_measurement_theta_min      3.657
_cell_measurement_theta_max      27.95

_exptl_crystal_description       diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             3696

_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.094
_exptl_absorpt_coefficient_mu    1.466

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21648
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.037
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             9062
_reflns_number_gt                6424
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9062
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Eu1 Eu 0.68812(2) 0.33977(2) 0.62435(2) 0.01479(7) Uani 1 1 d . . . . .
O1 O 0.68006(16) 0.8076(2) 0.65766(14) 0.0345(10) Uani 1 1 d . . . . .
O2 O 0.76738(15) 0.8493(2) 0.65826(13) 0.0318(9) Uani 1 1 d . . . . .
O3 O 0.91591(16) 0.1424(2) 0.59752(16) 0.0463(11) Uani 1 1 d . . . . .
O4 O 0.88464(16) -0.0088(2) 0.58612(14) 0.0400(10) Uani 1 1 d . . . . .
O5 O 0.45187(16) 0.0693(2) 0.58932(15) 0.0417(10) Uani 1 1 d . . . . .
O6 O 0.39752(15) 0.1775(2) 0.60586(14) 0.0367(9) Uani 1 1 d . . . . .
N1 N 0.78668(16) 0.5543(2) 0.64676(14) 0.0170(9) Uani 1 1 d . . . . .
N2 N 0.73065(16) 0.5274(2) 0.64278(14) 0.0175(9) Uani 1 1 d . . . . .
N3 N 0.80124(17) 0.4283(2) 0.59331(14) 0.0172(9) Uani 1 1 d . . . . .
N4 N 0.74359(16) 0.3876(2) 0.57232(14) 0.0175(9) Uani 1 1 d . . . . .
N5 N 0.84237(17) 0.4012(2) 0.68751(15) 0.0184(9) Uani 1 1 d . . . . .
N6 N 0.79681(16) 0.3490(2) 0.69206(14) 0.0187(9) Uani 1 1 d . . . . .
N7 N 0.7291(2) 0.7877(2) 0.65603(15) 0.0253(10) Uani 1 1 d . . . . .
N8 N 0.74274(17) 0.0966(2) 0.61084(14) 0.0177(9) Uani 1 1 d . . . . .
N9 N 0.76168(17) 0.1928(2) 0.61878(15) 0.0198(9) Uani 1 1 d . . . . .
N10 N 0.63212(16) 0.1234(2) 0.55813(14) 0.0168(9) Uani 1 1 d . . . . .
N11 N 0.63242(17) 0.2230(2) 0.55274(15) 0.0178(9) Uani 1 1 d . . . . .
N12 N 0.67247(16) 0.0985(2) 0.65229(14) 0.0173(9) Uani 1 1 d . . . . .
N13 N 0.68401(16) 0.1900(2) 0.67301(14) 0.0169(9) Uani 1 1 d . . . . .
N14 N 0.88030(19) 0.0771(3) 0.59640(16) 0.0296(11) Uani 1 1 d . . . . .
N15 N 0.53529(17) 0.3640(2) 0.61784(14) 0.0190(9) Uani 1 1 d . . . . .
N16 N 0.57299(16) 0.2956(2) 0.61190(14) 0.0185(9) Uani 1 1 d . . . . .
N17 N 0.61274(16) 0.4794(2) 0.67724(14) 0.0183(9) Uani 1 1 d . . . . .
N18 N 0.66450(16) 0.4240(2) 0.68943(14) 0.0151(8) Uani 1 1 d . . . . .
N19 N 0.56897(16) 0.5063(2) 0.58335(15) 0.0199(9) Uani 1 1 d . . . . .
N20 N 0.60930(16) 0.4614(2) 0.56909(14) 0.0177(9) Uani 1 1 d . . . . .
N21 N 0.44294(18) 0.1527(3) 0.60008(15) 0.0260(9) Uani 1 1 d . . . . .
C1 C 0.7026(2) 0.6086(3) 0.64540(16) 0.0164(10) Uani 1 1 d . . . . .
H1A H 0.662728 0.612474 0.643769 0.020 Uiso 1 1 calc R U . . .
C2 C 0.7415(2) 0.6878(3) 0.65100(17) 0.0184(11) Uani 1 1 d . . . . .
C3 C 0.7948(2) 0.6505(3) 0.65186(16) 0.0204(11) Uani 1 1 d . . . . .
H3A H 0.829933 0.686027 0.655361 0.024 Uiso 1 1 calc R U . . .
C4 C 0.7337(2) 0.3590(3) 0.52662(18) 0.0190(11) Uani 1 1 d . . . . .
H4 H 0.697153 0.329026 0.503268 0.023 Uiso 1 1 calc R U . . .
C5 C 0.8250(2) 0.4239(3) 0.55942(18) 0.0196(11) Uani 1 1 d . . . . .
H5 H 0.863696 0.448418 0.564240 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7840(2) 0.3788(3) 0.51774(18) 0.0214(11) Uani 1 1 d . . . . .
H6 H 0.788713 0.363861 0.488417 0.026 Uiso 1 1 calc R U . . .
C7 C 0.8246(2) 0.2963(3) 0.73318(19) 0.0237(12) Uani 1 1 d . . . . .
H7 H 0.804083 0.251763 0.745121 0.028 Uiso 1 1 calc R U . . .
C8 C 0.8867(2) 0.3136(3) 0.7567(2) 0.0320(13) Uani 1 1 d . . . . .
H8 H 0.916251 0.286119 0.786955 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8957(2) 0.3802(3) 0.72597(19) 0.0273(12) Uani 1 1 d . . . . .
H9 H 0.934093 0.407126 0.731322 0.033 Uiso 1 1 calc R U . . .
C10 C 0.8146(2) 0.1959(3) 0.61643(18) 0.0208(11) Uani 1 1 d . . . . .
H10 H 0.838524 0.252846 0.620393 0.025 Uiso 1 1 calc R U . . .
C11 C 0.8301(2) 0.1024(3) 0.60721(18) 0.0196(11) Uani 1 1 d . . . . .
C12 C 0.7839(2) 0.0418(3) 0.60401(17) 0.0187(11) Uani 1 1 d . . . . .
H12 H 0.781560 -0.026443 0.598065 0.022 Uiso 1 1 calc R U . . .
C13 C 0.5879(2) 0.2418(3) 0.50779(18) 0.0223(11) Uani 1 1 d . . . . .
H13 H 0.576928 0.305245 0.493906 0.027 Uiso 1 1 calc R U . . .
C14 C 0.5593(2) 0.1563(3) 0.48369(19) 0.0285(12) Uani 1 1 d . . . . .
H14 H 0.526454 0.149931 0.451246 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5886(2) 0.0841(3) 0.51668(19) 0.0238(12) Uani 1 1 d . . . . .
H15 H 0.579596 0.016590 0.511241 0.029 Uiso 1 1 calc R U . . .
C16 C 0.6729(2) 0.1854(3) 0.71293(18) 0.0199(11) Uani 1 1 d . . . . .
H16 H 0.677333 0.238789 0.734632 0.024 Uiso 1 1 calc R U . . .
C17 C 0.6538(2) 0.0926(3) 0.71896(18) 0.0225(11) Uani 1 1 d . . . . .
H17 H 0.642657 0.070888 0.744216 0.027 Uiso 1 1 calc R U . . .
C18 C 0.6547(2) 0.0396(3) 0.67997(18) 0.0218(11) Uani 1 1 d . . . . .
H18 H 0.644495 -0.027458 0.673567 0.026 Uiso 1 1 calc R U . . .
C19 C 0.5430(2) 0.2118(3) 0.60438(17) 0.0183(11) Uani 1 1 d . . . . .
H19 H 0.557530 0.150827 0.598855 0.022 Uiso 1 1 calc R U . . .
C20 C 0.4875(2) 0.2262(3) 0.60578(18) 0.0197(11) Uani 1 1 d . . . . .
C21 C 0.4843(2) 0.3238(3) 0.61461(17) 0.0204(11) Uani 1 1 d . . . . .
H21 H 0.451648 0.356219 0.617786 0.025 Uiso 1 1 calc R U . . .
C22 C 0.7039(2) 0.4515(3) 0.73608(18) 0.0199(11) Uani 1 1 d . . . . .
H22 H 0.743780 0.425555 0.754201 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6781(2) 0.5228(3) 0.75396(19) 0.0249(12) Uani 1 1 d . . . . .
H23 H 0.695902 0.554075 0.785654 0.030 Uiso 1 1 calc R U . . .
C24 C 0.6212(2) 0.5381(3) 0.71572(19) 0.0240(12) Uani 1 1 d . . . . .
H24 H 0.592127 0.583575 0.716396 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6070(2) 0.5136(3) 0.53034(18) 0.0223(11) Uani 1 1 d . . . . .
H25 H 0.630445 0.499881 0.512539 0.027 Uiso 1 1 calc R U . . .
C26 C 0.5661(2) 0.5903(3) 0.5195(2) 0.0322(13) Uani 1 1 d . . . . .
H26 H 0.556276 0.637648 0.493809 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5430(2) 0.5828(3) 0.55385(19) 0.0252(12) Uani 1 1 d . . . . .
H27 H 0.513495 0.624885 0.556339 0.030 Uiso 1 1 calc R U . . .
B1 B 0.8308(2) 0.4757(4) 0.6452(2) 0.0181(12) Uani 1 1 d . . . . .
H1 H 0.8733(19) 0.507(3) 0.6545(16) 0.027 Uiso 1 1 d . U . . .
B2 B 0.6786(3) 0.0690(4) 0.6051(2) 0.0199(13) Uani 1 1 d . . . . .
H2 H 0.6749(19) -0.005(3) 0.5972(17) 0.030 Uiso 1 1 d . U . . .
B3 B 0.5562(2) 0.4716(4) 0.6271(2) 0.0200(13) Uani 1 1 d . . . . .
H3 H 0.5181(19) 0.512(3) 0.6277(16) 0.030 Uiso 1 1 d . U . . .


_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
Eu1 N18 2.525(4) . ?
Eu1 N20 2.531(4) . ?
Eu1 N6 2.531(4) . ?
Eu1 N11 2.533(4) . ?
Eu1 N13 2.541(4) . ?
Eu1 N4 2.542(4) . ?
Eu1 N16 2.727(4) . ?
Eu1 N2 2.740(4) . ?
Eu1 N9 2.749(4) . ?
O1 N7 1.243(5) . ?
O2 N7 1.238(4) . ?
O3 N14 1.236(5) . ?
O4 N14 1.234(4) . ?
O5 N21 1.233(4) . ?
O6 N21 1.237(4) . ?
N1 C3 1.333(5) . ?
N1 N2 1.366(5) . ?
N1 B1 1.536(6) . ?
N2 C1 1.327(5) . ?
N3 C5 1.363(5) . ?
N3 N4 1.379(5) . ?
N3 B1 1.533(6) . ?
N4 C4 1.331(5) . ?
N5 C9 1.333(6) . ?
N5 N6 1.375(4) . ?
N5 B1 1.548(6) . ?
N6 C7 1.323(6) . ?
N7 C2 1.426(5) . ?
N8 C12 1.337(5) . ?
N8 N9 1.384(4) . ?
N8 B2 1.541(6) . ?
N9 C10 1.320(5) . ?
N10 C15 1.338(6) . ?
N10 N11 1.376(4) . ?
N10 B2 1.551(6) . ?
N11 C13 1.327(6) . ?
N12 C18 1.353(5) . ?
N12 N13 1.372(4) . ?
N12 B2 1.529(6) . ?
N13 C16 1.329(5) . ?
N14 C11 1.434(5) . ?
N15 C21 1.322(5) . ?
N15 N16 1.376(4) . ?
N15 B3 1.547(6) . ?
N16 C19 1.328(5) . ?
N17 C24 1.339(5) . ?
N17 N18 1.377(4) . ?
N17 B3 1.527(6) . ?
N18 C22 1.350(6) . ?
N19 C27 1.336(5) . ?
N19 N20 1.373(5) . ?
N19 B3 1.537(6) . ?
N20 C25 1.337(5) . ?
N21 C20 1.435(5) . ?
C1 C2 1.403(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.382(6) . ?
C3 H3A 0.9500 . ?
C4 C6 1.385(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.354(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.381(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(6) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.397(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.356(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.394(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.382(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.386(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.367(7) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.04(4) . ?
B2 H2 1.04(4) . ?
B3 H3 1.09(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
N18 Eu1 N20 80.46(12) . . ?
N18 Eu1 N6 82.85(12) . . ?
N20 Eu1 N6 135.62(11) . . ?
N18 Eu1 N11 135.74(11) . . ?
N20 Eu1 N11 84.06(12) . . ?
N6 Eu1 N11 133.59(11) . . ?
N18 Eu1 N13 81.69(11) . . ?
N20 Eu1 N13 134.11(12) . . ?
N6 Eu1 N13 82.81(11) . . ?
N11 Eu1 N13 80.02(12) . . ?
N18 Eu1 N4 134.93(11) . . ?
N20 Eu1 N4 83.54(12) . . ?
N6 Eu1 N4 79.85(13) . . ?
N11 Eu1 N4 83.31(12) . . ?
N13 Eu1 N4 135.94(11) . . ?
N18 Eu1 N16 69.03(11) . . ?
N20 Eu1 N16 67.47(11) . . ?
N6 Eu1 N16 140.58(12) . . ?
N11 Eu1 N16 66.73(11) . . ?
N13 Eu1 N16 66.68(11) . . ?
N4 Eu1 N16 139.53(12) . . ?
N18 Eu1 N2 66.98(10) . . ?
N20 Eu1 N2 67.83(12) . . ?
N6 Eu1 N2 67.79(11) . . ?
N11 Eu1 N2 141.21(11) . . ?
N13 Eu1 N2 138.76(12) . . ?
N4 Eu1 N2 67.95(11) . . ?
N16 Eu1 N2 120.75(10) . . ?
N18 Eu1 N9 138.90(12) . . ?
N20 Eu1 N9 140.64(12) . . ?
N6 Eu1 N9 66.66(11) . . ?
N11 Eu1 N9 66.92(12) . . ?
N13 Eu1 N9 68.20(11) . . ?
N4 Eu1 N9 67.74(11) . . ?
N16 Eu1 N9 119.02(11) . . ?
N2 Eu1 N9 120.22(11) . . ?
C3 N1 N2 111.7(3) . . ?
C3 N1 B1 128.9(4) . . ?
N2 N1 B1 119.4(3) . . ?
C1 N2 N1 106.7(3) . . ?
C1 N2 Eu1 130.0(3) . . ?
N1 N2 Eu1 123.1(2) . . ?
C5 N3 N4 108.8(4) . . ?
C5 N3 B1 126.7(4) . . ?
N4 N3 B1 124.3(3) . . ?
C4 N4 N3 106.0(3) . . ?
C4 N4 Eu1 129.6(3) . . ?
N3 N4 Eu1 122.3(3) . . ?
C9 N5 N6 109.1(4) . . ?
C9 N5 B1 127.1(4) . . ?
N6 N5 B1 123.7(4) . . ?
C7 N6 N5 105.5(4) . . ?
C7 N6 Eu1 129.9(3) . . ?
N5 N6 Eu1 123.7(3) . . ?
O2 N7 O1 124.0(4) . . ?
O2 N7 C2 118.2(4) . . ?
O1 N7 C2 117.8(4) . . ?
C12 N8 N9 110.3(3) . . ?
C12 N8 B2 129.4(3) . . ?
N9 N8 B2 119.9(3) . . ?
C10 N9 N8 106.4(3) . . ?
C10 N9 Eu1 130.9(3) . . ?
N8 N9 Eu1 122.3(3) . . ?
C15 N10 N11 109.6(4) . . ?
C15 N10 B2 127.3(4) . . ?
N11 N10 B2 123.0(4) . . ?
C13 N11 N10 105.5(4) . . ?
C13 N11 Eu1 128.6(3) . . ?
N10 N11 Eu1 124.0(3) . . ?
C18 N12 N13 109.3(4) . . ?
C18 N12 B2 125.8(4) . . ?
N13 N12 B2 124.9(3) . . ?
C16 N13 N12 106.1(3) . . ?
C16 N13 Eu1 128.3(3) . . ?
N12 N13 Eu1 122.4(3) . . ?
O4 N14 O3 124.3(4) . . ?
O4 N14 C11 117.4(4) . . ?
O3 N14 C11 118.3(4) . . ?
C21 N15 N16 111.2(3) . . ?
C21 N15 B3 129.6(4) . . ?
N16 N15 B3 119.2(3) . . ?
C19 N16 N15 105.4(3) . . ?
C19 N16 Eu1 132.2(3) . . ?
N15 N16 Eu1 122.2(2) . . ?
C24 N17 N18 109.0(4) . . ?
C24 N17 B3 127.9(4) . . ?
N18 N17 B3 123.2(3) . . ?
C22 N18 N17 105.8(3) . . ?
C22 N18 Eu1 128.2(3) . . ?
N17 N18 Eu1 122.6(3) . . ?
C27 N19 N20 110.2(4) . . ?
C27 N19 B3 125.9(4) . . ?
N20 N19 B3 123.8(3) . . ?
C25 N20 N19 105.0(3) . . ?
C25 N20 Eu1 130.3(3) . . ?
N19 N20 Eu1 122.4(3) . . ?
O5 N21 O6 124.1(4) . . ?
O5 N21 C20 118.3(4) . . ?
O6 N21 C20 117.6(4) . . ?
N2 C1 C2 108.7(4) . . ?
N2 C1 H1A 125.7 . . ?
C2 C1 H1A 125.7 . . ?
C3 C2 C1 107.0(4) . . ?
C3 C2 N7 126.5(4) . . ?
C1 C2 N7 126.4(4) . . ?
N1 C3 C2 106.0(4) . . ?
N1 C3 H3A 127.0 . . ?
C2 C3 H3A 127.0 . . ?
N4 C4 C6 110.8(4) . . ?
N4 C4 H4 124.6 . . ?
C6 C4 H4 124.6 . . ?
C6 C5 N3 108.4(4) . . ?
C6 C5 H5 125.8 . . ?
N3 C5 H5 125.8 . . ?
C5 C6 C4 105.9(4) . . ?
C5 C6 H6 127.1 . . ?
C4 C6 H6 127.1 . . ?
N6 C7 C8 112.2(4) . . ?
N6 C7 H7 123.9 . . ?
C8 C7 H7 123.9 . . ?
C9 C8 C7 103.5(5) . . ?
C9 C8 H8 128.2 . . ?
C7 C8 H8 128.2 . . ?
N5 C9 C8 109.6(4) . . ?
N5 C9 H9 125.2 . . ?
C8 C9 H9 125.2 . . ?
N9 C10 C11 109.4(4) . . ?
N9 C10 H10 125.3 . . ?
C11 C10 H10 125.3 . . ?
C12 C11 C10 106.8(4) . . ?
C12 C11 N14 126.2(4) . . ?
C10 C11 N14 126.5(4) . . ?
N8 C12 C11 107.1(4) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N11 C13 C14 111.0(4) . . ?
N11 C13 H13 124.5 . . ?
C14 C13 H13 124.5 . . ?
C15 C14 C13 104.9(4) . . ?
C15 C14 H14 127.5 . . ?
C13 C14 H14 127.5 . . ?
N10 C15 C14 109.0(4) . . ?
N10 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
N13 C16 C17 111.5(4) . . ?
N13 C16 H16 124.2 . . ?
C17 C16 H16 124.2 . . ?
C18 C17 C16 104.3(4) . . ?
C18 C17 H17 127.9 . . ?
C16 C17 H17 127.9 . . ?
N12 C18 C17 108.8(4) . . ?
N12 C18 H18 125.6 . . ?
C17 C18 H18 125.6 . . ?
N16 C19 C20 110.0(4) . . ?
N16 C19 H19 125.0 . . ?
C20 C19 H19 125.0 . . ?
C21 C20 C19 106.5(4) . . ?
C21 C20 N21 127.2(4) . . ?
C19 C20 N21 126.3(4) . . ?
N15 C21 C20 106.9(4) . . ?
N15 C21 H21 126.5 . . ?
C20 C21 H21 126.5 . . ?
N18 C22 C23 110.8(4) . . ?
N18 C22 H22 124.6 . . ?
C23 C22 H22 124.6 . . ?
C24 C23 C22 104.6(4) . . ?
C24 C23 H23 127.7 . . ?
C22 C23 H23 127.7 . . ?
N17 C24 C23 109.9(4) . . ?
N17 C24 H24 125.1 . . ?
C23 C24 H24 125.1 . . ?
N20 C25 C26 111.3(4) . . ?
N20 C25 H25 124.4 . . ?
C26 C25 H25 124.4 . . ?
C27 C26 C25 104.8(4) . . ?
C27 C26 H26 127.6 . . ?
C25 C26 H26 127.6 . . ?
N19 C27 C26 108.7(4) . . ?
N19 C27 H27 125.7 . . ?
C26 C27 H27 125.7 . . ?
N3 B1 N1 107.6(4) . . ?
N3 B1 N5 112.1(4) . . ?
N1 B1 N5 108.7(4) . . ?
N3 B1 H1 115(2) . . ?
N1 B1 H1 110(2) . . ?
N5 B1 H1 104(2) . . ?
N12 B2 N8 109.4(4) . . ?
N12 B2 N10 111.9(4) . . ?
N8 B2 N10 106.6(4) . . ?
N12 B2 H2 116(2) . . ?
N8 B2 H2 104(2) . . ?
N10 B2 H2 108(3) . . ?
N17 B3 N19 112.1(4) . . ?
N17 B3 N15 109.1(4) . . ?
N19 B3 N15 108.5(4) . . ?
N17 B3 H3 111(2) . . ?
N19 B3 H3 110(2) . . ?
N15 B3 H3 106(2) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.115



