#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:57:56 +0100 (jue 07 de nov de 2019) $
#$Revision: 223903 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/09/7700911.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7700911
loop_
_publ_author_name
'Reed, William R.'
'Dunstan, Maja A.'
'Gable, Robert W.'
'Phonsri, Wasinee'
'Murray, Keith S.'
'Mole, Richard A.'
'Boskovic, Colette'
_publ_section_title
;
 Tetraoxolene-bridged rare-earth complexes: a radical-bridged dinuclear Dy
 single-molecule magnet.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15635
_journal_page_last               15645
_journal_paper_doi               10.1039/c9dt01320b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C42 H40 B4 Br2 Dy2 N24 O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H44 B4 Br2 Cl4 Dy2 N24 O4'
_chemical_formula_weight         1642.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-27 deposited with the CCDC.    2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.024(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1280(4)
_cell_length_b                   15.0635(4)
_cell_length_c                   14.8028(4)
_cell_measurement_reflns_used    11056
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.9420
_cell_measurement_theta_min      4.2780
_cell_volume                     2995.70(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  23.00   0.50    0.50    --  -48.30  91.00  38.00  116
  2  ω    -76.00 -41.00   0.50    0.50    --  -48.30  91.00  38.00   70
  3  ω     20.00  50.00   0.50    0.50    --   48.30 -91.00 -74.00   60
  4  ω   -158.00-131.00   0.50    1.75    --  -86.25 -91.00 -74.00   54
  5  ω    118.00 151.00   0.50    1.75    --  107.75  91.00  38.00   66
  6  ω     36.00 134.00   0.50    1.75    --  107.75 -91.00 -74.00  196
  7  ω    -54.00  24.00   0.50    0.50    --  -48.30  38.00 150.00  156
  8  ω   -118.00 -86.00   0.50    0.50    --  -48.30-125.00-180.00   64
  9  ω    -57.00  18.00   0.50    0.50    --  -48.30  38.00-150.00  150
 10  ω    -71.00 -46.00   0.50    1.75    --  -86.25  91.00  38.00   50
 11  ω     35.00  61.00   0.50    1.75    --  107.75 -30.00-120.00   52
 12  ω     35.00  71.00   0.50    1.75    --  107.75 -30.00 -30.00   72
 13  ω     38.00  64.00   0.50    1.75    --  107.75 -30.00 -90.00   52
 14  ω     42.00  73.00   0.50    1.75    --  107.75 -45.00 -90.00   62
 15  ω     35.00  70.00   0.50    1.75    --  107.75 -30.00  30.00   70
 16  ω     37.00  68.00   0.50    1.75    --  107.75 -30.00  90.00   62
 17  ω     42.00  76.00   0.50    1.75    --  107.75 -45.00 -30.00   68
 18  ω     39.00  70.00   0.50    1.75    --  107.75 -45.00  60.00   62
 19  ω     38.00  77.00   0.50    1.75    --  107.75 -45.00-180.00   78
 20  ω     44.00  71.00   0.50    1.75    --  107.75 -45.00 -60.00   54
 21  ω    149.00 175.00   0.50    1.75    --  107.75  30.00 -30.00   52
 22  ω     98.00 123.00   0.50    1.75    --  107.75  30.00 -30.00   50
 23  ω     36.00  62.00   0.50    1.75    --  107.75 -30.00 -60.00   52
 24  ω     93.00 118.00   0.50    1.75    --  107.75 125.00  90.00   50
 25  ω    153.00 178.00   0.50    1.75    --  107.75 125.00  90.00   50
 26  ω     39.00  70.00   0.50    1.75    --  107.75 -30.00   0.00   62
 27  ω     40.00  71.00   0.50    1.75    --  107.75 -30.00 120.00   62
 28  ω     46.00  71.00   0.50    1.75    --  107.75 -30.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0494685000
_diffrn_orient_matrix_UB_12      0.0893624000
_diffrn_orient_matrix_UB_13      -0.0086186000
_diffrn_orient_matrix_UB_21      0.0942643000
_diffrn_orient_matrix_UB_22      -0.0285141000
_diffrn_orient_matrix_UB_23      0.0795329000
_diffrn_orient_matrix_UB_31      0.0426523000
_diffrn_orient_matrix_UB_32      -0.0407386000
_diffrn_orient_matrix_UB_33      -0.0746854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.463
_diffrn_reflns_theta_min         3.781
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.923
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation of dichloromethane/ethanol'
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0247P)²+5.1914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             6046
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01320b2.cif
_cod_data_source_block           2-Dy
_cod_depositor_comments
'Adding full bibliography for 7700911--7700914.cif.'