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Cmpd7
_audit_block_doi                 10.5517/ccdc.csd.cc2dr87p
_database_code_depnum_ccdc_archive 'CCDC 2226892'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Gd N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 Gd N21 O6'
_chemical_formula_weight         931.37

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.296(6)
_cell_length_b                   13.742(2)
_cell_length_c                   29.768(4)
_cell_angle_alpha                90
_cell_angle_beta                 116.414(8)
_cell_angle_gamma                90
_cell_volume                     8901(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    471
_cell_measurement_theta_min      3.480
_cell_measurement_theta_max      40.97

_exptl_crystal_description       diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             3704

_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.149
_exptl_absorpt_coefficient_mu    1.551

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50295
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.033
_diffrn_reflns_theta_max         26.325
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9047
_reflns_number_gt                7609
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0290P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9047
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0629
_refine_ls_wR_factor_gt          0.0601
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Gd1 Gd 0.31089(2) 0.33890(2) 0.37538(2) 0.01227(5) Uani 1 1 d . . . . .
O1 O 0.23204(10) 0.84802(12) 0.34264(8) 0.0295(5) Uani 1 1 d . . . . .
O2 O 0.31892(10) 0.80634(13) 0.34273(8) 0.0320(5) Uani 1 1 d . . . . .
O3 O 0.60163(10) 0.17608(14) 0.39375(9) 0.0353(5) Uani 1 1 d . . . . .
O4 O 0.54794(10) 0.06836(13) 0.41131(9) 0.0395(6) Uani 1 1 d . . . . .
O5 O 0.11386(10) -0.00717(14) 0.41376(8) 0.0355(5) Uani 1 1 d . . . . .
O6 O 0.08206(10) 0.14343(14) 0.40074(9) 0.0405(6) Uani 1 1 d . . . . .
N1 N 0.21187(10) 0.55279(14) 0.35209(8) 0.0156(5) Uani 1 1 d . . . . .
N2 N 0.26861(10) 0.52614(14) 0.35633(8) 0.0169(5) Uani 1 1 d . . . . .
N3 N 0.15601(10) 0.39998(14) 0.31113(8) 0.0161(5) Uani 1 1 d . . . . .
N4 N 0.20171(10) 0.34762(13) 0.30726(8) 0.0156(5) Uani 1 1 d . . . . .
N5 N 0.19768(10) 0.42719(14) 0.40593(8) 0.0161(5) Uani 1 1 d . . . . .
N6 N 0.25543(10) 0.38726(14) 0.42652(7) 0.0148(4) Uani 1 1 d . . . . .
N7 N 0.27027(12) 0.78661(15) 0.34443(8) 0.0226(5) Uani 1 1 d . . . . .
N8 N 0.46426(10) 0.36305(14) 0.38269(8) 0.0166(5) Uani 1 1 d . . . . .
N9 N 0.42671(10) 0.29487(14) 0.38902(8) 0.0165(5) Uani 1 1 d . . . . .
N10 N 0.43029(10) 0.50481(14) 0.41674(8) 0.0176(5) Uani 1 1 d . . . . .
N11 N 0.38949(10) 0.46122(14) 0.43070(8) 0.0169(5) Uani 1 1 d . . . . .
N12 N 0.38580(10) 0.47690(14) 0.32255(8) 0.0166(5) Uani 1 1 d . . . . .
N13 N 0.33375(10) 0.42181(14) 0.31029(8) 0.0156(5) Uani 1 1 d . . . . .
N14 N 0.55666(11) 0.15182(16) 0.40029(9) 0.0260(5) Uani 1 1 d . . . . .
N15 N 0.25592(10) 0.09684(14) 0.38885(7) 0.0151(5) Uani 1 1 d . . . . .
N16 N 0.23729(10) 0.19312(14) 0.38083(8) 0.0173(5) Uani 1 1 d . . . . .
N17 N 0.32708(10) 0.09829(14) 0.34825(8) 0.0155(5) Uani 1 1 d . . . . .
N18 N 0.31540(10) 0.18953(14) 0.32763(8) 0.0156(5) Uani 1 1 d . . . . .
N19 N 0.36754(10) 0.12454(14) 0.44257(8) 0.0166(5) Uani 1 1 d . . . . .
N20 N 0.36734(9) 0.22420(14) 0.44762(7) 0.0150(4) Uani 1 1 d . . . . .
N21 N 0.11795(11) 0.07851(16) 0.40240(9) 0.0258(5) Uani 1 1 d . . . . .
C1 C 0.29609(13) 0.60809(17) 0.35362(9) 0.0178(6) Uani 1 1 d . . . . .
H1A H 0.335771 0.612469 0.354869 0.021 Uiso 1 1 calc R U . . .
C2 C 0.25726(13) 0.68690(17) 0.34865(9) 0.0180(6) Uani 1 1 d . . . . .
C3 C 0.20433(13) 0.64990(16) 0.34793(9) 0.0177(6) Uani 1 1 d . . . . .
H3A H 0.169462 0.685667 0.345081 0.021 Uiso 1 1 calc R U . . .
C4 C 0.17367(13) 0.29408(18) 0.26549(9) 0.0202(6) Uani 1 1 d . . . . .
H4 H 0.194165 0.249526 0.253673 0.024 Uiso 1 1 calc R U . . .
C5 C 0.11104(13) 0.31194(19) 0.24175(11) 0.0268(7) Uani 1 1 d . . . . .
H5 H 0.081212 0.284408 0.211388 0.032 Uiso 1 1 calc R U . . .
C6 C 0.10189(13) 0.3790(2) 0.27235(10) 0.0260(6) Uani 1 1 d . . . . .
H6 H 0.063362 0.405876 0.266785 0.031 Uiso 1 1 calc R U . . .
C7 C 0.26568(13) 0.35806(17) 0.47242(9) 0.0178(6) Uani 1 1 d . . . . .
H7 H 0.302386 0.327269 0.495561 0.021 Uiso 1 1 calc R U . . .
C8 C 0.21591(13) 0.37840(18) 0.48201(10) 0.0198(6) Uani 1 1 d . . . . .
H8 H 0.211841 0.364918 0.511689 0.024 Uiso 1 1 calc R U . . .
C9 C 0.17379(13) 0.42251(17) 0.43883(10) 0.0191(6) Uani 1 1 d . . . . .
H9 H 0.134425 0.445743 0.433236 0.023 Uiso 1 1 calc R U . . .
C10 C 0.45668(12) 0.21065(18) 0.39694(9) 0.0177(6) Uani 1 1 d . . . . .
H10 H 0.442298 0.150090 0.402953 0.021 Uiso 1 1 calc R U . . .
C11 C 0.51214(12) 0.22491(17) 0.39507(9) 0.0184(6) Uani 1 1 d . . . . .
C12 C 0.51570(12) 0.32234(18) 0.38599(10) 0.0194(6) Uani 1 1 d . . . . .
H12 H 0.548404 0.354282 0.382713 0.023 Uiso 1 1 calc R U . . .
C13 C 0.39137(13) 0.51418(18) 0.46923(9) 0.0225(6) Uani 1 1 d . . . . .
H13 H 0.367659 0.500838 0.486700 0.027 Uiso 1 1 calc R U . . .
C14 C 0.43267(13) 0.5914(2) 0.48031(10) 0.0283(7) Uani 1 1 d . . . . .
H14 H 0.442379 0.639344 0.505695 0.034 Uiso 1 1 calc R U . . .
C15 C 0.45613(13) 0.58235(18) 0.44617(10) 0.0249(6) Uani 1 1 d . . . . .
H15 H 0.485829 0.624169 0.443753 0.030 Uiso 1 1 calc R U . . .
C16 C 0.29469(12) 0.44804(18) 0.26349(9) 0.0190(6) Uani 1 1 d . . . . .
H16 H 0.254777 0.421308 0.245142 0.023 Uiso 1 1 calc R U . . .
C17 C 0.32006(13) 0.51955(18) 0.24513(10) 0.0235(6) Uani 1 1 d . . . . .
H17 H 0.301789 0.550106 0.213176 0.028 Uiso 1 1 calc R U . . .
C18 C 0.37724(13) 0.53580(18) 0.28354(10) 0.0224(6) Uani 1 1 d . . . . .
H18 H 0.406346 0.581270 0.282909 0.027 Uiso 1 1 calc R U . . .
C19 C 0.18381(12) 0.19624(18) 0.38271(9) 0.0188(6) Uani 1 1 d . . . . .
H19 H 0.159715 0.253098 0.378359 0.023 Uiso 1 1 calc R U . . .
C20 C 0.16833(12) 0.10294(17) 0.39210(10) 0.0184(6) Uani 1 1 d . . . . .
C21 C 0.21515(12) 0.04203(18) 0.39576(9) 0.0195(6) Uani 1 1 d . . . . .
H21 H 0.217837 -0.026015 0.402025 0.023 Uiso 1 1 calc R U . . .
C22 C 0.32703(12) 0.18468(18) 0.28796(9) 0.0187(6) Uani 1 1 d . . . . .
H22 H 0.322806 0.237912 0.266303 0.022 Uiso 1 1 calc R U . . .
C23 C 0.34614(13) 0.09200(18) 0.28216(10) 0.0221(6) Uani 1 1 d . . . . .
H23 H 0.357036 0.069927 0.256943 0.027 Uiso 1 1 calc R U . . .
C24 C 0.34559(12) 0.03993(18) 0.32127(9) 0.0187(6) Uani 1 1 d . . . . .
H24 H 0.356522 -0.026690 0.328207 0.022 Uiso 1 1 calc R U . . .
C25 C 0.41197(12) 0.24336(19) 0.49313(10) 0.0207(6) Uani 1 1 d . . . . .
H25 H 0.422615 0.306957 0.506791 0.025 Uiso 1 1 calc R U . . .
C26 C 0.44106(13) 0.15909(19) 0.51820(10) 0.0260(6) Uani 1 1 d . . . . .
H26 H 0.474011 0.153617 0.550943 0.031 Uiso 1 1 calc R U . . .
C27 C 0.41161(12) 0.08576(19) 0.48514(10) 0.0224(6) Uani 1 1 d . . . . .
H27 H 0.420643 0.018374 0.491123 0.027 Uiso 1 1 calc R U . . .
B1 B 0.16749(15) 0.4741(2) 0.35356(11) 0.0178(6) Uani 1 1 d . . . . .
H1 H 0.1224(12) 0.5069(18) 0.3447(10) 0.027 Uiso 1 1 d . U . . .
B2 B 0.44363(14) 0.4702(2) 0.37339(11) 0.0185(6) Uani 1 1 d . . . . .
H2 H 0.4802(12) 0.5203(18) 0.3724(10) 0.028 Uiso 1 1 d . U . . .
B3 B 0.32093(14) 0.0695(2) 0.39569(11) 0.0173(6) Uani 1 1 d D . . . .
H3 H 0.3281(12) -0.0093(12) 0.4040(10) 0.026 Uiso 1 1 d D U . . .


_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
Gd1 N13 2.514(2) . ?
Gd1 N20 2.523(2) . ?
Gd1 N4 2.525(2) . ?
Gd1 N18 2.527(2) . ?
Gd1 N11 2.527(2) . ?
Gd1 N6 2.530(2) . ?
Gd1 N9 2.726(2) . ?
Gd1 N2 2.735(2) . ?
Gd1 N16 2.738(2) . ?
O1 N7 1.238(3) . ?
O2 N7 1.236(3) . ?
O3 N14 1.238(3) . ?
O4 N14 1.237(3) . ?
O5 N21 1.241(3) . ?
O6 N21 1.233(3) . ?
N1 C3 1.345(3) . ?
N1 N2 1.377(3) . ?
N1 B1 1.542(4) . ?
N2 C1 1.330(3) . ?
N3 C6 1.340(3) . ?
N3 N4 1.370(3) . ?
N3 B1 1.548(3) . ?
N4 C4 1.341(3) . ?
N5 C9 1.344(3) . ?
N5 N6 1.371(3) . ?
N5 B1 1.538(3) . ?
N6 C7 1.337(3) . ?
N7 C2 1.424(3) . ?
N8 C12 1.332(3) . ?
N8 N9 1.378(3) . ?
N8 B2 1.540(3) . ?
N9 C10 1.331(3) . ?
N10 C15 1.344(3) . ?
N10 N11 1.371(3) . ?
N10 B2 1.539(4) . ?
N11 C13 1.342(3) . ?
N12 C18 1.354(3) . ?
N12 N13 1.377(3) . ?
N12 B2 1.543(4) . ?
N13 C16 1.340(3) . ?
N14 C11 1.433(3) . ?
N15 C21 1.331(3) . ?
N15 N16 1.384(3) . ?
N15 B3 1.546(4) . ?
N16 C19 1.326(3) . ?
N17 C24 1.346(3) . ?
N17 N18 1.369(3) . ?
N17 B3 1.536(3) . ?
N18 C22 1.332(3) . ?
N19 C27 1.352(3) . ?
N19 N20 1.378(3) . ?
N19 B3 1.548(4) . ?
N20 C25 1.332(3) . ?
N21 C20 1.428(3) . ?
C1 C2 1.400(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.374(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.389(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.374(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.394(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.369(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.399(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.389(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.367(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.10(3) . ?
B2 H2 1.14(3) . ?
B3 H3 1.107(16) . ?