_cod_original_cell_volume        2995.68(14)
_cod_database_code               7700911
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H44 B4 Br2 Cl4 N24 O4 Dy2'
_chemical_oxdiff_usercomment     'Mg O-Bipy HBA'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.530
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1A), B2(H2A)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.633
_oxdiff_exptl_absorpt_empirical_full_min 0.518
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Dy1 Dy 0.58368(2) 0.36972(2) 0.27593(2) 0.01516(7) Uani 1 1 d .
Br1 Br 0.42684(3) 0.67640(2) 0.35894(3) 0.02287(10) Uani 1 1 d .
O1 O 0.53093(18) 0.50257(16) 0.32983(16) 0.0176(5) Uani 1 1 d .
O2 O 0.57416(18) 0.35907(16) 0.43257(17) 0.0188(5) Uani 1 1 d .
N1 N 0.3999(2) 0.3882(2) 0.1993(2) 0.0192(6) Uani 1 1 d .
N2 N 0.3400(2) 0.3202(2) 0.1530(2) 0.0205(6) Uani 1 1 d .
N3 N 0.5174(2) 0.2224(2) 0.2943(2) 0.0221(6) Uani 1 1 d .
N4 N 0.4366(2) 0.1835(2) 0.2291(2) 0.0217(6) Uani 1 1 d .
N5 N 0.5350(2) 0.2994(2) 0.1137(2) 0.0193(6) Uani 1 1 d .
N6 N 0.4542(2) 0.2454(2) 0.0782(2) 0.0205(6) Uani 1 1 d .
N7 N 0.6362(2) 0.47609(19) 0.1778(2) 0.0178(6) Uani 1 1 d .
N8 N 0.7308(2) 0.47502(19) 0.1709(2) 0.0179(6) Uani 1 1 d .
N9 N 0.7280(2) 0.2866(2) 0.2615(2) 0.0197(6) Uani 1 1 d .
N10 N 0.8060(2) 0.3293(2) 0.2440(2) 0.0204(6) Uani 1 1 d .
N11 N 0.7419(2) 0.4427(2) 0.3819(2) 0.0195(6) Uani 1 1 d .
N12 N 0.8175(2) 0.4645(2) 0.3456(2) 0.0212(6) Uani 1 1 d .
C1 C 0.3392(3) 0.4591(3) 0.1915(3) 0.0235(8) Uani 1 1 d .
H1 H 0.360301 0.516249 0.216833 0.028 Uiso 1 1 calc R
C2 C 0.2415(3) 0.4368(3) 0.1412(3) 0.0260(8) Uani 1 1 d .
H2 H 0.184571 0.474114 0.126018 0.031 Uiso 1 1 calc R
C3 C 0.2456(3) 0.3491(3) 0.1184(3) 0.0241(8) Uani 1 1 d .
H3 H 0.190416 0.314095 0.083578 0.029 Uiso 1 1 calc R
C4 C 0.5456(3) 0.1648(3) 0.3666(3) 0.0263(8) Uani 1 1 d .
H4 H 0.599447 0.174585 0.422850 0.032 Uiso 1 1 calc R
C5 C 0.4870(3) 0.0895(3) 0.3496(3) 0.0300(9) Uani 1 1 d .
H5 H 0.492656 0.038980 0.389336 0.036 Uiso 1 1 calc R
C6 C 0.4183(3) 0.1046(3) 0.2617(3) 0.0280(8) Uani 1 1 d .
H6 H 0.366281 0.065274 0.229511 0.034 Uiso 1 1 calc R
C7 C 0.5802(3) 0.3035(2) 0.0462(2) 0.0205(7) Uani 1 1 d .
H7 H 0.639320 0.336030 0.051603 0.025 Uiso 1 1 calc R
C8 C 0.5283(3) 0.2534(3) -0.0330(3) 0.0251(8) Uani 1 1 d .
H8 H 0.544498 0.245371 -0.090164 0.030 Uiso 1 1 calc R
C9 C 0.4488(3) 0.2183(2) -0.0103(3) 0.0234(8) Uani 1 1 d .
H9 H 0.398600 0.181216 -0.050069 0.028 Uiso 1 1 calc R
C10 C 0.5823(3) 0.5258(2) 0.1047(2) 0.0193(7) Uani 1 1 d .
H10 H 0.513430 0.538291 0.091639 0.023 Uiso 1 1 calc R
C11 C 0.6399(3) 0.5563(2) 0.0510(3) 0.0229(7) Uani 1 1 d .
H11 H 0.619334 0.592521 -0.004234 0.027 Uiso 1 1 calc R
C12 C 0.7331(3) 0.5230(2) 0.0946(3) 0.0221(7) Uani 1 1 d .
H12 H 0.790065 0.532238 0.074501 0.027 Uiso 1 1 calc R
C13 C 0.7389(3) 0.1996(3) 0.2457(3) 0.0258(8) Uani 1 1 d .
H13 H 0.695121 0.154102 0.252523 0.031 Uiso 1 1 calc R
C14 C 0.8232(3) 0.1860(3) 0.2180(3) 0.0293(9) Uani 1 1 d .
H14 H 0.847773 0.131169 0.202662 0.035 Uiso 1 1 calc R
C15 C 0.8632(3) 0.2693(3) 0.2175(3) 0.0291(9) Uani 1 1 d .
H15 H 0.921615 0.282354 0.201175 0.035 Uiso 1 1 calc R
C16 C 0.7648(3) 0.4834(2) 0.4668(3) 0.0225(7) Uani 1 1 d .
H16 H 0.725461 0.480270 0.508367 0.027 Uiso 1 1 calc R
C17 C 0.8535(3) 0.5305(3) 0.4859(3) 0.0267(8) Uani 1 1 d .
H17 H 0.885887 0.564351 0.540949 0.032 Uiso 1 1 calc R
C18 C 0.8840(3) 0.5169(2) 0.4066(3) 0.0245(8) Uani 1 1 d .
H18 H 0.942352 0.540861 0.397065 0.029 Uiso 1 1 calc R
C19 C 0.5121(3) 0.5058(2) 0.4074(2) 0.0164(7) Uani 1 1 d .
C20 C 0.4697(3) 0.5773(2) 0.4401(2) 0.0167(7) Uani 1 1 d .
C21 C 0.5414(2) 0.4221(2) 0.4698(2) 0.0159(6) Uani 1 1 d .
B1 B 0.3811(3) 0.2292(3) 0.1346(3) 0.0231(8) Uani 1 1 d .
H1A H 0.325124 0.190593 0.096957 0.028 Uiso 1 1 calc R
B2 B 0.8183(3) 0.4307(3) 0.2479(3) 0.0242(9) Uani 1 1 d .
H2A H 0.882703 0.447044 0.237425 0.029 Uiso 1 1 calc R
Cl1 Cl 0.27708(13) 0.16279(9) 0.44334(13) 0.0664(4) Uani 1 1 d .
Cl2 Cl 0.27075(14) 0.33968(11) 0.36175(10) 0.0698(4) Uani 1 1 d .
C22 C 0.3110(6) 0.2742(4) 0.4629(4) 0.073(2) Uani 1 1 d .
H22A H 0.283109 0.298280 0.511568 0.088 Uiso 1 1 calc R
H22B H 0.384396 0.278164 0.488635 0.088 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0326
1 -1 0 0.0326
-1 -1 0 0.0111
1 1 0 0.0111
-1 0 1 0.0237
1 0 -1 0.0237
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
O1 Dy1 O2 66.85(8) . .