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
N13 Gd1 N20 135.85(7) . . ?
N13 Gd1 N4 82.70(7) . . ?
N20 Gd1 N4 133.83(6) . . ?
N13 Gd1 N18 81.65(6) . . ?
N20 Gd1 N18 80.15(6) . . ?
N4 Gd1 N18 83.09(7) . . ?
N13 Gd1 N11 80.72(7) . . ?
N20 Gd1 N11 83.88(6) . . ?
N4 Gd1 N11 135.32(6) . . ?
N18 Gd1 N11 134.24(7) . . ?
N13 Gd1 N6 134.77(6) . . ?
N20 Gd1 N6 83.35(6) . . ?
N4 Gd1 N6 79.65(7) . . ?
N18 Gd1 N6 136.05(6) . . ?
N11 Gd1 N6 83.31(7) . . ?
N13 Gd1 N9 69.39(6) . . ?
N20 Gd1 N9 66.47(6) . . ?
N4 Gd1 N9 140.90(6) . . ?
N18 Gd1 N9 66.63(6) . . ?
N11 Gd1 N9 67.66(6) . . ?
N6 Gd1 N9 139.42(6) . . ?
N13 Gd1 N2 66.74(6) . . ?
N20 Gd1 N2 140.91(6) . . ?
N4 Gd1 N2 68.00(6) . . ?
N18 Gd1 N2 138.93(6) . . ?
N11 Gd1 N2 67.33(6) . . ?
N6 Gd1 N2 68.05(6) . . ?
N9 Gd1 N2 120.48(6) . . ?
N13 Gd1 N16 138.71(6) . . ?
N20 Gd1 N16 67.30(7) . . ?
N4 Gd1 N16 66.54(6) . . ?
N18 Gd1 N16 68.39(7) . . ?
N11 Gd1 N16 140.56(6) . . ?
N6 Gd1 N16 67.65(6) . . ?
N9 Gd1 N16 119.13(6) . . ?
N2 Gd1 N16 120.38(6) . . ?
C3 N1 N2 111.2(2) . . ?
C3 N1 B1 129.1(2) . . ?
N2 N1 B1 119.69(19) . . ?
C1 N2 N1 106.2(2) . . ?
C1 N2 Gd1 131.06(17) . . ?
N1 N2 Gd1 122.52(14) . . ?
C6 N3 N4 109.6(2) . . ?
C6 N3 B1 126.6(2) . . ?
N4 N3 B1 123.7(2) . . ?
C4 N4 N3 105.6(2) . . ?
C4 N4 Gd1 129.60(17) . . ?
N3 N4 Gd1 123.94(14) . . ?
C9 N5 N6 110.1(2) . . ?
C9 N5 B1 126.3(2) . . ?
N6 N5 B1 123.5(2) . . ?
C7 N6 N5 105.4(2) . . ?
C7 N6 Gd1 129.00(17) . . ?
N5 N6 Gd1 123.31(15) . . ?
O2 N7 O1 124.2(2) . . ?
O2 N7 C2 117.9(2) . . ?
O1 N7 C2 117.9(2) . . ?
C12 N8 N9 111.2(2) . . ?
C12 N8 B2 129.4(2) . . ?
N9 N8 B2 119.5(2) . . ?
C10 N9 N8 105.8(2) . . ?
C10 N9 Gd1 131.79(17) . . ?
N8 N9 Gd1 122.08(14) . . ?
C15 N10 N11 109.9(2) . . ?
C15 N10 B2 125.5(2) . . ?
N11 N10 B2 124.7(2) . . ?
C13 N11 N10 105.5(2) . . ?
C13 N11 Gd1 130.26(18) . . ?
N10 N11 Gd1 122.12(15) . . ?
C18 N12 N13 109.2(2) . . ?
C18 N12 B2 127.1(2) . . ?
N13 N12 B2 123.7(2) . . ?
C16 N13 N12 105.7(2) . . ?
C16 N13 Gd1 128.78(17) . . ?
N12 N13 Gd1 122.46(15) . . ?
O4 N14 O3 124.0(2) . . ?
O4 N14 C11 117.9(2) . . ?
O3 N14 C11 118.1(2) . . ?
C21 N15 N16 111.0(2) . . ?
C21 N15 B3 129.0(2) . . ?
N16 N15 B3 119.4(2) . . ?
C19 N16 N15 106.0(2) . . ?
C19 N16 Gd1 131.07(16) . . ?
N15 N16 Gd1 122.52(15) . . ?
C24 N17 N18 109.6(2) . . ?
C24 N17 B3 126.2(2) . . ?
N18 N17 B3 124.22(19) . . ?
C22 N18 N17 105.55(19) . . ?
C22 N18 Gd1 128.21(15) . . ?
N17 N18 Gd1 122.95(14) . . ?
C27 N19 N20 109.2(2) . . ?
C27 N19 B3 127.5(2) . . ?
N20 N19 B3 123.2(2) . . ?
C25 N20 N19 105.5(2) . . ?
C25 N20 Gd1 129.16(16) . . ?
N19 N20 Gd1 123.70(14) . . ?
O6 N21 O5 123.8(2) . . ?
O6 N21 C20 118.7(2) . . ?
O5 N21 C20 117.5(2) . . ?
N2 C1 C2 109.2(2) . . ?
N2 C1 H1A 125.4 . . ?
C2 C1 H1A 125.4 . . ?
C3 C2 C1 107.3(2) . . ?
C3 C2 N7 126.7(2) . . ?
C1 C2 N7 126.0(3) . . ?
N1 C3 C2 106.1(2) . . ?
N1 C3 H3A 126.9 . . ?
C2 C3 H3A 126.9 . . ?
N4 C4 C5 111.4(2) . . ?
N4 C4 H4 124.3 . . ?
C5 C4 H4 124.3 . . ?
C6 C5 C4 104.1(2) . . ?
C6 C5 H5 127.9 . . ?
C4 C5 H5 127.9 . . ?
N3 C6 C5 109.1(3) . . ?
N3 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
N6 C7 C8 111.5(2) . . ?
N6 C7 H7 124.3 . . ?
C8 C7 H7 124.3 . . ?
C9 C8 C7 104.5(2) . . ?
C9 C8 H8 127.8 . . ?
C7 C8 H8 127.8 . . ?
N5 C9 C8 108.6(2) . . ?
N5 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
N9 C10 C11 109.6(2) . . ?
N9 C10 H10 125.2 . . ?
C11 C10 H10 125.2 . . ?
C12 C11 C10 107.0(2) . . ?
C12 C11 N14 126.3(2) . . ?
C10 C11 N14 126.6(2) . . ?
N8 C12 C11 106.5(2) . . ?
N8 C12 H12 126.8 . . ?
C11 C12 H12 126.8 . . ?
N11 C13 C14 111.2(3) . . ?
N11 C13 H13 124.4 . . ?
C14 C13 H13 124.4 . . ?
C15 C14 C13 104.3(2) . . ?
C15 C14 H14 127.8 . . ?
C13 C14 H14 127.8 . . ?
N10 C15 C14 109.1(2) . . ?
N10 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
N13 C16 C17 111.4(2) . . ?
N13 C16 H16 124.3 . . ?
C17 C16 H16 124.3 . . ?
C18 C17 C16 104.4(2) . . ?
C18 C17 H17 127.8 . . ?
C16 C17 H17 127.8 . . ?
N12 C18 C17 109.3(2) . . ?
N12 C18 H18 125.3 . . ?
C17 C18 H18 125.3 . . ?
N16 C19 C20 109.5(2) . . ?
N16 C19 H19 125.2 . . ?
C20 C19 H19 125.2 . . ?
C21 C20 C19 106.7(2) . . ?
C21 C20 N21 126.7(2) . . ?
C19 C20 N21 126.2(2) . . ?
N15 C21 C20 106.8(2) . . ?
N15 C21 H21 126.6 . . ?
C20 C21 H21 126.6 . . ?
N18 C22 C23 111.7(2) . . ?
N18 C22 H22 124.2 . . ?
C23 C22 H22 124.2 . . ?
C24 C23 C22 104.0(2) . . ?
C24 C23 H23 128.0 . . ?
C22 C23 H23 128.0 . . ?
N17 C24 C23 109.1(2) . . ?
N17 C24 H24 125.4 . . ?
C23 C24 H24 125.4 . . ?
N20 C25 C26 111.8(2) . . ?
N20 C25 H25 124.1 . . ?
C26 C25 H25 124.1 . . ?
C27 C26 C25 104.5(2) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 109.1(2) . . ?
N19 C27 H27 125.5 . . ?
C26 C27 H27 125.5 . . ?
N5 B1 N1 107.4(2) . . ?
N5 B1 N3 112.5(2) . . ?
N1 B1 N3 108.2(2) . . ?
N5 B1 H1 112.9(14) . . ?
N1 B1 H1 109.8(13) . . ?
N3 B1 H1 105.9(13) . . ?
N10 B2 N8 108.5(2) . . ?
N10 B2 N12 111.4(2) . . ?
N8 B2 N12 108.4(2) . . ?
N10 B2 H2 107.1(13) . . ?
N8 B2 H2 112.9(13) . . ?
N12 B2 H2 108.6(13) . . ?
N17 B3 N15 109.1(2) . . ?
N17 B3 N19 111.8(2) . . ?
N15 B3 N19 107.1(2) . . ?
N17 B3 H3 112.9(14) . . ?
N15 B3 H3 108.4(14) . . ?
N19 B3 H3 107.2(14) . . ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.078



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Cmpd9
_audit_block_doi                 10.5517/ccdc.csd.cc2dr89r
_database_code_depnum_ccdc_archive 'CCDC 2226894'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Dy N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 Dy N21 O6'
_chemical_formula_weight         936.62

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.291(5)
_cell_length_b                   13.695(3)
_cell_length_c                   29.707(8)
_cell_angle_alpha                90
_cell_angle_beta                 115.032(5)
_cell_angle_gamma                90
_cell_volume                     8954(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1483
_cell_measurement_theta_min      3.478
_cell_measurement_theta_max      38.43

_exptl_crystal_description       diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             3720

_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.258
_exptl_absorpt_coefficient_mu    1.729

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4684
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40697
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.043
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9159
_reflns_number_gt                8195
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          
;
;

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+64.8766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9159
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Dy1 Dy 0.68716(2) 0.65946(2) 0.62439(2) 0.01581(6) Uani 1 1 d . . . . .
O1 O 0.67756(17) 0.1913(2) 0.65658(13) 0.0358(8) Uani 1 1 d . . . . .
O2 O 0.76541(16) 0.1496(2) 0.65880(12) 0.0325(8) Uani 1 1 d . . . . .
O3 O 0.39675(15) 0.8235(2) 0.60506(14) 0.0363(8) Uani 1 1 d . . . . .
O4 O 0.45111(16) 0.9313(2) 0.58853(15) 0.0423(9) Uani 1 1 d . . . . .
O5 O 0.88455(16) 1.0074(2) 0.58523(14) 0.0401(9) Uani 1 1 d . . . . .
O6 O 0.91528(17) 0.8560(2) 0.59581(16) 0.0463(10) Uani 1 1 d . . . . .
N1 N 0.78472(16) 0.4453(2) 0.64619(12) 0.0180(7) Uani 1 1 d . . . . .
N2 N 0.72833(16) 0.4720(2) 0.64211(13) 0.0196(7) Uani 1 1 d . . . . .
N3 N 0.83836(16) 0.5990(2) 0.68601(13) 0.0195(7) Uani 1 1 d . . . . .
N4 N 0.79251(16) 0.6512(2) 0.69021(12) 0.0199(7) Uani 1 1 d . . . . .
N5 N 0.79882(16) 0.5715(2) 0.59246(12) 0.0180(7) Uani 1 1 d . . . . .
N6 N 0.74204(16) 0.6126(2) 0.57292(12) 0.0172(7) Uani 1 1 d . . . . .
N7 N 0.72654(19) 0.2110(2) 0.65567(13) 0.0255(8) Uani 1 1 d . . . . .
N8 N 0.53488(16) 0.6365(2) 0.61847(13) 0.0200(8) Uani 1 1 d . . . . .
N9 N 0.57309(16) 0.7049(2) 0.61288(13) 0.0196(7) Uani 1 1 d . . . . .
N10 N 0.61235(16) 0.5217(2) 0.67748(13) 0.0203(7) Uani 1 1 d . . . . .
N11 N 0.66381(16) 0.5759(2) 0.68874(12) 0.0170(7) Uani 1 1 d . . . . .
N12 N 0.56889(16) 0.4949(2) 0.58400(13) 0.0210(8) Uani 1 1 d . . . . .
N13 N 0.61026(16) 0.5391(2) 0.57016(13) 0.0210(8) Uani 1 1 d . . . . .
N14 N 0.44238(18) 0.8479(3) 0.59937(15) 0.0306(9) Uani 1 1 d . . . . .
N15 N 0.74274(16) 0.9022(2) 0.61093(12) 0.0170(7) Uani 1 1 d . . . . .
N16 N 0.76141(16) 0.8057(2) 0.61814(13) 0.0184(7) Uani 1 1 d . . . . .
N17 N 0.63323(16) 0.8738(2) 0.55922(13) 0.0187(7) Uani 1 1 d . . . . .
N18 N 0.63281(16) 0.7737(2) 0.55411(12) 0.0188(7) Uani 1 1 d . . . . .
N19 N 0.67239(15) 0.8997(2) 0.65279(12) 0.0164(7) Uani 1 1 d . . . . .
N20 N 0.68305(16) 0.8069(2) 0.67248(12) 0.0178(7) Uani 1 1 d . . . . .
N21 N 0.88030(19) 0.9212(3) 0.59559(15) 0.0314(9) Uani 1 1 d . . . . .
C1 C 0.7008(2) 0.3897(3) 0.64521(15) 0.0203(9) Uani 1 1 d . . . . .
H1A H 0.661106 0.385394 0.643889 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7393(2) 0.3114(3) 0.65065(15) 0.0191(9) Uani 1 1 d . . . . .
C3 C 0.7925(2) 0.3486(3) 0.65114(15) 0.0224(9) Uani 1 1 d . . . . .
H3A H 0.827420 0.312679 0.654326 0.027 Uiso 1 1 calc R U . . .
C4 C 0.8197(2) 0.7047(3) 0.73134(16) 0.0249(10) Uani 1 1 d . . . . .
H4 H 0.798902 0.749027 0.743324 0.030 Uiso 1 1 calc R U . . .
C5 C 0.8821(2) 0.6879(3) 0.75464(18) 0.0307(11) Uani 1 1 d . . . . .
H5 H 0.911193 0.716234 0.784408 0.037 Uiso 1 1 calc R U . . .
C6 C 0.8916(2) 0.6210(3) 0.72448(17) 0.0270(10) Uani 1 1 d . . . . .
H6 H 0.929887 0.594078 0.729825 0.032 Uiso 1 1 calc R U . . .
C7 C 0.7321(2) 0.6422(3) 0.52696(15) 0.0192(9) Uani 1 1 d . . . . .
H7 H 0.696074 0.673323 0.504336 0.023 Uiso 1 1 calc R U . . .
C8 C 0.7822(2) 0.6209(3) 0.51702(16) 0.0226(9) Uani 1 1 d . . . . .
H8 H 0.787119 0.634912 0.487597 0.027 Uiso 1 1 calc R U . . .
C9 C 0.8226(2) 0.5757(3) 0.55897(16) 0.0211(9) Uani 1 1 d . . . . .
H9 H 0.861198 0.551004 0.563750 0.025 Uiso 1 1 calc R U . . .
C10 C 0.54300(19) 0.7895(3) 0.60476(15) 0.0202(9) Uani 1 1 d . . . . .
H10 H 0.557820 0.850413 0.599248 0.024 Uiso 1 1 calc R U . . .
C11 C 0.48671(19) 0.7750(3) 0.60557(16) 0.0215(9) Uani 1 1 d . . . . .
C12 C 0.4831(2) 0.6771(3) 0.61425(16) 0.0228(9) Uani 1 1 d . . . . .
H12 H 0.449960 0.644554 0.616751 0.027 Uiso 1 1 calc R U . . .
C13 C 0.7020(2) 0.5487(3) 0.73448(15) 0.0219(9) Uani 1 1 d . . . . .
H13 H 0.741686 0.574714 0.752016 0.026 Uiso 1 1 calc R U . . .
C14 C 0.6766(2) 0.4777(3) 0.75334(17) 0.0286(10) Uani 1 1 d . . . . .
H14 H 0.694429 0.446641 0.784862 0.034 Uiso 1 1 calc R U . . .
C15 C 0.6197(2) 0.4629(3) 0.71585(16) 0.0260(10) Uani 1 1 d . . . . .
H15 H 0.590240 0.418332 0.716893 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6084(2) 0.4879(3) 0.53112(16) 0.0254(10) Uani 1 1 d . . . . .
H16 H 0.632194 0.502031 0.513503 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5670(2) 0.4111(3) 0.51967(17) 0.0311(11) Uani 1 1 d . . . . .
H17 H 0.557320 0.364248 0.493871 0.037 Uiso 1 1 calc R U . . .
C18 C 0.5434(2) 0.4185(3) 0.55384(17) 0.0298(11) Uani 1 1 d . . . . .
H18 H 0.513633 0.376248 0.556015 0.036 Uiso 1 1 calc R U . . .
C19 C 0.81408(19) 0.8025(3) 0.61556(15) 0.0192(9) Uani 1 1 d . . . . .
H19 H 0.837688 0.745219 0.619232 0.023 Uiso 1 1 calc R U . . .
C20 C 0.8301(2) 0.8964(3) 0.60655(16) 0.0229(9) Uani 1 1 d . . . . .
C21 C 0.78440(19) 0.9574(3) 0.60418(15) 0.0213(9) Uani 1 1 d . . . . .
H21 H 0.782454 1.025949 0.598789 0.026 Uiso 1 1 calc R U . . .
C22 C 0.5886(2) 0.7551(3) 0.50917(16) 0.0234(9) Uani 1 1 d . . . . .
H22 H 0.577884 0.691480 0.495490 0.028 Uiso 1 1 calc R U . . .
C23 C 0.5602(2) 0.8403(3) 0.48483(17) 0.0307(10) Uani 1 1 d . . . . .
H23 H 0.527678 0.846427 0.452739 0.037 Uiso 1 1 calc R U . . .
C24 C 0.5898(2) 0.9135(3) 0.51773(16) 0.0257(10) Uani 1 1 d . . . . .
H24 H 0.581231 0.981218 0.512216 0.031 Uiso 1 1 calc R U . . .
C25 C 0.67230(19) 0.8109(3) 0.71297(15) 0.0197(9) Uani 1 1 d . . . . .
H25 H 0.675963 0.757060 0.734212 0.024 Uiso 1 1 calc R U . . .
C26 C 0.6549(2) 0.9050(3) 0.71987(16) 0.0228(9) Uani 1 1 d . . . . .
H26 H 0.644754 0.927340 0.745670 0.027 Uiso 1 1 calc R U . . .
C27 C 0.65592(19) 0.9576(3) 0.68122(16) 0.0214(9) Uani 1 1 d . . . . .
H27 H 0.646361 1.025008 0.675395 0.026 Uiso 1 1 calc R U . . .
B1 B 0.8286(2) 0.5245(3) 0.64432(18) 0.0200(10) Uani 1 1 d . . . . .
H1 H 0.873(2) 0.489(3) 0.6522(17) 0.030 Uiso 1 1 d . U . . .
B2 B 0.5558(2) 0.5281(3) 0.62781(18) 0.0207(10) Uani 1 1 d . . . . .
H2 H 0.516(2) 0.485(3) 0.6297(17) 0.031 Uiso 1 1 d . U . . .
B3 B 0.6788(2) 0.9280(3) 0.60547(18) 0.0180(9) Uani 1 1 d D . . . .
H3 H 0.666(2) 1.0005(17) 0.5956(16) 0.027 Uiso 1 1 d D U . . .


_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
Dy1 N4 2.480(4) . ?
Dy1 N11 2.491(3) . ?
Dy1 N18 2.493(3) . ?
Dy1 N20 2.500(3) . ?
Dy1 N6 2.500(3) . ?
Dy1 N13 2.501(3) . ?
Dy1 N9 2.716(4) . ?
Dy1 N2 2.725(3) . ?
Dy1 N16 2.754(3) . ?
O1 N7 1.231(5) . ?
O2 N7 1.238(5) . ?
O3 N14 1.236(5) . ?
O4 N14 1.229(5) . ?
O5 N21 1.236(5) . ?
O6 N21 1.230(5) . ?
N1 C3 1.338(5) . ?
N1 N2 1.373(5) . ?
N1 B1 1.538(6) . ?
N2 C1 1.333(5) . ?
N3 C6 1.348(6) . ?
N3 N4 1.373(5) . ?
N3 B1 1.543(6) . ?
N4 C4 1.335(5) . ?
N5 C9 1.346(5) . ?
N5 N6 1.371(5) . ?
N5 B1 1.539(6) . ?
N6 C7 1.345(5) . ?
N7 C2 1.430(5) . ?
N8 C12 1.331(5) . ?
N8 N9 1.377(5) . ?
N8 B2 1.556(6) . ?
N9 C10 1.337(5) . ?
N10 C15 1.345(5) . ?
N10 N11 1.368(5) . ?
N10 B2 1.535(6) . ?
N11 C13 1.333(5) . ?
N12 C18 1.345(5) . ?
N12 N13 1.377(5) . ?
N12 B2 1.534(6) . ?
N13 C16 1.340(5) . ?
N14 C11 1.422(5) . ?
N15 C21 1.345(5) . ?
N15 N16 1.383(4) . ?
N15 B3 1.534(6) . ?
N16 C19 1.315(5) . ?
N17 C24 1.351(5) . ?
N17 N18 1.380(4) . ?
N17 B3 1.542(6) . ?
N18 C22 1.337(5) . ?
N19 C27 1.337(5) . ?
N19 N20 1.377(4) . ?
N19 B3 1.528(6) . ?
N20 C25 1.335(5) . ?
N21 C20 1.430(5) . ?
C1 C2 1.386(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.384(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.394(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.399(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.365(6) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.392(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.394(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.363(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.402(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.367(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.393(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.398(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.364(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.10(5) . ?
B2 H2 1.14(5) . ?
B3 H3 1.045(19) . ?