O1 Dy1 N1 70.58(9) . .
O1 Dy1 N3 123.92(9) . .
O1 Dy1 N5 131.14(9) . .
O1 Dy1 N7 80.19(9) . .
O1 Dy1 N9 144.97(9) . .
O1 Dy1 N11 74.61(9) . .
O2 Dy1 N1 94.92(9) . .
O2 Dy1 N3 72.04(9) . .
O2 Dy1 N5 145.41(9) . .
O2 Dy1 N7 138.65(9) . .
O2 Dy1 N9 110.50(9) . .
O2 Dy1 N11 74.42(9) . .
N1 Dy1 N5 71.09(9) . .
N1 Dy1 N11 144.99(9) . .
N3 Dy1 N1 76.90(10) . .
N3 Dy1 N5 73.97(10) . .
N3 Dy1 N9 84.51(10) . .
N3 Dy1 N11 127.84(10) . .
N5 Dy1 N11 134.22(9) . .
N7 Dy1 N1 96.98(9) . .
N7 Dy1 N3 149.31(10) . .
N7 Dy1 N5 75.60(10) . .
N7 Dy1 N9 82.47(10) . .
N7 Dy1 N11 73.22(9) . .
N9 Dy1 N1 142.04(10) . .
N9 Dy1 N5 72.08(10) . .
N9 Dy1 N11 71.33(10) . .
C19 O1 Dy1 121.3(2) . .
C21 O2 Dy1 121.2(2) . .
N2 N1 Dy1 122.5(2) . .
C1 N1 Dy1 131.9(2) . .
C1 N1 N2 105.7(3) . .
N1 N2 B1 123.0(3) . .
C3 N2 N1 109.6(3) . .
C3 N2 B1 127.0(3) . .
N4 N3 Dy1 124.7(2) . .
C4 N3 Dy1 130.1(3) . .
C4 N3 N4 105.1(3) . .
N3 N4 B1 121.7(3) . .
C6 N4 N3 109.6(3) . .
C6 N4 B1 128.6(3) . .
N6 N5 Dy1 124.5(2) . .
C7 N5 Dy1 129.6(2) . .
C7 N5 N6 105.9(3) . .
N5 N6 B1 120.5(3) . .
C9 N6 N5 110.1(3) . .
C9 N6 B1 129.3(3) . .
N8 N7 Dy1 121.5(2) . .
C10 N7 Dy1 130.4(2) . .
C10 N7 N8 105.7(3) . .
N7 N8 B2 121.6(3) . .
C12 N8 N7 109.4(3) . .
C12 N8 B2 128.7(3) . .
N10 N9 Dy1 121.0(2) . .
C13 N9 Dy1 130.7(3) . .
C13 N9 N10 106.4(3) . .
N9 N10 B2 123.3(3) . .
C15 N10 N9 109.3(3) . .
C15 N10 B2 127.3(3) . .
N12 N11 Dy1 120.1(2) . .
C16 N11 Dy1 133.1(2) . .
C16 N11 N12 105.4(3) . .
N11 N12 B2 121.4(3) . .
C18 N12 N11 110.1(3) . .
C18 N12 B2 128.5(3) . .
N1 C1 H1 124.7 . .
N1 C1 C2 110.7(3) . .
C2 C1 H1 124.7 . .
C1 C2 H2 127.6 . .
C3 C2 C1 104.7(3) . .
C3 C2 H2 127.6 . .
N2 C3 C2 109.3(3) . .
N2 C3 H3 125.3 . .
C2 C3 H3 125.3 . .
N3 C4 H4 124.0 . .
N3 C4 C5 112.0(4) . .
C5 C4 H4 124.0 . .
C4 C5 H5 128.0 . .
C4 C5 C6 104.1(3) . .
C6 C5 H5 128.0 . .
N4 C6 C5 109.2(3) . .
N4 C6 H6 125.4 . .
C5 C6 H6 125.4 . .
N5 C7 H7 124.7 . .
N5 C7 C8 110.6(3) . .
C8 C7 H7 124.7 . .