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
N4 Dy1 N11 82.42(11) . . ?
N4 Dy1 N18 133.87(11) . . ?
N11 Dy1 N18 135.98(11) . . ?
N4 Dy1 N20 82.17(11) . . ?
N11 Dy1 N20 81.68(10) . . ?
N18 Dy1 N20 80.61(11) . . ?
N4 Dy1 N6 80.28(11) . . ?
N11 Dy1 N6 134.82(10) . . ?
N18 Dy1 N6 83.07(11) . . ?
N20 Dy1 N6 135.84(11) . . ?
N4 Dy1 N13 135.90(11) . . ?
N11 Dy1 N13 80.85(11) . . ?
N18 Dy1 N13 83.53(11) . . ?
N20 Dy1 N13 134.50(11) . . ?
N6 Dy1 N13 83.29(11) . . ?
N4 Dy1 N9 140.09(11) . . ?
N11 Dy1 N9 69.54(11) . . ?
N18 Dy1 N9 66.45(11) . . ?
N20 Dy1 N9 66.54(11) . . ?
N6 Dy1 N9 139.56(11) . . ?
N13 Dy1 N9 68.01(11) . . ?
N4 Dy1 N2 68.45(10) . . ?
N11 Dy1 N2 66.60(10) . . ?
N18 Dy1 N2 140.71(10) . . ?
N20 Dy1 N2 138.67(10) . . ?
N6 Dy1 N2 68.24(10) . . ?
N13 Dy1 N2 67.45(11) . . ?
N9 Dy1 N2 120.76(10) . . ?
N4 Dy1 N16 66.40(10) . . ?
N11 Dy1 N16 138.97(10) . . ?
N18 Dy1 N16 67.48(11) . . ?
N20 Dy1 N16 68.69(10) . . ?
N6 Dy1 N16 67.15(10) . . ?
N13 Dy1 N16 140.17(11) . . ?
N9 Dy1 N16 119.16(10) . . ?
N2 Dy1 N16 120.08(10) . . ?
C3 N1 N2 111.2(3) . . ?
C3 N1 B1 129.4(4) . . ?
N2 N1 B1 119.4(3) . . ?
C1 N2 N1 106.3(3) . . ?
C1 N2 Dy1 131.0(3) . . ?
N1 N2 Dy1 122.6(2) . . ?
C6 N3 N4 109.3(3) . . ?
C6 N3 B1 126.5(4) . . ?
N4 N3 B1 124.2(3) . . ?
C4 N4 N3 105.2(4) . . ?
C4 N4 Dy1 130.0(3) . . ?
N3 N4 Dy1 123.9(2) . . ?
C9 N5 N6 109.8(3) . . ?
C9 N5 B1 126.2(4) . . ?
N6 N5 B1 123.9(3) . . ?
C7 N6 N5 105.6(3) . . ?
C7 N6 Dy1 129.1(3) . . ?
N5 N6 Dy1 123.2(2) . . ?
O1 N7 O2 124.2(4) . . ?
O1 N7 C2 117.8(4) . . ?
O2 N7 C2 118.0(4) . . ?
C12 N8 N9 111.3(3) . . ?
C12 N8 B2 129.7(3) . . ?
N9 N8 B2 119.0(3) . . ?
C10 N9 N8 105.4(3) . . ?
C10 N9 Dy1 132.2(3) . . ?
N8 N9 Dy1 122.2(2) . . ?
C15 N10 N11 109.8(3) . . ?
C15 N10 B2 126.3(4) . . ?
N11 N10 B2 123.9(3) . . ?
C13 N11 N10 105.5(3) . . ?
C13 N11 Dy1 128.6(3) . . ?
N10 N11 Dy1 122.9(2) . . ?
C18 N12 N13 109.4(4) . . ?
C18 N12 B2 126.4(4) . . ?
N13 N12 B2 124.2(3) . . ?
C16 N13 N12 105.4(3) . . ?
C16 N13 Dy1 130.2(3) . . ?
N12 N13 Dy1 122.6(2) . . ?
O4 N14 O3 123.5(4) . . ?
O4 N14 C11 118.8(4) . . ?
O3 N14 C11 117.8(4) . . ?
C21 N15 N16 110.0(3) . . ?
C21 N15 B3 130.3(3) . . ?
N16 N15 B3 119.2(3) . . ?
C19 N16 N15 106.7(3) . . ?
C19 N16 Dy1 131.3(3) . . ?
N15 N16 Dy1 121.6(2) . . ?
C24 N17 N18 109.4(3) . . ?
C24 N17 B3 127.5(3) . . ?
N18 N17 B3 123.1(3) . . ?
C22 N18 N17 105.3(3) . . ?
C22 N18 Dy1 129.3(3) . . ?
N17 N18 Dy1 123.7(2) . . ?
C27 N19 N20 109.4(3) . . ?
C27 N19 B3 127.2(3) . . ?
N20 N19 B3 123.4(3) . . ?
C25 N20 N19 105.7(3) . . ?
C25 N20 Dy1 128.2(3) . . ?
N19 N20 Dy1 123.3(2) . . ?
O6 N21 O5 124.4(4) . . ?
O6 N21 C20 118.7(4) . . ?
O5 N21 C20 116.9(4) . . ?
N2 C1 C2 109.2(4) . . ?
N2 C1 H1A 125.4 . . ?
C2 C1 H1A 125.4 . . ?
C3 C2 C1 107.3(4) . . ?
C3 C2 N7 126.5(4) . . ?
C1 C2 N7 126.2(4) . . ?
N1 C3 C2 106.0(4) . . ?
N1 C3 H3A 127.0 . . ?
C2 C3 H3A 127.0 . . ?
N4 C4 C5 112.1(4) . . ?
N4 C4 H4 123.9 . . ?
C5 C4 H4 123.9 . . ?
C6 C5 C4 103.5(4) . . ?
C6 C5 H5 128.2 . . ?
C4 C5 H5 128.2 . . ?
N3 C6 C5 109.8(4) . . ?
N3 C6 H6 125.1 . . ?
C5 C6 H6 125.1 . . ?
N6 C7 C8 110.7(4) . . ?
N6 C7 H7 124.6 . . ?
C8 C7 H7 124.6 . . ?
C9 C8 C7 104.7(4) . . ?
C9 C8 H8 127.6 . . ?
C7 C8 H8 127.6 . . ?
N5 C9 C8 109.1(4) . . ?
N5 C9 H9 125.4 . . ?
C8 C9 H9 125.4 . . ?
N9 C10 C11 109.9(4) . . ?
N9 C10 H10 125.1 . . ?
C11 C10 H10 125.1 . . ?
C12 C11 C10 106.4(4) . . ?
C12 C11 N14 127.2(4) . . ?
C10 C11 N14 126.4(4) . . ?
N8 C12 C11 107.0(4) . . ?
N8 C12 H12 126.5 . . ?
C11 C12 H12 126.5 . . ?
N11 C13 C14 111.7(4) . . ?
N11 C13 H13 124.2 . . ?
C14 C13 H13 124.2 . . ?
C15 C14 C13 104.0(4) . . ?
C15 C14 H14 128.0 . . ?
C13 C14 H14 128.0 . . ?
N10 C15 C14 109.0(4) . . ?
N10 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
N13 C16 C17 111.3(4) . . ?
N13 C16 H16 124.4 . . ?
C17 C16 H16 124.4 . . ?
C18 C17 C16 104.4(4) . . ?
C18 C17 H17 127.8 . . ?
C16 C17 H17 127.8 . . ?
N12 C18 C17 109.5(4) . . ?
N12 C18 H18 125.2 . . ?
C17 C18 H18 125.2 . . ?
N16 C19 C20 109.6(4) . . ?
N16 C19 H19 125.2 . . ?
C20 C19 H19 125.2 . . ?
C21 C20 C19 106.6(4) . . ?
C21 C20 N21 126.5(4) . . ?
C19 C20 N21 126.4(4) . . ?
N15 C21 C20 107.1(3) . . ?
N15 C21 H21 126.4 . . ?
C20 C21 H21 126.4 . . ?
N18 C22 C23 111.8(4) . . ?
N18 C22 H22 124.1 . . ?
C23 C22 H22 124.1 . . ?
C24 C23 C22 104.3(4) . . ?
C24 C23 H23 127.9 . . ?
C22 C23 H23 127.9 . . ?
N17 C24 C23 109.2(4) . . ?
N17 C24 H24 125.4 . . ?
C23 C24 H24 125.4 . . ?
N20 C25 C26 110.9(4) . . ?
N20 C25 H25 124.6 . . ?
C26 C25 H25 124.6 . . ?
C27 C26 C25 104.4(4) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 109.6(4) . . ?
N19 C27 H27 125.2 . . ?
C26 C27 H27 125.2 . . ?
N1 B1 N5 107.0(4) . . ?
N1 B1 N3 108.1(3) . . ?
N5 B1 N3 112.0(3) . . ?
N1 B1 H1 108(2) . . ?
N5 B1 H1 113(2) . . ?
N3 B1 H1 108(2) . . ?
N12 B2 N10 112.1(4) . . ?
N12 B2 N8 107.5(3) . . ?
N10 B2 N8 108.5(3) . . ?
N12 B2 H2 111(2) . . ?
N10 B2 H2 111(2) . . ?
N8 B2 H2 107(2) . . ?
N19 B3 N15 109.7(3) . . ?
N19 B3 N17 112.6(3) . . ?
N15 B3 N17 107.2(3) . . ?
N19 B3 H3 111(2) . . ?
N15 B3 H3 115(3) . . ?
N17 B3 H3 101(3) . . ?

_refine_diff_density_max         1.518
_refine_diff_density_min         -1.755
_refine_diff_density_rms         0.102



####################################################################### 
# 
# 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_Cmpd2
_audit_block_doi                 10.5517/ccdc.csd.cc2dr81h
_database_code_depnum_ccdc_archive 'CCDC 2226886'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Ce N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 Ce N21 O6'
_chemical_formula_weight         914.24

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.400(8)
_cell_length_b                   13.801(3)
_cell_length_c                   29.778(10)
_cell_angle_alpha                90
_cell_angle_beta                 116.759(12)
_cell_angle_gamma                90
_cell_volume                     8954(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    319
_cell_measurement_theta_min      3.484
_cell_measurement_theta_max      35.42

_exptl_crystal_description       diamond
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_F_000             3656

_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.128
_exptl_absorpt_coefficient_mu    1.077

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
 Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68665
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.027
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9144
_reflns_number_gt                7799
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0229P)²+3.7912P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9144
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Ce1 Ce 0.31120(2) 0.33824(2) 0.37561(2) 0.01260(4) Uani 1 1 d . . . . .
O1 O 0.08606(8) 0.14063(12) 0.40362(8) 0.0420(5) Uani 1 1 d . . . . .
O2 O 0.11628(8) -0.00980(11) 0.41465(7) 0.0369(4) Uani 1 1 d . . . . .
O3 O 0.23047(8) 0.84581(10) 0.34178(6) 0.0312(4) Uani 1 1 d . . . . .
O4 O 0.31610(8) 0.80417(11) 0.34070(6) 0.0331(4) Uani 1 1 d . . . . .
O5 O 0.60155(8) 0.17812(12) 0.39341(7) 0.0369(4) Uani 1 1 d . . . . .
O6 O 0.54811(8) 0.07122(11) 0.41054(7) 0.0417(5) Uani 1 1 d . . . . .
N1 N 0.25676(8) 0.09360(11) 0.38877(6) 0.0155(4) Uani 1 1 d . . . . .
N2 N 0.23822(8) 0.18951(11) 0.38107(6) 0.0161(4) Uani 1 1 d . . . . .
N3 N 0.32752(8) 0.09262(11) 0.34788(6) 0.0158(4) Uani 1 1 d . . . . .
N4 N 0.31553(8) 0.18337(11) 0.32695(6) 0.0161(4) Uani 1 1 d . . . . .
N5 N 0.36885(8) 0.11730(11) 0.44261(6) 0.0162(4) Uani 1 1 d . . . . .
N6 N 0.36917(8) 0.21543(11) 0.44873(6) 0.0159(4) Uani 1 1 d . . . . .
N7 N 0.12073(9) 0.07544(14) 0.40402(7) 0.0291(5) Uani 1 1 d . . . . .
N8 N 0.21075(8) 0.55277(11) 0.35237(6) 0.0160(4) Uani 1 1 d . . . . .
N9 N 0.26679(8) 0.52602(11) 0.35601(6) 0.0165(4) Uani 1 1 d . . . . .
N10 N 0.19564(8) 0.42809(11) 0.40619(6) 0.0157(4) Uani 1 1 d . . . . .
N11 N 0.25327(8) 0.38889(11) 0.42725(6) 0.0165(4) Uani 1 1 d . . . . .
N12 N 0.15279(8) 0.40154(12) 0.31128(6) 0.0169(4) Uani 1 1 d . . . . .
N13 N 0.19748(8) 0.34935(11) 0.30635(6) 0.0172(4) Uani 1 1 d . . . . .
N14 N 0.26814(9) 0.78463(12) 0.34333(7) 0.0239(4) Uani 1 1 d . . . . .
N15 N 0.46508(8) 0.36414(11) 0.38253(6) 0.0163(4) Uani 1 1 d . . . . .
N16 N 0.42805(8) 0.29618(12) 0.38905(6) 0.0165(4) Uani 1 1 d . . . . .
N17 N 0.43297(8) 0.50788(12) 0.41669(6) 0.0185(4) Uani 1 1 d . . . . .
N18 N 0.39326(8) 0.46484(11) 0.43160(6) 0.0177(4) Uani 1 1 d . . . . .
N19 N 0.38768(8) 0.47944(11) 0.32217(6) 0.0174(4) Uani 1 1 d . . . . .
N20 N 0.33607(8) 0.42411(11) 0.30911(6) 0.0163(4) Uani 1 1 d . . . . .
N21 N 0.55698(9) 0.15419(13) 0.39985(7) 0.0276(4) Uani 1 1 d . . . . .
C1 C 0.18563(10) 0.19254(15) 0.38358(8) 0.0202(5) Uani 1 1 d . . . . .
H1A H 0.161861 0.249311 0.379620 0.024 Uiso 1 1 calc R U . . .
C2 C 0.17013(10) 0.10026(14) 0.39288(8) 0.0201(5) Uani 1 1 d . . . . .
C3 C 0.21638(10) 0.03923(14) 0.39605(8) 0.0186(5) Uani 1 1 d . . . . .
H3A H 0.218974 -0.028548 0.402241 0.022 Uiso 1 1 calc R U . . .
C4 C 0.32795(10) 0.17915(14) 0.28755(8) 0.0196(5) Uani 1 1 d . . . . .
H4 H 0.323932 0.232087 0.265890 0.023 Uiso 1 1 calc R U . . .
C5 C 0.34753(10) 0.08682(15) 0.28257(8) 0.0226(5) Uani 1 1 d . . . . .
H5 H 0.358926 0.064878 0.257703 0.027 Uiso 1 1 calc R U . . .
C6 C 0.34676(10) 0.03457(15) 0.32137(8) 0.0198(5) Uani 1 1 d . . . . .
H6 H 0.357946 -0.031653 0.328459 0.024 Uiso 1 1 calc R U . . .
C7 C 0.41464(10) 0.23382(16) 0.49449(8) 0.0231(5) Uani 1 1 d . . . . .
H7 H 0.425630 0.296602 0.508855 0.028 Uiso 1 1 calc R U . . .
C8 C 0.44362(11) 0.14848(16) 0.51815(8) 0.0274(5) Uani 1 1 d . . . . .
H8 H 0.477082 0.141593 0.550700 0.033 Uiso 1 1 calc R U . . .
C9 C 0.41347(10) 0.07671(15) 0.48436(8) 0.0235(5) Uani 1 1 d . . . . .
H9 H 0.422406 0.009439 0.489402 0.028 Uiso 1 1 calc R U . . .
C10 C 0.29408(10) 0.60700(14) 0.35295(7) 0.0174(4) Uani 1 1 d . . . . .
H10 H 0.333486 0.611004 0.353944 0.021 Uiso 1 1 calc R U . . .
C11 C 0.25569(10) 0.68548(13) 0.34802(7) 0.0170(4) Uani 1 1 d . . . . .
C12 C 0.20328(10) 0.64850(13) 0.34786(7) 0.0175(4) Uani 1 1 d . . . . .
H12 H 0.168595 0.684171 0.345086 0.021 Uiso 1 1 calc R U . . .
C13 C 0.26336(10) 0.35910(14) 0.47311(8) 0.0184(5) Uani 1 1 d . . . . .
H13 H 0.300155 0.328931 0.496564 0.022 Uiso 1 1 calc R U . . .
C14 C 0.21310(10) 0.37795(14) 0.48206(8) 0.0200(5) Uani 1 1 d . . . . .
H14 H 0.208626 0.363364 0.511414 0.024 Uiso 1 1 calc R U . . .
C15 C 0.17141(10) 0.42239(14) 0.43887(8) 0.0195(5) Uani 1 1 d . . . . .
H15 H 0.132036 0.445323 0.432986 0.023 Uiso 1 1 calc R U . . .
C16 C 0.16846(10) 0.29698(15) 0.26449(8) 0.0219(5) Uani 1 1 d . . . . .
H16 H 0.188254 0.253098 0.251937 0.026 Uiso 1 1 calc R U . . .
C17 C 0.10600(11) 0.31460(16) 0.24171(9) 0.0298(6) Uani 1 1 d . . . . .
H17 H 0.075569 0.287103 0.211516 0.036 Uiso 1 1 calc R U . . .
C18 C 0.09789(11) 0.38110(16) 0.27273(9) 0.0267(5) Uani 1 1 d . . . . .
H18 H 0.059734 0.408100 0.267687 0.032 Uiso 1 1 calc R U . . .
C19 C 0.45797(10) 0.21255(14) 0.39673(7) 0.0175(4) Uani 1 1 d . . . . .
H19 H 0.443705 0.152199 0.402714 0.021 Uiso 1 1 calc R U . . .
C20 C 0.51294(10) 0.22649(14) 0.39472(8) 0.0187(5) Uani 1 1 d . . . . .
C21 C 0.51629(10) 0.32368(14) 0.38587(8) 0.0192(5) Uani 1 1 d . . . . .
H21 H 0.548872 0.355704 0.382746 0.023 Uiso 1 1 calc R U . . .
C22 C 0.39579(10) 0.51842(15) 0.46990(8) 0.0231(5) Uani 1 1 d . . . . .
H22 H 0.372740 0.505783 0.487834 0.028 Uiso 1 1 calc R U . . .
C23 C 0.43681(11) 0.59544(16) 0.48003(8) 0.0295(6) Uani 1 1 d . . . . .
H23 H 0.447130 0.643624 0.505332 0.035 Uiso 1 1 calc R U . . .
C24 C 0.45883(11) 0.58588(14) 0.44524(8) 0.0252(5) Uani 1 1 d . . . . .
H24 H 0.487704 0.627727 0.441920 0.030 Uiso 1 1 calc R U . . .
C25 C 0.29680(10) 0.45173(15) 0.26271(8) 0.0203(5) Uani 1 1 d . . . . .
H25 H 0.256960 0.425124 0.243993 0.024 Uiso 1 1 calc R U . . .
C26 C 0.32177(11) 0.52447(16) 0.24533(8) 0.0260(5) Uani 1 1 d . . . . .
H26 H 0.303253 0.556435 0.213700 0.031 Uiso 1 1 calc R U . . .
C27 C 0.37900(11) 0.53974(15) 0.28396(8) 0.0232(5) Uani 1 1 d . . . . .
H27 H 0.407998 0.585561 0.283858 0.028 Uiso 1 1 calc R U . . .
B1 B 0.32114(11) 0.06444(17) 0.39535(9) 0.0170(5) Uani 1 1 d . . . . .
H1 H 0.3260(10) -0.0139(15) 0.4020(8) 0.025 Uiso 1 1 d . U . . .
B2 B 0.16595(11) 0.47545(17) 0.35378(9) 0.0175(5) Uani 1 1 d . . . . .
H2 H 0.1241(10) 0.5091(15) 0.3473(8) 0.026 Uiso 1 1 d . U . . .
B3 B 0.44525(12) 0.47142(17) 0.37306(9) 0.0196(5) Uani 1 1 d . . . . .
H3 H 0.4820(10) 0.5149(15) 0.3715(8) 0.029 Uiso 1 1 d . U . . .