C7 C8 H8 127.5 . .
C9 C8 C7 105.0(3) . .
C9 C8 H8 127.5 . .
N6 C9 C8 108.4(3) . .
N6 C9 H9 125.8 . .
C8 C9 H9 125.8 . .
N7 C10 H10 124.4 . .
N7 C10 C11 111.2(3) . .
C11 C10 H10 124.4 . .
C10 C11 H11 127.5 . .
C12 C11 C10 105.0(3) . .
C12 C11 H11 127.5 . .
N8 C12 C11 108.7(3) . .
N8 C12 H12 125.6 . .
C11 C12 H12 125.6 . .
N9 C13 H13 124.8 . .
N9 C13 C14 110.5(4) . .
C14 C13 H13 124.8 . .
C13 C14 H14 127.6 . .
C15 C14 C13 104.9(3) . .
C15 C14 H14 127.6 . .
N10 C15 C14 109.0(4) . .
N10 C15 H15 125.5 . .
C14 C15 H15 125.5 . .
N11 C16 H16 124.3 . .
N11 C16 C17 111.3(3) . .
C17 C16 H16 124.3 . .
C16 C17 H17 127.8 . .
C18 C17 C16 104.4(3) . .
C18 C17 H17 127.8 . .
N12 C18 C17 108.8(3) . .
N12 C18 H18 125.6 . .
C17 C18 H18 125.6 . .
O1 C19 C20 125.6(3) . .
O1 C19 C21 115.0(3) . .
C20 C19 C21 119.4(3) . .
C19 C20 Br1 118.6(2) . .
C19 C20 C21 121.8(3) . 3_666
C21 C20 Br1 119.6(2) 3_666 .
O2 C21 C19 115.0(3) . .
O2 C21 C20 126.3(3) . 3_666
C20 C21 C19 118.7(3) 3_666 .
N2 B1 H1A 109.8 . .
N4 B1 N2 110.5(3) . .
N4 B1 H1A 109.8 . .
N6 B1 N2 107.9(3) . .
N6 B1 N4 109.0(3) . .
N6 B1 H1A 109.8 . .
N8 B2 H2A 109.7 . .
N10 B2 N8 110.2(3) . .
N10 B2 H2A 109.7 . .
N12 B2 N8 108.2(3) . .
N12 B2 N10 109.4(3) . .
N12 B2 H2A 109.7 . .
Cl1 C22 H22A 108.8 . .
Cl1 C22 H22B 108.8 . .
Cl2 C22 Cl1 113.8(4) . .
Cl2 C22 H22A 108.8 . .
Cl2 C22 H22B 108.8 . .
H22A C22 H22B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.359(2) .
Dy1 O2 2.369(2) .
Dy1 N1 2.506(3) .
Dy1 N3 2.456(3) .
Dy1 N5 2.518(3) .
Dy1 N7 2.428(3) .
Dy1 N9 2.458(3) .
Dy1 N11 2.549(3) .
Br1 C20 1.894(3) .
O1 C19 1.257(4) .
O2 C21 1.256(4) .
N1 N2 1.370(4) .
N1 C1 1.352(5) .
N2 C3 1.344(5) .
N2 B1 1.545(5) .
N3 N4 1.377(4) .
N3 C4 1.339(5) .
N4 C6 1.337(5) .
N4 B1 1.539(5) .
N5 N6 1.366(4) .
N5 C7 1.345(4) .
N6 C9 1.352(4) .
N6 B1 1.536(5) .
N7 N8 1.371(4) .
N7 C10 1.342(4) .
N8 C12 1.351(5) .
N8 B2 1.550(5) .
N9 N10 1.367(4) .
N9 C13 1.348(5) .
N10 C15 1.349(5) .
N10 B2 1.537(6) .
N11 N12 1.376(4) .
N11 C16 1.344(5) .
N12 C18 1.340(5) .
N12 B2 1.536(5) .
C1 H1 0.9500 .
C1 C2 1.391(5) .
C2 H2 0.9500 .
C2 C3 1.369(6) .
C3 H3 0.9500 .