_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
Ce1 N20 2.6030(17) . ?
Ce1 N11 2.6095(18) . ?
Ce1 N4 2.6109(16) . ?
Ce1 N13 2.6122(19) . ?
Ce1 N18 2.6146(17) . ?
Ce1 N6 2.6156(17) . ?
Ce1 N16 2.7565(19) . ?
Ce1 N9 2.7681(17) . ?
Ce1 N2 2.7697(17) . ?
O1 N7 1.231(2) . ?
O2 N7 1.236(2) . ?
O3 N14 1.234(2) . ?
O4 N14 1.237(2) . ?
O5 N21 1.231(2) . ?
O6 N21 1.233(2) . ?
N1 C3 1.332(3) . ?
N1 N2 1.384(2) . ?
N1 B1 1.546(3) . ?
N2 C1 1.319(3) . ?
N3 C6 1.349(2) . ?
N3 N4 1.371(2) . ?
N3 B1 1.540(3) . ?
N4 C4 1.338(3) . ?
N5 C9 1.351(3) . ?
N5 N6 1.366(2) . ?
N5 B1 1.547(3) . ?
N6 C7 1.338(3) . ?
N7 C2 1.428(3) . ?
N8 C12 1.332(2) . ?
N8 N9 1.373(2) . ?
N8 B2 1.542(3) . ?
N9 C10 1.325(3) . ?
N10 C15 1.350(3) . ?
N10 N11 1.367(2) . ?
N10 B2 1.539(3) . ?
N11 C13 1.338(3) . ?
N12 C18 1.344(3) . ?
N12 N13 1.369(2) . ?
N12 B2 1.543(3) . ?
N13 C16 1.335(3) . ?
N14 C11 1.422(2) . ?
N15 C21 1.331(3) . ?
N15 N16 1.375(2) . ?
N15 B3 1.544(3) . ?
N16 C19 1.329(2) . ?
N17 C24 1.340(3) . ?
N17 N18 1.370(2) . ?
N17 B3 1.543(3) . ?
N18 C22 1.337(3) . ?
N19 C27 1.347(3) . ?
N19 N20 1.371(2) . ?
N19 B3 1.538(3) . ?
N20 C25 1.334(3) . ?
N21 C20 1.423(3) . ?
C1 C2 1.391(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.377(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.391(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.367(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.396(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.373(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.382(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.368(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.10(2) . ?
B2 H2 1.06(2) . ?
B3 H3 1.10(2) . ?

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
N20 Ce1 N11 134.43(5) . . ?
N20 Ce1 N4 82.47(5) . . ?
N11 Ce1 N4 135.59(5) . . ?
N20 Ce1 N13 84.33(6) . . ?
N11 Ce1 N13 77.57(6) . . ?
N4 Ce1 N13 84.49(5) . . ?
N20 Ce1 N18 78.87(6) . . ?
N11 Ce1 N18 84.70(6) . . ?
N4 Ce1 N18 133.65(6) . . ?
N13 Ce1 N18 134.47(5) . . ?
N20 Ce1 N6 134.79(5) . . ?
N11 Ce1 N6 85.20(5) . . ?
N4 Ce1 N6 77.86(5) . . ?
N13 Ce1 N6 132.79(5) . . ?
N18 Ce1 N6 86.01(5) . . ?
N20 Ce1 N16 68.05(5) . . ?
N11 Ce1 N16 140.37(5) . . ?
N4 Ce1 N16 67.08(5) . . ?
N13 Ce1 N16 142.06(5) . . ?
N18 Ce1 N16 66.61(5) . . ?
N6 Ce1 N16 66.82(5) . . ?
N20 Ce1 N9 67.45(5) . . ?
N11 Ce1 N9 66.98(5) . . ?
N4 Ce1 N9 139.40(5) . . ?
N13 Ce1 N9 66.59(5) . . ?
N18 Ce1 N9 67.88(5) . . ?
N6 Ce1 N9 142.74(5) . . ?
N16 Ce1 N9 120.59(5) . . ?
N20 Ce1 N2 139.31(5) . . ?
N11 Ce1 N2 68.33(5) . . ?
N4 Ce1 N2 67.27(5) . . ?
N13 Ce1 N2 66.88(5) . . ?
N18 Ce1 N2 141.80(5) . . ?
N6 Ce1 N2 65.91(5) . . ?
N16 Ce1 N2 119.06(5) . . ?
N9 Ce1 N2 120.35(5) . . ?
C3 N1 N2 110.80(17) . . ?
C3 N1 B1 128.07(17) . . ?
N2 N1 B1 120.50(16) . . ?
C1 N2 N1 105.94(16) . . ?
C1 N2 Ce1 130.34(13) . . ?
N1 N2 Ce1 123.20(12) . . ?
C6 N3 N4 109.63(16) . . ?
C6 N3 B1 126.36(17) . . ?
N4 N3 B1 123.99(16) . . ?
C4 N4 N3 105.82(15) . . ?
C4 N4 Ce1 127.13(12) . . ?
N3 N4 Ce1 123.33(12) . . ?
C9 N5 N6 109.53(17) . . ?
C9 N5 B1 127.31(18) . . ?
N6 N5 B1 123.07(16) . . ?
C7 N6 N5 106.04(16) . . ?
C7 N6 Ce1 127.91(13) . . ?
N5 N6 Ce1 124.25(12) . . ?
O1 N7 O2 124.0(2) . . ?
O1 N7 C2 118.07(19) . . ?
O2 N7 C2 117.95(19) . . ?
C12 N8 N9 111.15(17) . . ?
C12 N8 B2 128.51(18) . . ?
N9 N8 B2 120.34(16) . . ?
C10 N9 N8 106.35(16) . . ?
C10 N9 Ce1 130.02(14) . . ?
N8 N9 Ce1 123.36(11) . . ?
C15 N10 N11 109.88(16) . . ?
C15 N10 B2 126.64(18) . . ?
N11 N10 B2 123.42(16) . . ?
C13 N11 N10 105.58(17) . . ?
C13 N11 Ce1 128.26(14) . . ?
N10 N11 Ce1 123.62(12) . . ?
C18 N12 N13 109.49(17) . . ?
C18 N12 B2 126.78(18) . . ?
N13 N12 B2 123.66(17) . . ?
C16 N13 N12 105.76(17) . . ?
C16 N13 Ce1 129.32(14) . . ?
N12 N13 Ce1 124.10(12) . . ?
O3 N14 O4 123.95(18) . . ?
O3 N14 C11 118.28(19) . . ?
O4 N14 C11 117.77(18) . . ?
C21 N15 N16 110.96(16) . . ?
C21 N15 B3 128.51(18) . . ?
N16 N15 B3 120.53(17) . . ?
C19 N16 N15 105.76(17) . . ?
C19 N16 Ce1 131.29(13) . . ?
N15 N16 Ce1 122.56(12) . . ?
C24 N17 N18 110.01(18) . . ?
C24 N17 B3 125.57(19) . . ?
N18 N17 B3 124.42(16) . . ?
C22 N18 N17 105.60(17) . . ?
C22 N18 Ce1 129.90(15) . . ?
N17 N18 Ce1 122.24(12) . . ?
C27 N19 N20 109.23(17) . . ?
C27 N19 B3 127.11(18) . . ?
N20 N19 B3 123.65(16) . . ?
C25 N20 N19 105.92(16) . . ?
C25 N20 Ce1 127.82(14) . . ?
N19 N20 Ce1 122.47(12) . . ?
O5 N21 O6 123.99(19) . . ?
O5 N21 C20 118.18(19) . . ?
O6 N21 C20 117.83(19) . . ?
N2 C1 C2 109.92(18) . . ?
N2 C1 H1A 125.0 . . ?
C2 C1 H1A 125.0 . . ?
C3 C2 C1 106.61(19) . . ?
C3 C2 N7 126.05(19) . . ?
C1 C2 N7 126.8(2) . . ?
N1 C3 C2 106.73(18) . . ?
N1 C3 H3A 126.6 . . ?
C2 C3 H3A 126.6 . . ?
N4 C4 C5 110.93(18) . . ?
N4 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
C6 C5 C4 104.85(19) . . ?
C6 C5 H5 127.6 . . ?
C4 C5 H5 127.6 . . ?
N3 C6 C5 108.77(18) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 110.77(19) . . ?
N6 C7 H7 124.6 . . ?
C8 C7 H7 124.6 . . ?
C9 C8 C7 104.97(19) . . ?
C9 C8 H8 127.5 . . ?
C7 C8 H8 127.5 . . ?
N5 C9 C8 108.70(19) . . ?
N5 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
N9 C10 C11 109.11(19) . . ?
N9 C10 H10 125.4 . . ?
C11 C10 H10 125.4 . . ?
C12 C11 C10 106.95(17) . . ?
C12 C11 N14 126.61(19) . . ?
C10 C11 N14 126.4(2) . . ?
N8 C12 C11 106.44(18) . . ?
N8 C12 H12 126.8 . . ?
C11 C12 H12 126.8 . . ?
N11 C13 C14 111.38(19) . . ?
N11 C13 H13 124.3 . . ?
C14 C13 H13 124.3 . . ?
C15 C14 C13 104.43(19) . . ?
C15 C14 H14 127.8 . . ?
C13 C14 H14 127.8 . . ?
N10 C15 C14 108.73(19) . . ?
N10 C15 H15 125.6 . . ?
C14 C15 H15 125.6 . . ?
N13 C16 C17 111.5(2) . . ?
N13 C16 H16 124.2 . . ?
C17 C16 H16 124.2 . . ?
C18 C17 C16 104.3(2) . . ?
C18 C17 H17 127.8 . . ?
C16 C17 H17 127.8 . . ?
N12 C18 C17 108.9(2) . . ?
N12 C18 H18 125.6 . . ?
C17 C18 H18 125.6 . . ?
N16 C19 C20 109.88(18) . . ?
N16 C19 H19 125.1 . . ?
C20 C19 H19 125.1 . . ?
C21 C20 C19 106.63(18) . . ?
C21 C20 N21 126.6(2) . . ?
C19 C20 N21 126.73(19) . . ?
N15 C21 C20 106.76(19) . . ?
N15 C21 H21 126.6 . . ?
C20 C21 H21 126.6 . . ?
N18 C22 C23 111.0(2) . . ?
N18 C22 H22 124.5 . . ?
C23 C22 H22 124.5 . . ?
C24 C23 C22 104.48(19) . . ?
C24 C23 H23 127.8 . . ?
C22 C23 H23 127.8 . . ?
N17 C24 C23 108.9(2) . . ?
N17 C24 H24 125.6 . . ?
C23 C24 H24 125.6 . . ?
N20 C25 C26 111.2(2) . . ?
N20 C25 H25 124.4 . . ?
C26 C25 H25 124.4 . . ?
C27 C26 C25 104.53(19) . . ?
C27 C26 H26 127.7 . . ?
C25 C26 H26 127.7 . . ?
N19 C27 C26 109.15(19) . . ?
N19 C27 H27 125.4 . . ?
C26 C27 H27 125.4 . . ?
N3 B1 N1 109.55(17) . . ?
N3 B1 N5 111.73(17) . . ?
N1 B1 N5 107.34(17) . . ?
N3 B1 H1 111.5(11) . . ?
N1 B1 H1 107.6(11) . . ?
N5 B1 H1 109.0(11) . . ?
N10 B2 N8 107.80(17) . . ?
N10 B2 N12 112.34(17) . . ?
N8 B2 N12 108.88(17) . . ?
N10 B2 H2 110.3(12) . . ?
N8 B2 H2 109.3(12) . . ?
N12 B2 H2 108.2(12) . . ?
N19 B3 N17 111.64(18) . . ?
N19 B3 N15 108.73(17) . . ?
N17 B3 N15 108.83(17) . . ?
N19 B3 H3 108.7(12) . . ?
N17 B3 H3 109.3(12) . . ?
N15 B3 H3 109.7(12) . . ?

_refine_diff_density_max         0.320
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.062



####################################################################### 
# 
# 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_Cmpd5
_audit_block_doi                 10.5517/ccdc.csd.cc2dr84l
_database_code_depnum_ccdc_archive 'CCDC 2226889'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Sm N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 N21 O6 Sm'
_chemical_formula_weight         924.47

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'
B B 0.0013 0.0007 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.324(15)
_cell_length_b                   13.756(10)
_cell_length_c                   28.833(15)
_cell_angle_alpha                90
_cell_angle_beta                 112.49(2)
_cell_angle_gamma                90
_cell_volume                     8913(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    302
_cell_measurement_theta_min      3.496
_cell_measurement_theta_max      40.95

_exptl_crystal_description       diamond
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             3688