C4 H4 0.9500 .
C4 C5 1.380(6) .
C5 H5 0.9500 .
C5 C6 1.381(6) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C7 C8 1.396(5) .
C8 H8 0.9500 .
C8 C9 1.374(5) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C10 C11 1.381(5) .
C11 H11 0.9500 .
C11 C12 1.370(5) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C13 C14 1.389(6) .
C14 H14 0.9500 .
C14 C15 1.377(6) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C16 C17 1.391(5) .
C17 H17 0.9500 .
C17 C18 1.384(6) .
C18 H18 0.9500 .
C19 C20 1.390(5) .
C19 C21 1.541(5) .
C20 C21 1.391(4) 3_666
B1 H1A 1.0000 .
B2 H2A 1.0000 .
Cl1 C22 1.745(6) .
Cl2 C22 1.735(6) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Dy1 O1 C19 C20 -171.9(3) .
Dy1 O1 C19 C21 8.9(4) .
Dy1 O2 C21 C19 -2.0(4) .
Dy1 O2 C21 C20 178.5(3) 3_666
Dy1 N1 N2 C3 -179.5(2) .
Dy1 N1 N2 B1 -6.5(4) .
Dy1 N1 C1 C2 179.4(2) .
Dy1 N3 N4 C6 -178.3(2) .
Dy1 N3 N4 B1 2.1(4) .
Dy1 N3 C4 C5 178.5(3) .
Dy1 N5 N6 C9 -179.8(2) .
Dy1 N5 N6 B1 4.6(4) .
Dy1 N5 C7 C8 179.3(2) .
Dy1 N7 N8 C12 163.6(2) .
Dy1 N7 N8 B2 -21.4(4) .
Dy1 N7 C10 C11 -161.6(2) .
Dy1 N9 N10 C15 -165.8(2) .
Dy1 N9 N10 B2 10.1(4) .
Dy1 N9 C13 C14 164.1(3) .
Dy1 N11 N12 C18 168.0(2) .
Dy1 N11 N12 B2 -11.6(4) .
Dy1 N11 C16 C17 -166.1(3) .
O1 Dy1 O2 C21 4.5(2) .
O1 Dy1 N1 N2 -165.7(3) .
O1 Dy1 N1 C1 15.3(3) .
O1 Dy1 N3 N4 90.0(3) .
O1 Dy1 N3 C4 -86.9(3) .
O1 Dy1 N5 N6 -85.2(3) .
O1 Dy1 N5 C7 96.5(3) .
O1 Dy1 N7 N8 130.1(2) .
O1 Dy1 N7 C10 -70.5(3) .
O1 Dy1 N9 N10 -35.6(3) .
O1 Dy1 N9 C13 162.1(3) .
O1 Dy1 N11 N12 -120.8(2) .
O1 Dy1 N11 C16 43.4(3) .
O1 C19 C20 Br1 4.8(5) .
O1 C19 C20 C21 -174.9(3) 3_666
O1 C19 C21 O2 -4.5(4) .
O1 C19 C21 C20 175.1(3) 3_666
O2 Dy1 O1 C19 -7.3(2) .
O2 Dy1 N1 N2 -102.4(2) .
O2 Dy1 N1 C1 78.6(3) .
O2 Dy1 N3 N4 134.3(3) .
O2 Dy1 N3 C4 -42.7(3) .
O2 Dy1 N5 N6 25.1(3) .
O2 Dy1 N5 C7 -153.2(3) .
O2 Dy1 N7 N8 93.2(3) .
O2 Dy1 N7 C10 -107.4(3) .
O2 Dy1 N9 N10 -114.2(2) .
O2 Dy1 N9 C13 83.5(3) .
O2 Dy1 N11 N12 169.4(3) .
O2 Dy1 N11 C16 -26.3(3) .
N1 Dy1 O1 C19 97.1(3) .
N1 Dy1 O2 C21 -61.9(3) .
N1 Dy1 N3 N4 34.6(3) .
N1 Dy1 N3 C4 -142.3(3) .
N1 Dy1 N5 N6 -45.2(3) .
N1 Dy1 N5 C7 136.5(3) .
N1 Dy1 N7 N8 -161.1(2) .
N1 Dy1 N7 C10 -1.7(3) .
N1 Dy1 N9 N10 116.8(2) .
N1 Dy1 N9 C13 -45.4(4) .
N1 Dy1 N11 N12 -114.6(2) .
N1 Dy1 N11 C16 49.6(4) .
N1 N2 C3 C2 0.1(4) .
N1 N2 B1 N4 61.6(4) .
N1 N2 B1 N6 -57.5(4) .
N1 C1 C2 C3 -0.2(4) .
N2 N1 C1 C2 0.3(4) .
N3 Dy1 O1 C19 38.9(3) .
N3 Dy1 O2 C21 -136.5(3) .
N3 Dy1 N1 N2 -32.1(2) .
N3 Dy1 N1 C1 148.9(3) .
N3 Dy1 N5 N6 36.1(3) .
N3 Dy1 N5 C7 -142.2(3) .
N3 Dy1 N7 N8 -85.0(3) .
N3 Dy1 N7 C10 74.3(4) .
N3 Dy1 N9 N10 177.3(2) .
N3 Dy1 N9 C13 15.0(3) .
N3 Dy1 N11 N12 117.9(2) .
N3 Dy1 N11 C16 -77.8(3) .
N3 N4 C6 C5 0.0(5) .
N3 N4 B1 N2 -59.1(4) .
N3 N4 B1 N6 59.3(4) .
N3 C4 C5 C6 -1.1(5) .
N4 N3 C4 C5 1.1(4) .
N5 Dy1 O1 C19 137.3(2) .
N5 Dy1 O2 C21 -125.3(3) .
N5 Dy1 N1 N2 45.2(2) .
N5 Dy1 N1 C1 -133.8(3) .
N5 Dy1 N3 N4 -39.2(3) .
N5 Dy1 N3 C4 143.9(3) .
N5 Dy1 N7 N8 -92.7(2) .
N5 Dy1 N7 C10 66.7(3) .
N5 Dy1 N9 N10 102.4(2) .
N5 Dy1 N9 C13 -59.9(3) .
N5 Dy1 N11 N12 12.3(3) .
N5 Dy1 N11 C16 176.6(3) .
N5 N6 C9 C8 1.1(4) .
N5 N6 B1 N2 57.8(4) .
N5 N6 B1 N4 -62.2(4) .
N5 C7 C8 C9 0.0(4) .
N6 N5 C7 C8 0.7(4) .
N7 Dy1 O1 C19 -161.8(3) .
N7 Dy1 O2 C21 44.5(3) .
N7 Dy1 N1 N2 117.3(2) .
N7 Dy1 N1 C1 -61.7(3) .
N7 Dy1 N3 N4 -46.9(4) .
N7 Dy1 N3 C4 136.1(3) .
N7 Dy1 N5 N6 -147.9(3) .
N7 Dy1 N5 C7 33.8(3) .
N7 Dy1 N9 N10 25.1(2) .
N7 Dy1 N9 C13 -137.1(3) .
N7 Dy1 N11 N12 -36.7(2) .
N7 Dy1 N11 C16 127.6(3) .
N7 N8 C12 C11 0.2(4) .
N7 N8 B2 N10 70.4(4) .
N7 N8 B2 N12 -49.2(4) .
N7 C10 C11 C12 -0.1(4) .
N8 N7 C10 C11 0.2(4) .
N9 Dy1 O1 C19 -100.4(3) .
N9 Dy1 O2 C21 146.8(2) .
N9 Dy1 N1 N2 30.6(3) .
N9 Dy1 N1 C1 -148.4(3) .
N9 Dy1 N3 N4 -112.1(3) .
N9 Dy1 N3 C4 71.0(3) .
N9 Dy1 N5 N6 125.5(3) .
N9 Dy1 N5 C7 -52.8(3) .
N9 Dy1 N7 N8 -19.4(2) .
N9 Dy1 N7 C10 140.0(3) .
N9 Dy1 N11 N12 50.9(2) .