_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.378

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41519
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.071
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8142
_reflns_number_gt                6773
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8142
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0268
_refine_ls_wR_factor_ref         0.0613
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
Sm1 Sm 0.68550(2) 0.58877(2) 0.62453(2) 0.01227(5) Uani 1 1 d . . . . .
O1 O 0.95799(9) 0.42686(16) 0.60639(9) 0.0345(6) Uani 1 1 d . . . . .
O2 O 0.88682(10) 0.31923(15) 0.58875(9) 0.0374(6) Uani 1 1 d . . . . .
O3 O 0.45052(9) 0.24210(15) 0.58599(9) 0.0340(6) Uani 1 1 d . . . . .
O4 O 0.43171(10) 0.39304(16) 0.59846(10) 0.0388(6) Uani 1 1 d . . . . .
O5 O 0.72607(10) 1.05588(15) 0.65785(8) 0.0308(5) Uani 1 1 d . . . . .
O6 O 0.63943(10) 1.09750(14) 0.65779(8) 0.0292(5) Uani 1 1 d . . . . .
N1 N 0.83208(10) 0.61356(16) 0.61763(9) 0.0162(5) Uani 1 1 d . . . . .
N2 N 0.78804(10) 0.54547(16) 0.61109(8) 0.0171(5) Uani 1 1 d . . . . .
N3 N 0.76446(10) 0.75624(16) 0.58325(8) 0.0167(5) Uani 1 1 d . . . . .
N4 N 0.70973(10) 0.71237(16) 0.56924(8) 0.0168(5) Uani 1 1 d . . . . .
N5 N 0.81406(10) 0.72808(16) 0.67784(8) 0.0156(5) Uani 1 1 d . . . . .
N6 N 0.77454(10) 0.67251(15) 0.69006(8) 0.0137(5) Uani 1 1 d . . . . .
N7 N 0.90655(11) 0.40244(19) 0.60014(10) 0.0252(6) Uani 1 1 d . . . . .
N8 N 0.61739(10) 0.34621(15) 0.61106(8) 0.0144(5) Uani 1 1 d . . . . .
N9 N 0.60688(10) 0.44217(16) 0.61902(8) 0.0157(5) Uani 1 1 d . . . . .
N10 N 0.72929(10) 0.34653(15) 0.65187(8) 0.0141(5) Uani 1 1 d . . . . .
N11 N 0.73800(10) 0.43811(15) 0.67260(8) 0.0141(5) Uani 1 1 d . . . . .
N12 N 0.67536(10) 0.37231(16) 0.55745(8) 0.0154(5) Uani 1 1 d . . . . .
N13 N 0.66989(10) 0.47135(16) 0.55208(8) 0.0150(5) Uani 1 1 d . . . . .
N14 N 0.46598(11) 0.32743(19) 0.59723(10) 0.0260(6) Uani 1 1 d . . . . .
N15 N 0.60916(10) 0.80285(16) 0.64787(8) 0.0150(5) Uani 1 1 d . . . . .
N16 N 0.66184(10) 0.77605(16) 0.64383(8) 0.0155(5) Uani 1 1 d . . . . .
N17 N 0.59373(10) 0.65010(16) 0.68874(8) 0.0162(5) Uani 1 1 d . . . . .
N18 N 0.64346(10) 0.59813(16) 0.69282(8) 0.0157(5) Uani 1 1 d . . . . .
N19 N 0.54109(10) 0.67718(16) 0.59396(8) 0.0158(5) Uani 1 1 d . . . . .
N20 N 0.57823(10) 0.63785(16) 0.57342(8) 0.0144(5) Uani 1 1 d . . . . .
N21 N 0.67552(11) 1.03598(17) 0.65585(9) 0.0218(6) Uani 1 1 d . . . . .
C1 C 0.81018(12) 0.4612(2) 0.60337(10) 0.0179(6) Uani 1 1 d . . . . .
H1A H 0.789828 0.400715 0.597422 0.021 Uiso 1 1 calc R U . . .
C2 C 0.86786(12) 0.4754(2) 0.60535(10) 0.0174(6) Uani 1 1 d . . . . .
C3 C 0.87979(12) 0.5727(2) 0.61432(10) 0.0183(6) Uani 1 1 d . . . . .
H3A H 0.915660 0.604776 0.617568 0.022 Uiso 1 1 calc R U . . .
C4 C 0.67334(14) 0.7653(2) 0.53058(10) 0.0210(7) Uani 1 1 d . . . . .
H4 H 0.632220 0.752278 0.512893 0.025 Uiso 1 1 calc R U . . .
C5 C 0.70398(14) 0.8421(2) 0.51988(11) 0.0274(8) Uani 1 1 d . . . . .
H5 H 0.688552 0.889859 0.494385 0.033 Uiso 1 1 calc R U . . .
C6 C 0.76101(14) 0.8335(2) 0.55401(11) 0.0234(7) Uani 1 1 d . . . . .
H6 H 0.793052 0.875559 0.556607 0.028 Uiso 1 1 calc R U . . .
C7 C 0.78202(12) 0.6992(2) 0.73667(10) 0.0182(6) Uani 1 1 d . . . . .
H7 H 0.760570 0.672392 0.755099 0.022 Uiso 1 1 calc R U . . .
C8 C 0.82520(13) 0.7711(2) 0.75477(11) 0.0235(7) Uani 1 1 d . . . . .
H8 H 0.838524 0.802247 0.786592 0.028 Uiso 1 1 calc R U . . .
C9 C 0.84415(13) 0.7869(2) 0.71643(11) 0.0233(7) Uani 1 1 d . . . . .
H9 H 0.873847 0.832308 0.717000 0.028 Uiso 1 1 calc R U . . .
C10 C 0.55162(12) 0.4450(2) 0.61712(10) 0.0180(6) Uani 1 1 d . . . . .
H10 H 0.531995 0.501780 0.621587 0.022 Uiso 1 1 calc R U . . .
C11 C 0.52654(12) 0.3527(2) 0.60764(11) 0.0171(6) Uani 1 1 d . . . . .
C12 C 0.56979(12) 0.2919(2) 0.60424(10) 0.0178(6) Uani 1 1 d . . . . .
H12 H 0.566245 0.223860 0.598148 0.021 Uiso 1 1 calc R U . . .
C13 C 0.78936(12) 0.4332(2) 0.71230(10) 0.0176(6) Uani 1 1 d . . . . .
H13 H 0.806762 0.486216 0.734105 0.021 Uiso 1 1 calc R U . . .
C14 C 0.81420(13) 0.3408(2) 0.71775(11) 0.0210(7) Uani 1 1 d . . . . .
H14 H 0.850435 0.318938 0.742839 0.025 Uiso 1 1 calc R U . . .
C15 C 0.77476(12) 0.2883(2) 0.67885(10) 0.0177(6) Uani 1 1 d . . . . .
H15 H 0.778828 0.221697 0.672032 0.021 Uiso 1 1 calc R U . . .
C16 C 0.66927(12) 0.4905(2) 0.50640(10) 0.0201(7) Uani 1 1 d . . . . .
H16 H 0.666283 0.553836 0.492553 0.024 Uiso 1 1 calc R U . . .
C17 C 0.67354(13) 0.4061(2) 0.48191(11) 0.0242(7) Uani 1 1 d . . . . .
H17 H 0.673804 0.400231 0.449162 0.029 Uiso 1 1 calc R U . . .
C18 C 0.67730(13) 0.3331(2) 0.51498(11) 0.0206(7) Uani 1 1 d . . . . .
H18 H 0.680714 0.265790 0.509203 0.025 Uiso 1 1 calc R U . . .
C19 C 0.69186(12) 0.85772(19) 0.64650(10) 0.0168(6) Uani 1 1 d . . . . .
H19 H 0.730195 0.862023 0.645141 0.020 Uiso 1 1 calc R U . . .
C20 C 0.65850(12) 0.93604(19) 0.65159(10) 0.0165(6) Uani 1 1 d . . . . .
C21 C 0.60617(12) 0.89933(19) 0.65213(10) 0.0161(6) Uani 1 1 d . . . . .
H21 H 0.574266 0.935309 0.654973 0.019 Uiso 1 1 calc R U . . .
C22 C 0.65717(13) 0.5451(2) 0.73459(10) 0.0211(7) Uani 1 1 d . . . . .
H22 H 0.689621 0.501003 0.746631 0.025 Uiso 1 1 calc R U . . .
C23 C 0.61801(14) 0.5628(2) 0.75811(11) 0.0265(7) Uani 1 1 d . . . . .
H23 H 0.618401 0.535104 0.788408 0.032 Uiso 1 1 calc R U . . .
C24 C 0.57847(14) 0.6295(2) 0.72771(11) 0.0260(7) Uani 1 1 d . . . . .
H24 H 0.545666 0.656660 0.733385 0.031 Uiso 1 1 calc R U . . .
C25 C 0.54247(12) 0.60832(19) 0.52737(10) 0.0171(6) Uani 1 1 d . . . . .
H25 H 0.555989 0.577588 0.504169 0.020 Uiso 1 1 calc R U . . .
C26 C 0.48296(13) 0.6284(2) 0.51787(11) 0.0184(6) Uani 1 1 d . . . . .
H26 H 0.449193 0.614911 0.488227 0.022 Uiso 1 1 calc R U . . .
C27 C 0.48419(13) 0.6722(2) 0.56107(11) 0.0196(7) Uani 1 1 d . . . . .
H27 H 0.450505 0.695204 0.566812 0.024 Uiso 1 1 calc R U . . .
B1 B 0.82087(15) 0.7210(2) 0.62682(13) 0.0190(7) Uani 1 1 d . . . . .
H1 H 0.8589(13) 0.767(2) 0.6276(10) 0.029 Uiso 1 1 d . U . . .
B2 B 0.67529(14) 0.3178(2) 0.60438(12) 0.0156(7) Uani 1 1 d . . . . .
H2 H 0.6746(12) 0.240(2) 0.5979(10) 0.023 Uiso 1 1 d . U . . .
B3 B 0.56352(14) 0.7246(2) 0.64634(12) 0.0162(7) Uani 1 1 d . . . . .
H3 H 0.5282(12) 0.761(2) 0.6538(10) 0.024 Uiso 1 1 d . U . . .


_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
Sm1 N6 2.541(2) . ?
Sm1 N18 2.546(2) . ?
Sm1 N11 2.548(2) . ?
Sm1 N20 2.548(3) . ?
Sm1 N4 2.549(2) . ?
Sm1 N13 2.551(2) . ?
Sm1 N2 2.732(3) . ?
Sm1 N9 2.742(3) . ?
Sm1 N16 2.743(3) . ?
O1 N7 1.240(3) . ?
O2 N7 1.236(3) . ?
O3 N14 1.237(3) . ?
O4 N14 1.238(3) . ?
O5 N21 1.239(3) . ?
O6 N21 1.236(3) . ?
N1 C3 1.326(3) . ?
N1 N2 1.381(3) . ?
N1 B1 1.545(4) . ?
N2 C1 1.332(3) . ?
N3 C6 1.340(4) . ?
N3 N4 1.374(3) . ?
N3 B1 1.541(4) . ?
N4 C4 1.343(3) . ?
N5 C9 1.344(3) . ?
N5 N6 1.375(3) . ?
N5 B1 1.545(4) . ?
N6 C7 1.337(3) . ?
N7 C2 1.423(4) . ?
N8 C12 1.328(3) . ?
N8 N9 1.380(3) . ?
N8 B2 1.543(4) . ?
N9 C10 1.325(4) . ?
N10 C15 1.346(3) . ?
N10 N11 1.376(3) . ?
N10 B2 1.543(4) . ?
N11 C13 1.335(3) . ?
N12 C18 1.355(3) . ?
N12 N13 1.372(3) . ?
N12 B2 1.548(4) . ?
N13 C16 1.338(3) . ?
N14 C11 1.429(4) . ?
N15 C21 1.337(3) . ?
N15 N16 1.380(3) . ?
N15 B3 1.535(4) . ?
N16 C19 1.326(3) . ?
N17 C24 1.341(4) . ?
N17 N18 1.371(3) . ?
N17 B3 1.548(4) . ?
N18 C22 1.336(4) . ?
N19 C27 1.347(3) . ?
N19 N20 1.367(3) . ?
N19 B3 1.541(4) . ?
N20 C25 1.342(3) . ?
N21 C20 1.427(4) . ?
C1 C2 1.396(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.372(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.393(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.391(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.368(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.389(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.383(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.363(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.390(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.394(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.374(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.11(3) . ?
B2 H2 1.08(3) . ?
B3 H3 1.09(3) . ?

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
N6 Sm1 N18 83.25(8) . . ?
N6 Sm1 N11 81.78(8) . . ?
N18 Sm1 N11 83.48(8) . . ?
N6 Sm1 N20 134.66(8) . . ?
N18 Sm1 N20 78.96(8) . . ?
N11 Sm1 N20 135.99(7) . . ?
N6 Sm1 N4 80.06(8) . . ?
N18 Sm1 N4 135.03(7) . . ?
N11 Sm1 N4 134.02(8) . . ?
N20 Sm1 N4 83.81(8) . . ?
N6 Sm1 N13 135.50(7) . . ?
N18 Sm1 N13 133.42(7) . . ?
N11 Sm1 N13 79.45(8) . . ?
N20 Sm1 N13 84.00(7) . . ?
N4 Sm1 N13 84.71(8) . . ?
N6 Sm1 N2 68.87(8) . . ?
N18 Sm1 N2 141.21(7) . . ?
N11 Sm1 N2 66.74(7) . . ?
N20 Sm1 N2 139.82(7) . . ?
N4 Sm1 N2 67.34(7) . . ?
N13 Sm1 N2 66.66(7) . . ?
N6 Sm1 N9 138.93(7) . . ?
N18 Sm1 N9 66.69(7) . . ?
N11 Sm1 N9 68.07(8) . . ?
N20 Sm1 N9 67.92(8) . . ?
N4 Sm1 N9 141.01(7) . . ?
N13 Sm1 N9 66.72(7) . . ?
N2 Sm1 N9 119.06(8) . . ?
N6 Sm1 N16 66.97(7) . . ?
N18 Sm1 N16 67.54(7) . . ?
N11 Sm1 N16 138.95(7) . . ?
N20 Sm1 N16 67.70(7) . . ?
N4 Sm1 N16 67.49(8) . . ?
N13 Sm1 N16 141.60(7) . . ?
N2 Sm1 N16 120.49(7) . . ?
N9 Sm1 N16 120.45(8) . . ?
C3 N1 N2 110.9(2) . . ?
C3 N1 B1 129.5(2) . . ?
N2 N1 B1 119.6(2) . . ?
C1 N2 N1 105.7(2) . . ?
C1 N2 Sm1 131.52(18) . . ?
N1 N2 Sm1 122.38(16) . . ?
C6 N3 N4 110.1(2) . . ?
C6 N3 B1 125.7(3) . . ?
N4 N3 B1 124.2(2) . . ?
C4 N4 N3 105.2(2) . . ?
C4 N4 Sm1 130.13(19) . . ?
N3 N4 Sm1 122.60(17) . . ?
C9 N5 N6 109.6(2) . . ?
C9 N5 B1 127.1(2) . . ?
N6 N5 B1 123.3(2) . . ?
C7 N6 N5 105.4(2) . . ?
C7 N6 Sm1 128.42(18) . . ?
N5 N6 Sm1 122.82(16) . . ?
O2 N7 O1 123.8(3) . . ?
O2 N7 C2 118.4(2) . . ?
O1 N7 C2 117.7(3) . . ?
C12 N8 N9 110.9(2) . . ?
C12 N8 B2 128.6(2) . . ?
N9 N8 B2 119.9(2) . . ?
C10 N9 N8 105.7(2) . . ?
C10 N9 Sm1 130.95(19) . . ?
N8 N9 Sm1 122.93(16) . . ?
C15 N10 N11 109.8(2) . . ?
C15 N10 B2 126.3(2) . . ?
N11 N10 B2 123.9(2) . . ?
C13 N11 N10 105.3(2) . . ?
C13 N11 Sm1 128.13(18) . . ?
N10 N11 Sm1 123.14(16) . . ?
C18 N12 N13 109.2(2) . . ?
C18 N12 B2 127.5(2) . . ?
N13 N12 B2 123.2(2) . . ?
C16 N13 N12 105.7(2) . . ?
C16 N13 Sm1 128.60(19) . . ?
N12 N13 Sm1 123.97(16) . . ?
O3 N14 O4 124.0(3) . . ?
O3 N14 C11 118.1(3) . . ?
O4 N14 C11 117.9(2) . . ?
C21 N15 N16 111.0(2) . . ?
C21 N15 B3 129.4(2) . . ?
N16 N15 B3 119.7(2) . . ?
C19 N16 N15 106.1(2) . . ?
C19 N16 Sm1 130.83(19) . . ?
N15 N16 Sm1 122.79(16) . . ?
C24 N17 N18 109.6(2) . . ?
C24 N17 B3 126.9(2) . . ?
N18 N17 B3 123.3(2) . . ?
C22 N18 N17 105.6(2) . . ?
C22 N18 Sm1 129.34(19) . . ?
N17 N18 Sm1 124.23(16) . . ?
C27 N19 N20 110.3(2) . . ?
C27 N19 B3 126.5(2) . . ?
N20 N19 B3 123.2(2) . . ?
C25 N20 N19 105.2(2) . . ?
C25 N20 Sm1 128.67(18) . . ?
N19 N20 Sm1 123.67(16) . . ?
O6 N21 O5 123.8(2) . . ?
O6 N21 C20 118.4(3) . . ?
O5 N21 C20 117.8(2) . . ?
N2 C1 C2 109.6(3) . . ?
N2 C1 H1A 125.2 . . ?
C2 C1 H1A 125.2 . . ?
C3 C2 C1 106.3(2) . . ?
C3 C2 N7 127.4(3) . . ?
C1 C2 N7 126.3(3) . . ?
N1 C3 C2 107.4(3) . . ?
N1 C3 H3A 126.3 . . ?
C2 C3 H3A 126.3 . . ?
N4 C4 C5 110.9(3) . . ?
N4 C4 H4 124.6 . . ?
C5 C4 H4 124.6 . . ?
C6 C5 C4 104.9(3) . . ?
C6 C5 H5 127.5 . . ?
C4 C5 H5 127.5 . . ?
N3 C6 C5 108.9(3) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 111.4(3) . . ?
N6 C7 H7 124.3 . . ?
C8 C7 H7 124.3 . . ?
C9 C8 C7 104.4(3) . . ?
C9 C8 H8 127.8 . . ?
C7 C8 H8 127.8 . . ?
N5 C9 C8 109.1(3) . . ?
N5 C9 H9 125.4 . . ?
C8 C9 H9 125.4 . . ?
N9 C10 C11 110.1(3) . . ?
N9 C10 H10 124.9 . . ?
C11 C10 H10 124.9 . . ?
C12 C11 C10 106.2(3) . . ?
C12 C11 N14 126.3(3) . . ?
C10 C11 N14 127.1(3) . . ?
N8 C12 C11 107.1(2) . . ?
N8 C12 H12 126.4 . . ?
C11 C12 H12 126.4 . . ?
N11 C13 C14 111.5(3) . . ?
N11 C13 H13 124.2 . . ?
C14 C13 H13 124.2 . . ?
C15 C14 C13 104.6(3) . . ?
C15 C14 H14 127.7 . . ?
C13 C14 H14 127.7 . . ?
N10 C15 C14 108.8(3) . . ?
N10 C15 H15 125.6 . . ?
C14 C15 H15 125.6 . . ?
N13 C16 C17 111.3(3) . . ?
N13 C16 H16 124.4 . . ?
C17 C16 H16 124.4 . . ?
C18 C17 C16 105.0(3) . . ?
C18 C17 H17 127.5 . . ?
C16 C17 H17 127.5 . . ?
N12 C18 C17 108.8(3) . . ?
N12 C18 H18 125.6 . . ?
C17 C18 H18 125.6 . . ?
N16 C19 C20 109.4(3) . . ?
N16 C19 H19 125.3 . . ?
C20 C19 H19 125.3 . . ?
C21 C20 C19 107.3(2) . . ?
C21 C20 N21 126.3(3) . . ?
C19 C20 N21 126.4(3) . . ?
N15 C21 C20 106.3(2) . . ?
N15 C21 H21 126.9 . . ?
C20 C21 H21 126.9 . . ?
N18 C22 C23 111.3(3) . . ?
N18 C22 H22 124.3 . . ?
C23 C22 H22 124.3 . . ?
C24 C23 C22 104.4(3) . . ?
C24 C23 H23 127.8 . . ?
C22 C23 H23 127.8 . . ?
N17 C24 C23 108.9(3) . . ?
N17 C24 H24 125.5 . . ?
C23 C24 H24 125.5 . . ?
N20 C25 C26 111.4(3) . . ?
N20 C25 H25 124.3 . . ?
C26 C25 H25 124.3 . . ?
C27 C26 C25 104.4(3) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 108.7(3) . . ?
N19 C27 H27 125.7 . . ?
C26 C27 H27 125.7 . . ?
N3 B1 N1 108.7(2) . . ?
N3 B1 N5 111.7(2) . . ?
N1 B1 N5 108.3(2) . . ?
N3 B1 H1 108.1(15) . . ?
N1 B1 H1 110.3(15) . . ?
N5 B1 H1 109.7(14) . . ?
N8 B2 N10 109.4(2) . . ?
N8 B2 N12 107.0(2) . . ?
N10 B2 N12 111.5(2) . . ?
N8 B2 H2 108.5(15) . . ?
N10 B2 H2 111.0(15) . . ?
N12 B2 H2 109.4(15) . . ?
N15 B3 N19 107.8(2) . . ?
N15 B3 N17 108.8(2) . . ?
N19 B3 N17 112.1(2) . . ?
N15 B3 H3 106.8(15) . . ?
N19 B3 H3 112.4(15) . . ?
N17 B3 H3 108.7(14) . . ?

_refine_diff_density_max         0.446
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.075



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Cmpd3
_audit_block_doi                 10.5517/ccdc.csd.cc2dr82j
_database_code_depnum_ccdc_archive 'CCDC 2226887'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 Pr N21 O6 [+ solvent]'
_chemical_formula_sum            'C27 H27 B3 N21 O6 Pr'
_chemical_formula_weight         915.03

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'
B B 0.0013 0.0007 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   24.369(6)
_cell_length_b                   13.783(3)
_cell_length_c                   28.792(7)
_cell_angle_alpha                90
_cell_angle_beta                 112.453(8)
_cell_angle_gamma                90
_cell_volume                     8937(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    719
_cell_measurement_theta_min      3.491
_cell_measurement_theta_max      41.78

_exptl_crystal_description       diamond
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             3664

_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.341
_exptl_crystal_size_min          0.221
_exptl_absorpt_coefficient_mu    1.151

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45388
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.029
_diffrn_reflns_theta_max         26.377
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9125
_reflns_number_gt                7895
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          SQUEEZE

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0313P)²+4.1757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9125
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Pr1 Pr 0.68568(2) 0.41156(2) 0.62447(2) 0.01256(4) Uani 1 1 d . . . . .
O1 O 0.88734(9) 0.67983(13) 0.58923(8) 0.0422(5) Uani 1 1 d . . . . .
O2 O 0.95820(8) 0.57242(14) 0.60645(8) 0.0377(5) Uani 1 1 d . . . . .
O3 O 0.72550(8) -0.05489(13) 0.65849(7) 0.0340(5) Uani 1 1 d . . . . .
O4 O 0.63879(8) -0.09650(12) 0.65788(7) 0.0314(4) Uani 1 1 d . . . . .
O5 O 0.45117(8) 0.75881(13) 0.58560(7) 0.0362(5) Uani 1 1 d . . . . .
O6 O 0.43200(8) 0.60846(14) 0.59725(8) 0.0403(5) Uani 1 1 d . . . . .
N1 N 0.83236(8) 0.38623(13) 0.61752(7) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.78859(8) 0.45443(13) 0.61088(7) 0.0161(4) Uani 1 1 d . . . . .
N3 N 0.76586(8) 0.24278(13) 0.58351(7) 0.0178(4) Uani 1 1 d . . . . .
N4 N 0.71107(8) 0.28617(13) 0.56836(7) 0.0173(4) Uani 1 1 d . . . . .
N5 N 0.81486(8) 0.27109(13) 0.67790(7) 0.0170(4) Uani 1 1 d . . . . .
N6 N 0.77623(8) 0.32671(13) 0.69075(7) 0.0156(4) Uani 1 1 d . . . . .
N7 N 0.90704(10) 0.59653(15) 0.60007(8) 0.0285(5) Uani 1 1 d . . . . .
N8 N 0.60876(8) 0.19723(13) 0.64776(7) 0.0161(4) Uani 1 1 d . . . . .
N9 N 0.66137(8) 0.22398(13) 0.64390(7) 0.0163(4) Uani 1 1 d . . . . .
N10 N 0.59247(8) 0.34871(13) 0.68866(7) 0.0173(4) Uani 1 1 d . . . . .
N11 N 0.64214(8) 0.40099(13) 0.69382(7) 0.0170(4) Uani 1 1 d . . . . .
N12 N 0.54008(8) 0.32240(13) 0.59379(7) 0.0163(4) Uani 1 1 d . . . . .
N13 N 0.57684(8) 0.36130(13) 0.57269(7) 0.0157(4) Uani 1 1 d . . . . .
N14 N 0.67491(10) -0.03532(14) 0.65626(7) 0.0248(5) Uani 1 1 d . . . . .
N15 N 0.61773(8) 0.65529(13) 0.61118(7) 0.0151(4) Uani 1 1 d . . . . .
N16 N 0.60690(8) 0.55932(13) 0.61894(7) 0.0165(4) Uani 1 1 d . . . . .
N17 N 0.72947(8) 0.65588(13) 0.65198(7) 0.0154(4) Uani 1 1 d . . . . .
N18 N 0.73856(8) 0.56506(13) 0.67306(7) 0.0160(4) Uani 1 1 d . . . . .
N19 N 0.67612(8) 0.63090(13) 0.55740(7) 0.0167(4) Uani 1 1 d . . . . .
N20 N 0.66992(8) 0.53231(13) 0.55138(7) 0.0161(4) Uani 1 1 d . . . . .
N21 N 0.46641(9) 0.67336(16) 0.59644(8) 0.0285(5) Uani 1 1 d . . . . .
C1 C 0.81066(10) 0.53818(16) 0.60327(8) 0.0188(5) Uani 1 1 d . . . . .
H1A H 0.790410 0.598614 0.597536 0.023 Uiso 1 1 calc R U . . .
C2 C 0.86791(10) 0.52421(17) 0.60496(8) 0.0190(5) Uani 1 1 d . . . . .
C3 C 0.88018(10) 0.42703(16) 0.61407(9) 0.0192(5) Uani 1 1 d . . . . .
H3A H 0.915997 0.395080 0.617298 0.023 Uiso 1 1 calc R U . . .
C4 C 0.67524(11) 0.23255(17) 0.53007(8) 0.0238(5) Uani 1 1 d . . . . .
H4 H 0.634236 0.245387 0.512095 0.029 Uiso 1 1 calc R U . . .
C5 C 0.70596(12) 0.15535(18) 0.51999(9) 0.0286(6) Uani 1 1 d . . . . .
H5 H 0.690852 0.107078 0.494732 0.034 Uiso 1 1 calc R U . . .
C6 C 0.76279(12) 0.16465(17) 0.55464(9) 0.0249(6) Uani 1 1 d . . . . .
H6 H 0.794919 0.122627 0.557782 0.030 Uiso 1 1 calc R U . . .
C7 C 0.78342(10) 0.29938(17) 0.73729(8) 0.0190(5) Uani 1 1 d . . . . .
H7 H 0.762260 0.326189 0.755946 0.023 Uiso 1 1 calc R U . . .
C8 C 0.82595(11) 0.22654(18) 0.75483(9) 0.0246(5) Uani 1 1 d . . . . .
H8 H 0.839043 0.194688 0.786468 0.030 Uiso 1 1 calc R U . . .
C9 C 0.84474(11) 0.21105(17) 0.71615(9) 0.0242(5) Uani 1 1 d . . . . .
H9 H 0.874035 0.165419 0.716333 0.029 Uiso 1 1 calc R U . . .
C10 C 0.69154(10) 0.14281(16) 0.64677(8) 0.0175(5) Uani 1 1 d . . . . .
H10 H 0.729907 0.138678 0.645601 0.021 Uiso 1 1 calc R U . . .
C11 C 0.65797(10) 0.06402(15) 0.65179(8) 0.0177(5) Uani 1 1 d . . . . .
C12 C 0.60573(10) 0.10120(15) 0.65207(8) 0.0177(5) Uani 1 1 d . . . . .
H12 H 0.573749 0.065497 0.654789 0.021 Uiso 1 1 calc R U . . .
C13 C 0.65512(11) 0.45336(17) 0.73543(8) 0.0217(5) Uani 1 1 d . . . . .
H13 H 0.687612 0.497124 0.747947 0.026 Uiso 1 1 calc R U . . .
C14 C 0.61511(12) 0.43596(19) 0.75831(10) 0.0306(6) Uani 1 1 d . . . . .
H14 H 0.614792 0.463592 0.788433 0.037 Uiso 1 1 calc R U . . .
C15 C 0.57603(12) 0.36941(18) 0.72724(9) 0.0266(6) Uani 1 1 d . . . . .
H15 H 0.542812 0.342438 0.732218 0.032 Uiso 1 1 calc R U . . .
C16 C 0.54088(10) 0.39101(16) 0.52679(9) 0.0191(5) Uani 1 1 d . . . . .
H16 H 0.554156 0.421376 0.503342 0.023 Uiso 1 1 calc R U . . .
C17 C 0.48189(10) 0.37180(17) 0.51789(9) 0.0206(5) Uani 1 1 d . . . . .
H17 H 0.448071 0.385929 0.488442 0.025 Uiso 1 1 calc R U . . .
C18 C 0.48319(10) 0.32774(16) 0.56118(9) 0.0200(5) Uani 1 1 d . . . . .
H18 H 0.449628 0.304931 0.567074 0.024 Uiso 1 1 calc R U . . .
C19 C 0.55180(10) 0.55645(17) 0.61672(8) 0.0189(5) Uani 1 1 d . . . . .
H19 H 0.532077 0.499753 0.621025 0.023 Uiso 1 1 calc R U . . .
C20 C 0.52685(10) 0.64904(17) 0.60712(9) 0.0200(5) Uani 1 1 d . . . . .
C21 C 0.57026(10) 0.71004(16) 0.60410(8) 0.0189(5) Uani 1 1 d . . . . .
H21 H 0.566890 0.777981 0.598120 0.023 Uiso 1 1 calc R U . . .
C22 C 0.78993(10) 0.56962(17) 0.71251(8) 0.0194(5) Uani 1 1 d . . . . .
H22 H 0.807395 0.516777 0.734342 0.023 Uiso 1 1 calc R U . . .
C23 C 0.81472(11) 0.66218(17) 0.71753(9) 0.0226(5) Uani 1 1 d . . . . .
H23 H 0.851008 0.684161 0.742389 0.027 Uiso 1 1 calc R U . . .
C24 C 0.77507(10) 0.71434(16) 0.67864(8) 0.0189(5) Uani 1 1 d . . . . .
H24 H 0.779024 0.780723 0.671592 0.023 Uiso 1 1 calc R U . . .
C25 C 0.66973(10) 0.51420(18) 0.50570(8) 0.0215(5) Uani 1 1 d . . . . .
H25 H 0.666444 0.451218 0.491474 0.026 Uiso 1 1 calc R U . . .
C26 C 0.67493(12) 0.59909(18) 0.48162(9) 0.0275(6) Uani 1 1 d . . . . .
H26 H 0.675788 0.605628 0.449055 0.033 Uiso 1 1 calc R U . . .
C27 C 0.67855(11) 0.67134(18) 0.51549(9) 0.0228(5) Uani 1 1 d . . . . .
H27 H 0.682180 0.738722 0.510311 0.027 Uiso 1 1 calc R U . . .
B1 B 0.82179(12) 0.27878(19) 0.62685(10) 0.0185(6) Uani 1 1 d . . . . .
H1 H 0.8602(11) 0.2322(18) 0.6269(9) 0.028 Uiso 1 1 d . U . . .
B2 B 0.56262(12) 0.27482(19) 0.64614(10) 0.0181(5) Uani 1 1 d . . . . .
H2 H 0.5275(11) 0.2428(18) 0.6534(9) 0.027 Uiso 1 1 d . U . . .
B3 B 0.67574(12) 0.68398(19) 0.60468(10) 0.0170(5) Uani 1 1 d . . . . .
H3 H 0.6750(10) 0.7601(18) 0.5991(9) 0.026 Uiso 1 1 d . U . . .


_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
Pr1 N6 2.5810(18) . ?
Pr1 N18 2.5916(18) . ?
Pr1 N13 2.5918(19) . ?
Pr1 N20 2.5939(19) . ?
Pr1 N4 2.5967(19) . ?
Pr1 N11 2.598(2) . ?
Pr1 N2 2.7461(19) . ?
Pr1 N9 2.7570(19) . ?
Pr1 N16 2.7612(19) . ?
O1 N7 1.237(3) . ?
O2 N7 1.234(3) . ?
O3 N14 1.240(3) . ?
O4 N14 1.232(3) . ?
O5 N21 1.238(3) . ?
O6 N21 1.233(3) . ?
N1 C3 1.331(3) . ?
N1 N2 1.379(3) . ?
N1 B1 1.544(3) . ?
N2 C1 1.327(3) . ?
N3 C6 1.345(3) . ?
N3 N4 1.373(3) . ?
N3 B1 1.537(3) . ?
N4 C4 1.338(3) . ?
N5 C9 1.347(3) . ?
N5 N6 1.370(2) . ?
N5 B1 1.546(3) . ?
N6 C7 1.337(3) . ?
N7 C2 1.423(3) . ?
N8 C12 1.334(3) . ?
N8 N9 1.379(3) . ?
N8 B2 1.540(3) . ?
N9 C10 1.324(3) . ?
N10 C15 1.347(3) . ?
N10 N11 1.367(3) . ?
N10 B2 1.544(3) . ?
N11 C13 1.329(3) . ?
N12 C18 1.347(3) . ?
N12 N13 1.369(3) . ?
N12 B2 1.540(3) . ?
N13 C16 1.341(3) . ?
N14 C11 1.422(3) . ?
N15 C21 1.330(3) . ?
N15 N16 1.384(2) . ?
N15 B3 1.546(3) . ?
N16 C19 1.320(3) . ?
N17 C24 1.350(3) . ?
N17 N18 1.372(2) . ?
N17 B3 1.535(3) . ?
N18 C22 1.332(3) . ?
N19 C27 1.351(3) . ?
N19 N20 1.371(3) . ?
N19 B3 1.549(3) . ?
N20 C25 1.337(3) . ?
N21 C20 1.425(3) . ?
C1 C2 1.391(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.376(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.392(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.373(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.400(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.378(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.386(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.395(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.370(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.373(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
B1 H1 1.13(2) . ?
B2 H2 1.05(3) . ?
B3 H3 1.06(2) . ?

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
N6 Pr1 N18 82.09(6) . . ?
N6 Pr1 N13 134.61(6) . . ?
N18 Pr1 N13 135.83(6) . . ?
N6 Pr1 N20 135.27(6) . . ?
N18 Pr1 N20 78.65(6) . . ?
N13 Pr1 N20 84.43(6) . . ?
N6 Pr1 N4 79.56(6) . . ?
N18 Pr1 N4 133.76(6) . . ?
N13 Pr1 N4 84.20(6) . . ?
N20 Pr1 N4 85.35(6) . . ?
N6 Pr1 N11 83.75(6) . . ?
N18 Pr1 N11 84.02(6) . . ?
N13 Pr1 N11 78.37(6) . . ?
N20 Pr1 N11 133.00(6) . . ?
N4 Pr1 N11 134.83(6) . . ?
N6 Pr1 N2 68.50(6) . . ?
N18 Pr1 N2 66.95(6) . . ?
N13 Pr1 N2 139.93(6) . . ?
N20 Pr1 N2 66.84(6) . . ?
N4 Pr1 N2 66.86(6) . . ?
N11 Pr1 N2 141.69(6) . . ?
N6 Pr1 N9 67.32(6) . . ?
N18 Pr1 N9 139.21(6) . . ?
N13 Pr1 N9 67.30(5) . . ?
N20 Pr1 N9 142.14(6) . . ?
N4 Pr1 N9 67.84(6) . . ?
N11 Pr1 N9 66.99(6) . . ?
N2 Pr1 N9 120.62(5) . . ?
N6 Pr1 N16 139.12(6) . . ?
N18 Pr1 N16 67.69(6) . . ?
N13 Pr1 N16 68.14(6) . . ?
N20 Pr1 N16 66.16(6) . . ?
N4 Pr1 N16 141.31(6) . . ?
N11 Pr1 N16 66.84(6) . . ?
N2 Pr1 N16 119.06(6) . . ?
N9 Pr1 N16 120.31(6) . . ?
C3 N1 N2 110.77(18) . . ?
C3 N1 B1 128.8(2) . . ?
N2 N1 B1 120.40(18) . . ?
C1 N2 N1 105.96(18) . . ?
C1 N2 Pr1 131.36(15) . . ?
N1 N2 Pr1 122.26(13) . . ?
C6 N3 N4 109.54(19) . . ?
C6 N3 B1 125.7(2) . . ?
N4 N3 B1 124.78(18) . . ?
C4 N4 N3 105.70(19) . . ?
C4 N4 Pr1 130.16(16) . . ?
N3 N4 Pr1 121.74(13) . . ?
C9 N5 N6 109.60(19) . . ?
C9 N5 B1 126.7(2) . . ?
N6 N5 B1 123.66(17) . . ?
C7 N6 N5 105.80(18) . . ?
C7 N6 Pr1 128.04(15) . . ?
N5 N6 Pr1 122.38(13) . . ?
O2 N7 O1 124.0(2) . . ?
O2 N7 C2 118.3(2) . . ?
O1 N7 C2 117.7(2) . . ?
C12 N8 N9 111.04(18) . . ?
C12 N8 B2 128.8(2) . . ?
N9 N8 B2 120.18(18) . . ?
C10 N9 N8 106.28(18) . . ?
C10 N9 Pr1 130.38(15) . . ?
N8 N9 Pr1 123.07(13) . . ?
C15 N10 N11 109.18(19) . . ?
C15 N10 B2 126.5(2) . . ?
N11 N10 B2 124.27(18) . . ?
C13 N11 N10 106.27(19) . . ?
C13 N11 Pr1 129.46(16) . . ?
N10 N11 Pr1 123.41(13) . . ?
C18 N12 N13 110.06(18) . . ?
C18 N12 B2 126.4(2) . . ?
N13 N12 B2 123.49(18) . . ?
C16 N13 N12 105.36(18) . . ?
C16 N13 Pr1 128.71(15) . . ?
N12 N13 Pr1 123.28(13) . . ?
O4 N14 O3 124.0(2) . . ?
O4 N14 C11 118.4(2) . . ?
O3 N14 C11 117.6(2) . . ?
C21 N15 N16 111.02(18) . . ?
C21 N15 B3 128.18(19) . . ?
N16 N15 B3 120.24(17) . . ?
C19 N16 N15 105.90(18) . . ?
C19 N16 Pr1 130.73(15) . . ?
N15 N16 Pr1 122.89(13) . . ?
C24 N17 N18 109.54(17) . . ?
C24 N17 B3 126.29(19) . . ?
N18 N17 B3 124.16(17) . . ?
C22 N18 N17 105.93(17) . . ?
C22 N18 Pr1 127.61(14) . . ?
N17 N18 Pr1 122.90(13) . . ?
C27 N19 N20 109.66(19) . . ?
C27 N19 B3 127.4(2) . . ?
N20 N19 B3 122.81(18) . . ?
C25 N20 N19 105.56(18) . . ?
C25 N20 Pr1 128.47(15) . . ?
N19 N20 Pr1 123.95(13) . . ?
O6 N21 O5 123.7(2) . . ?
O6 N21 C20 118.7(2) . . ?
O5 N21 C20 117.6(2) . . ?
N2 C1 C2 109.8(2) . . ?
N2 C1 H1A 125.1 . . ?
C2 C1 H1A 125.1 . . ?
C3 C2 C1 106.5(2) . . ?
C3 C2 N7 126.6(2) . . ?
C1 C2 N7 126.9(2) . . ?
N1 C3 C2 107.0(2) . . ?
N1 C3 H3A 126.5 . . ?
C2 C3 H3A 126.5 . . ?
N4 C4 C5 111.1(2) . . ?
N4 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
C6 C5 C4 104.5(2) . . ?
C6 C5 H5 127.7 . . ?
C4 C5 H5 127.7 . . ?
N3 C6 C5 109.1(2) . . ?
N3 C6 H6 125.4 . . ?
C5 C6 H6 125.4 . . ?
N6 C7 C8 111.2(2) . . ?
N6 C7 H7 124.4 . . ?
C8 C7 H7 124.4 . . ?
C9 C8 C7 104.5(2) . . ?
C9 C8 H8 127.7 . . ?
C7 C8 H8 127.7 . . ?
N5 C9 C8 108.9(2) . . ?
N5 C9 H9 125.5 . . ?
C8 C9 H9 125.5 . . ?
N9 C10 C11 109.2(2) . . ?
N9 C10 H10 125.4 . . ?
C11 C10 H10 125.4 . . ?
C12 C11 C10 106.9(2) . . ?
C12 C11 N14 126.6(2) . . ?
C10 C11 N14 126.5(2) . . ?
N8 C12 C11 106.6(2) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N11 C13 C14 111.4(2) . . ?
N11 C13 H13 124.3 . . ?
C14 C13 H13 124.3 . . ?
C15 C14 C13 104.1(2) . . ?
C15 C14 H14 128.0 . . ?
C13 C14 H14 128.0 . . ?
N10 C15 C14 109.1(2) . . ?
N10 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
N13 C16 C17 111.4(2) . . ?
N13 C16 H16 124.3 . . ?
C17 C16 H16 124.3 . . ?
C18 C17 C16 104.7(2) . . ?
C18 C17 H17 127.7 . . ?
C16 C17 H17 127.7 . . ?
N12 C18 C17 108.5(2) . . ?
N12 C18 H18 125.8 . . ?
C17 C18 H18 125.8 . . ?
N16 C19 C20 109.9(2) . . ?
N16 C19 H19 125.0 . . ?
C20 C19 H19 125.0 . . ?
C21 C20 C19 106.5(2) . . ?
C21 C20 N21 126.7(2) . . ?
C19 C20 N21 126.5(2) . . ?
N15 C21 C20 106.7(2) . . ?
N15 C21 H21 126.6 . . ?
C20 C21 H21 126.6 . . ?
N18 C22 C23 111.1(2) . . ?
N18 C22 H22 124.4 . . ?
C23 C22 H22 124.4 . . ?
C24 C23 C22 104.6(2) . . ?
C24 C23 H23 127.7 . . ?
C22 C23 H23 127.7 . . ?
N17 C24 C23 108.8(2) . . ?
N17 C24 H24 125.6 . . ?
C23 C24 H24 125.6 . . ?
N20 C25 C26 111.5(2) . . ?
N20 C25 H25 124.2 . . ?
C26 C25 H25 124.2 . . ?
C27 C26 C25 104.5(2) . . ?
C27 C26 H26 127.8 . . ?
C25 C26 H26 127.8 . . ?
N19 C27 C26 108.8(2) . . ?
N19 C27 H27 125.6 . . ?
C26 C27 H27 125.6 . . ?
N3 B1 N1 108.88(19) . . ?
N3 B1 N5 111.39(19) . . ?
N1 B1 N5 108.50(19) . . ?
N3 B1 H1 107.1(12) . . ?
N1 B1 H1 110.5(13) . . ?
N5 B1 H1 110.4(12) . . ?
N8 B2 N12 107.99(19) . . ?
N8 B2 N10 108.45(18) . . ?
N12 B2 N10 112.28(19) . . ?
N8 B2 H2 110.0(14) . . ?
N12 B2 H2 111.1(13) . . ?
N10 B2 H2 107.0(13) . . ?
N17 B3 N15 109.73(19) . . ?
N17 B3 N19 111.79(19) . . ?
N15 B3 N19 107.35(18) . . ?
N17 B3 H3 110.1(13) . . ?
N15 B3 H3 107.9(13) . . ?
N19 B3 H3 109.8(13) . . ?