N9 Dy1 N11 C16 -144.9(3) .
N9 N10 C15 C14 -0.4(4) .
N9 N10 B2 N8 -63.2(4) .
N9 N10 B2 N12 55.7(4) .
N9 C13 C14 C15 -0.1(4) .
N10 N9 C13 C14 -0.1(4) .
N11 Dy1 O1 C19 -86.7(3) .
N11 Dy1 O2 C21 84.1(3) .
N11 Dy1 N1 N2 -172.1(2) .
N11 Dy1 N1 C1 8.9(4) .
N11 Dy1 N3 N4 -173.2(2) .
N11 Dy1 N3 C4 9.8(4) .
N11 Dy1 N5 N6 163.8(2) .
N11 Dy1 N5 C7 -14.5(4) .
N11 Dy1 N7 N8 53.3(2) .
N11 Dy1 N7 C10 -147.3(3) .
N11 Dy1 N9 N10 -49.6(2) .
N11 Dy1 N9 C13 148.1(3) .
N11 N12 C18 C17 0.4(4) .
N11 N12 B2 N8 67.3(4) .
N11 N12 B2 N10 -52.7(4) .
N11 C16 C17 C18 0.4(4) .
N12 N11 C16 C17 -0.2(4) .
C1 N1 N2 C3 -0.2(4) .
C1 N1 N2 B1 172.7(3) .
C1 C2 C3 N2 0.1(4) .
C3 N2 B1 N4 -126.7(4) .
C3 N2 B1 N6 114.2(4) .
C4 N3 N4 C6 -0.7(4) .
C4 N3 N4 B1 179.7(3) .
C4 C5 C6 N4 0.7(5) .
C6 N4 B1 N2 121.4(4) .
C6 N4 B1 N6 -120.3(4) .
C7 N5 N6 C9 -1.1(4) .
C7 N5 N6 B1 -176.8(3) .
C7 C8 C9 N6 -0.7(4) .
C9 N6 B1 N2 -116.9(4) .
C9 N6 B1 N4 123.1(4) .
C10 N7 N8 C12 -0.3(4) .
C10 N7 N8 B2 174.7(3) .
C10 C11 C12 N8 -0.1(4) .
C12 N8 B2 N10 -115.7(4) .
C12 N8 B2 N12 124.8(4) .
C13 N9 N10 C15 0.3(4) .
C13 N9 N10 B2 176.2(3) .
C13 C14 C15 N10 0.3(4) .
C15 N10 B2 N8 111.9(4) .
C15 N10 B2 N12 -129.2(4) .
C16 N11 N12 C18 -0.2(4) .
C16 N11 N12 B2 -179.7(3) .
C16 C17 C18 N12 -0.5(4) .
C18 N12 B2 N8 -112.2(4) .
C18 N12 B2 N10 127.8(4) .
C20 C19 C21 O2 176.3(3) .
C20 C19 C21 C20 -4.1(5) 3_666
C21 C19 C20 Br1 -176.1(2) .
C21 C19 C20 C21 4.2(5) 3_666
B1 N2 C3 C2 -172.5(3) .
B1 N4 C6 C5 179.6(4) .
B1 N6 C9 C8 176.3(4) .
B2 N8 C12 C11 -174.3(3) .
B2 N10 C15 C14 -176.0(3) .
B2 N12 C18 C17 180.0(3) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9992 1.0004 -0.0003 0.0400 -0.1227 -0.0833
0.9992 -1.0004 0.0003 -0.0400 0.1227 0.0833
-1.0010 -0.9998 0.0000 -0.1389 -0.0658 -0.0020
1.0010 0.9998 -0.0000 0.1389 0.0658 0.0020
-1.0000 0.0024 1.0002 -0.0579 -0.0148 -0.1175
1.0000 -0.0024 -1.0002 0.0579 0.0148 0.1175
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.029 0.386 0.167 35.0 1.6
2 -0.029 0.614 0.833 35.0 1.6
3 0.471 0.886 0.333 35.0 1.6
4 0.529 0.114 0.667 35.0 2.0