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.069



_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_Cmpd5b
_audit_block_doi                 10.5517/ccdc.csd.cc2dr85m
_database_code_depnum_ccdc_archive 'CCDC 2226890'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-wwpbt 2023
loop_
_audit_author_name
_audit_author_address
'Christopher Hossack'
;The George Washington University
United States of America
;
_audit_update_record             
;
2022-12-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H27 B3 N21 O6 Sm, 7(C6 H6)'
_chemical_formula_sum            'C69 H69 B3 N21 O6 Sm'
_chemical_formula_weight         1471.24

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'
B B 0.0013 0.0007 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   21.6878(4)
_cell_length_b                   21.6878(4)
_cell_length_c                   25.7723(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10498.2(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2961
_cell_measurement_theta_min      2.679
_cell_measurement_theta_max      49.99

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_F_000             4530

_exptl_crystal_size_max          0.896
_exptl_crystal_size_mid          0.892
_exptl_crystal_size_min          0.658
_exptl_absorpt_coefficient_mu    0.907

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5644
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon II'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            86049
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.308
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4769
_reflns_number_gt                4611
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_refine_special_details          
;
;

_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.
;

_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0134P)²+21.8884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Dual-space/Direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4769
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0426
_refine_ls_wR_factor_gt          0.0422
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

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
Sm1 Sm 0.666667 0.333333 0.57908(2) 0.00982(4) Uani 1 3 d S T P . .
O1 O 0.74659(6) 0.66610(6) 0.58898(5) 0.0316(3) Uani 1 1 d . . . . .
O2 O 0.64229(7) 0.65301(6) 0.57271(5) 0.0322(3) Uani 1 1 d . . . . .
N1 N 0.57904(6) 0.44034(6) 0.57370(4) 0.0147(2) Uani 1 1 d . . . . .
N2 N 0.64553(6) 0.44780(6) 0.57901(4) 0.0148(2) Uani 1 1 d . . . . .
N3 N 0.51447(6) 0.33072(6) 0.62688(4) 0.0157(2) Uani 1 1 d . . . . .
N4 N 0.56912(6) 0.31963(6) 0.64080(4) 0.0155(2) Uani 1 1 d . . . . .
N5 N 0.51337(6) 0.32355(6) 0.52769(4) 0.0150(2) Uani 1 1 d . . . . .
N6 N 0.57043(6) 0.31609(6) 0.51466(4) 0.0141(2) Uani 1 1 d . . . . .
N7 N 0.68259(7) 0.62901(6) 0.57954(5) 0.0222(3) Uani 1 1 d . . . . .
C1 C 0.69084(8) 0.51726(7) 0.58105(5) 0.0163(3) Uani 1 1 d . . . . .
H1A H 0.740972 0.538701 0.584902 0.020 Uiso 1 1 calc R U . . .
C2 C 0.65347(8) 0.55407(7) 0.57666(5) 0.0175(3) Uani 1 1 d . . . . .
C3 C 0.58242(8) 0.50350(7) 0.57210(5) 0.0174(3) Uani 1 1 d . . . . .
H3 H 0.543643 0.511907 0.568521 0.021 Uiso 1 1 calc R U . . .
C4 C 0.55494(8) 0.29428(8) 0.68925(5) 0.0193(3) Uani 1 1 d . . . . .
H4 H 0.583888 0.281347 0.708798 0.023 Uiso 1 1 calc R U . . .
C5 C 0.49205(8) 0.28934(8) 0.70727(6) 0.0241(3) Uani 1 1 d . . . . .
H5 H 0.470493 0.273341 0.740329 0.029 Uiso 1 1 calc R U . . .
C6 C 0.46818(8) 0.31271(8) 0.66669(6) 0.0215(3) Uani 1 1 d . . . . .
H6 H 0.425970 0.315736 0.666626 0.026 Uiso 1 1 calc R U . . .
C7 C 0.55266(8) 0.27953(7) 0.47012(5) 0.0179(3) Uani 1 1 d . . . . .
H7 H 0.582402 0.266389 0.451868 0.021 Uiso 1 1 calc R U . . .
C8 C 0.48505(8) 0.26329(8) 0.45403(6) 0.0226(3) Uani 1 1 d . . . . .
H8 H 0.460227 0.237768 0.423869 0.027 Uiso 1 1 calc R U . . .
C9 C 0.46207(8) 0.29227(8) 0.49137(6) 0.0202(3) Uani 1 1 d . . . . .
H9 H 0.417451 0.290596 0.491603 0.024 Uiso 1 1 calc R U . . .
C10 C 0.39935(12) 0.10126(10) 0.76394(8) 0.0442(5) Uani 1 1 d . . . . .
H10 H 0.358329 0.106337 0.765144 0.053 Uiso 1 1 calc R U . . .
C11 C 0.43710(12) 0.11365(10) 0.71803(7) 0.0432(5) Uani 1 1 d . . . . .
H11 H 0.421893 0.127074 0.687648 0.052 Uiso 1 1 calc R U . . .
C12 C 0.49634(12) 0.10651(11) 0.71655(7) 0.0476(5) Uani 1 1 d . . . . .
H12 H 0.522344 0.115461 0.685122 0.057 Uiso 1 1 calc R U . . .
C13 C 0.51863(12) 0.08643(11) 0.76032(8) 0.0482(5) Uani 1 1 d . . . . .
H13 H 0.559703 0.081448 0.759009 0.058 Uiso 1 1 calc R U . . .
C14 C 0.48065(12) 0.07354(11) 0.80629(8) 0.0469(5) Uani 1 1 d . . . . .
H14 H 0.495426 0.059285 0.836473 0.056 Uiso 1 1 calc R U . . .
C15 C 0.42167(12) 0.08146(11) 0.80801(7) 0.0462(5) Uani 1 1 d . . . . .
H15 H 0.396094 0.073320 0.839570 0.055 Uiso 1 1 calc R U . . .
C16 C 0.37122(11) 0.45899(12) 0.57756(8) 0.0440(5) Uani 1 1 d . . . . .
H16 H 0.338517 0.434456 0.550295 0.053 Uiso 1 1 calc R U . . .
C17 C 0.36903(10) 0.42300(10) 0.62319(8) 0.0379(4) Uani 1 1 d . . . . .
H17 H 0.334756 0.374010 0.627227 0.045 Uiso 1 1 calc R U . . .
C18 C 0.41733(9) 0.45954(9) 0.66241(7) 0.0295(4) Uani 1 1 d . . . . .
H18 H 0.416197 0.435865 0.693710 0.035 Uiso 1 1 calc R U . . .
C19 C 0.46691(9) 0.53027(9) 0.65580(6) 0.0275(3) Uani 1 1 d . . . . .
H19 H 0.500548 0.555120 0.682490 0.033 Uiso 1 1 calc R U . . .
C20 C 0.46844(10) 0.56542(9) 0.61113(7) 0.0323(4) Uani 1 1 d . . . . .
H20 H 0.502644 0.614461 0.607258 0.039 Uiso 1 1 calc R U . . .
C21 C 0.42098(11) 0.53013(11) 0.57228(7) 0.0391(5) Uani 1 1 d . . . . .
H21 H 0.422226 0.554721 0.541442 0.047 Uiso 1 1 calc R U . . .
C22 C 0.59720(10) 0.27775(10) 0.83330(8) 0.0392(4) Uani 1 1 d . . . . .
H22 H 0.549412 0.239512 0.833200 0.047 Uiso 1 1 calc R U . . .
C23 C 0.39967(8) 0.67179(8) 0.66667(6) 0.0215(3) Uani 1 1 d . . . . .
H23 H 0.445120 0.675305 0.666656 0.026 Uiso 1 1 calc R U . . .
B1 B 0.51240(8) 0.36567(8) 0.57534(6) 0.0165(3) Uani 1 1 d . . . . .
H1 H 0.4642(9) 0.3706(9) 0.5737(7) 0.025 Uiso 1 1 d . U . . .


_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
Sm1 N4 2.5427(11) . ?
Sm1 N4 2.5428(11) 2_655 ?
Sm1 N4 2.5428(11) 3_665 ?
Sm1 N6 2.5439(11) 2_655 ?
Sm1 N6 2.5439(11) 3_665 ?
Sm1 N6 2.5440(11) . ?
Sm1 N2 2.7407(11) 3_665 ?
Sm1 N2 2.7408(11) 2_655 ?
Sm1 N2 2.7408(11) . ?
O1 N7 1.2315(18) . ?
O2 N7 1.2330(17) . ?
N1 C3 1.3353(18) . ?
N1 N2 1.3750(16) . ?
N1 B1 1.5402(19) . ?
N2 C1 1.3256(18) . ?
N3 C6 1.3495(18) . ?
N3 N4 1.3700(16) . ?
N3 B1 1.5411(19) . ?
N4 C4 1.3369(18) . ?
N5 C9 1.3488(18) . ?
N5 N6 1.3675(16) . ?
N5 B1 1.5370(19) . ?
N6 C7 1.3377(17) . ?
N7 C2 1.4212(18) . ?
C1 C2 1.398(2) . ?
C1 H1A 0.9500 . ?
C2 C3 1.379(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.389(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.372(2) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.384(3) . ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.369(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.389(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.374(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C21 1.378(3) . ?
C16 C17 1.399(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.374(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.372(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.364(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C22 1.3808(19) 17_556 ?
C22 C22 1.3809(19) 18_546 ?
C22 H22 0.9500 . ?
C23 C23 1.3864(15) 14_456 ?
C23 C23 1.3864(15) 15_556 ?
C23 H23 0.9500 . ?
B1 H1 1.103(18) . ?

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
N4 Sm1 N4 85.01(4) . 2_655 ?
N4 Sm1 N4 85.01(4) . 3_665 ?
N4 Sm1 N4 85.01(4) 2_655 3_665 ?
N4 Sm1 N6 136.34(4) . 2_655 ?
N4 Sm1 N6 79.49(4) 2_655 2_655 ?
N4 Sm1 N6 133.14(4) 3_665 2_655 ?
N4 Sm1 N6 133.14(4) . 3_665 ?
N4 Sm1 N6 136.34(4) 2_655 3_665 ?
N4 Sm1 N6 79.49(4) 3_665 3_665 ?
N6 Sm1 N6 82.02(4) 2_655 3_665 ?
N4 Sm1 N6 79.49(4) . . ?
N4 Sm1 N6 133.14(4) 2_655 . ?
N4 Sm1 N6 136.34(4) 3_665 . ?
N6 Sm1 N6 82.02(4) 2_655 . ?
N6 Sm1 N6 82.02(4) 3_665 . ?
N4 Sm1 N2 141.30(4) . 3_665 ?
N4 Sm1 N2 67.71(3) 2_655 3_665 ?
N4 Sm1 N2 66.42(4) 3_665 3_665 ?
N6 Sm1 N2 66.76(3) 2_655 3_665 ?
N6 Sm1 N2 68.67(3) 3_665 3_665 ?
N6 Sm1 N2 139.21(3) . 3_665 ?
N4 Sm1 N2 67.71(4) . 2_655 ?
N4 Sm1 N2 66.42(4) 2_655 2_655 ?
N4 Sm1 N2 141.30(4) 3_665 2_655 ?
N6 Sm1 N2 68.67(3) 2_655 2_655 ?
N6 Sm1 N2 139.21(3) 3_665 2_655 ?
N6 Sm1 N2 66.76(3) . 2_655 ?
N2 Sm1 N2 120.0 3_665 2_655 ?
N4 Sm1 N2 66.42(4) . . ?
N4 Sm1 N2 141.30(4) 2_655 . ?
N4 Sm1 N2 67.71(4) 3_665 . ?
N6 Sm1 N2 139.21(3) 2_655 . ?
N6 Sm1 N2 66.76(3) 3_665 . ?
N6 Sm1 N2 68.67(3) . . ?
N2 Sm1 N2 119.999(1) 3_665 . ?
N2 Sm1 N2 120.0 2_655 . ?
C3 N1 N2 111.45(11) . . ?
C3 N1 B1 128.37(12) . . ?
N2 N1 B1 119.91(11) . . ?
C1 N2 N1 106.01(11) . . ?
C1 N2 Sm1 131.64(9) . . ?
N1 N2 Sm1 122.27(8) . . ?
C6 N3 N4 109.49(11) . . ?
C6 N3 B1 126.68(12) . . ?
N4 N3 B1 123.55(11) . . ?
C4 N4 N3 105.99(11) . . ?
C4 N4 Sm1 129.74(9) . . ?
N3 N4 Sm1 123.92(8) . . ?
C9 N5 N6 109.75(11) . . ?
C9 N5 B1 126.89(12) . . ?
N6 N5 B1 123.27(11) . . ?
C7 N6 N5 105.74(11) . . ?
C7 N6 Sm1 128.26(9) . . ?
N5 N6 Sm1 123.15(8) . . ?
O1 N7 O2 123.91(13) . . ?
O1 N7 C2 117.93(13) . . ?
O2 N7 C2 118.15(13) . . ?
N2 C1 C2 109.48(13) . . ?
N2 C1 H1A 125.3 . . ?
C2 C1 H1A 125.3 . . ?
C3 C2 C1 106.80(12) . . ?
C3 C2 N7 126.52(13) . . ?
C1 C2 N7 126.58(14) . . ?
N1 C3 C2 106.25(12) . . ?
N1 C3 H3 126.9 . . ?
C2 C3 H3 126.9 . . ?
N4 C4 C5 110.98(13) . . ?
N4 C4 H4 124.5 . . ?
C5 C4 H4 124.5 . . ?
C6 C5 C4 104.67(13) . . ?
C6 C5 H5 127.7 . . ?
C4 C5 H5 127.7 . . ?
N3 C6 C5 108.86(13) . . ?
N3 C6 H6 125.6 . . ?
C5 C6 H6 125.6 . . ?
N6 C7 C8 111.17(13) . . ?
N6 C7 H7 124.4 . . ?
C8 C7 H7 124.4 . . ?
C9 C8 C7 104.69(13) . . ?
C9 C8 H8 127.7 . . ?
C7 C8 H8 127.7 . . ?
N5 C9 C8 108.64(13) . . ?
N5 C9 H9 125.7 . . ?
C8 C9 H9 125.7 . . ?
C15 C10 C11 119.7(2) . . ?
C15 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 119.9(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.62(19) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C10 120.27(19) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
C21 C16 C17 119.78(18) . . ?
C21 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 119.30(17) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.3 . . ?
C19 C18 C17 119.63(16) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 120.81(17) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C21 C20 C19 120.16(17) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C16 120.31(17) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
C22 C22 C22 119.999(4) 17_556 18_546 ?
C22 C22 H22 120.0 17_556 . ?
C22 C22 H22 120.0 18_546 . ?
C23 C23 C23 119.994(2) 14_456 15_556 ?
C23 C23 H23 120.0 14_456 . ?
C23 C23 H23 120.0 15_556 . ?
N5 B1 N1 108.57(11) . . ?
N5 B1 N3 112.57(11) . . ?
N1 B1 N3 107.33(11) . . ?
N5 B1 H1 108.9(9) . . ?
N1 B1 H1 109.4(9) . . ?
N3 B1 H1 110.0(9) . . ?

_refine_diff_density_max         0.319
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.043

