# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1820463'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2017-08-01
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H48 Dy2 N6 O20 Zn2'
_chemical_formula_sum            'C46 H48 Dy2 N6 O20 Zn2'
_chemical_formula_weight         1460.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zn Yb C22 H22 N4 O10'
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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.1539(8)
_cell_length_b                   12.8094(7)
_cell_length_c                   18.1769(12)
_cell_angle_alpha                90
_cell_angle_beta                 104.998(7)
_cell_angle_gamma                90
_cell_volume                     2733.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6910
_cell_measurement_theta_min      2.3390
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.839
_exptl_absorpt_coefficient_mu    3.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7980
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         2.320
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  73.00   1.00   10.00    --  -17.00  72.00 150.00  108
  2  ω    -69.00  22.00   1.00   10.00    --  -17.00 -72.00  30.00   91
  3  ω    -69.00  22.00   1.00   10.00    --  -17.00 -72.00-150.00   91
  4  ω    -56.00   8.00   1.00   10.00    --  -17.00   0.00   0.00   64
  5  ω    -31.00 -14.00   1.00   10.00    --  -17.00  54.00   0.00   17
  6  ω   -107.00  30.00   1.00   10.00    --  -17.00 -18.00  60.00  137
  7  ω    -80.00 -29.00   1.00   10.00    --  -17.00 -72.00   0.00   51
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0569793000
_diffrn_orient_matrix_UB_12      -0.0155937000
_diffrn_orient_matrix_UB_13      -0.0030496000
_diffrn_orient_matrix_UB_21      -0.0099177000
_diffrn_orient_matrix_UB_22      0.0472552000
_diffrn_orient_matrix_UB_23      0.0175481000
_diffrn_orient_matrix_UB_31      -0.0174214000
_diffrn_orient_matrix_UB_32      0.0242845000
_diffrn_orient_matrix_UB_33      -0.0362730000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6921
_reflns_number_total             7980
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.195
_refine_diff_density_min         -2.539
_refine_diff_density_rms         0.310
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0953
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1159P)²+99.0667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2627
_refine_special_details          
'Structure has been refined as 2-componant twin. RIGU and SADI restraints have been applied to disordered cyclohexane moiety.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.560(3)
 0.440(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C6A-C1A \\sim C1B-C6B \\sim C1A-C2 \\sim C3A-C2 \\sim C3A-C4A \\sim C3B-C4B
\\sim C5-C4B \\sim C6B-C5
 with sigma of 0.02
 C1B-C2 \\sim C1A-C2 \\sim C6A-C1A \\sim C1B-C6B \\sim C6A-C5 \\sim C6B-C5
\\sim C5-C4A \\sim C5-C4B \\sim C3A-
 C4A \\sim C3B-C4B \\sim C3B-C2 \\sim C3A-C2
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C1A, C1B, C2, C3A, C3B, C4A, C4B, C5, C6A, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6B)=Sof(H6B)=Sof(C1B)=Sof(H1B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=1-FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C6A)=Sof(H6A)=
 Sof(C1A)=Sof(H1A)=FVAR(1)
 Fixed Sof: H5AA(0.5) H5AB(0.5) H5BC(0.5) H5BD(0.5) H2AA(0.5) H2AB(0.5)
 H2BC(0.5) H2BD(0.5)
6.a Ternary CH refined with riding coordinates:
 C6A(H6A), C1A(H1A), C6B(H6B), C1B(H1B)
6.b Secondary CH2 refined with riding coordinates:
 C4A(H4AA,H4AB), C3A(H3AA,H3AB), C4B(H4BA,H4BB), C3B(H3BA,H3BB), C5(H5AA,H5AB),
  C5(H5BC,H5BD), C2(H2AA,H2AB), C2(H2BC,H2BD)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C19(H19), C7(H7), C10(H10), C17(H17), C15(H15), C18(H18)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.35398(7) 0.56685(7) 0.43859(5) 0.0307(3) Uani 1 1 d . . . . .
Zn1 Zn 0.78494(18) 0.66218(17) 0.56504(12) 0.0291(5) Uani 1 1 d . . . . .
O3 O 0.7300(11) 0.5700(9) 0.6385(7) 0.029(3) Uani 1 1 d . . . . .
O6 O 0.5503(10) 0.5856(9) 0.4994(8) 0.029(3) Uani 1 1 d . . . . .
O1 O 0.7799(11) 0.5209(9) 0.5148(7) 0.031(3) Uani 1 1 d . . . . .
O2 O 0.6663(10) 0.3832(10) 0.4265(7) 0.028(3) Uani 1 1 d . . . . .
O4 O 0.5730(12) 0.4733(11) 0.6782(8) 0.038(3) Uani 1 1 d . . . . .
O7 O 0.4610(11) 0.7264(9) 0.4482(8) 0.036(3) Uani 1 1 d . . . . .
O5 O 0.6477(10) 0.7344(10) 0.5085(7) 0.032(3) Uani 1 1 d . . . . .
O8 O 0.2052(11) 0.6989(11) 0.4288(8) 0.038(3) Uani 1 1 d . . . . .
O9 O 0.2506(12) 0.6684(12) 0.3235(8) 0.045(4) Uani 1 1 d . . . . .
N1 N 0.9234(14) 0.6983(13) 0.5273(10) 0.036(4) Uani 1 1 d . . . . .
O10 O 0.1198(13) 0.7851(12) 0.3262(10) 0.055(4) Uani 1 1 d . . . . .
N3 N 0.1902(13) 0.7180(11) 0.3571(9) 0.031(4) Uani 1 1 d . . . . .
N2 N 0.8630(16) 0.7537(13) 0.6521(9) 0.039(4) Uani 1 1 d . . . . .
C13 C 0.8125(16) 0.5077(15) 0.4510(10) 0.030(4) Uani 1 1 d . . . . .
C23 C 0.5561(16) 0.6841(14) 0.4857(12) 0.032(4) Uani 1 1 d . . . . .
C20 C 0.6251(16) 0.5512(14) 0.7275(11) 0.030(4) Uani 1 1 d . . . . .
C8 C 0.9000(17) 0.5604(14) 0.4346(11) 0.030(4) Uani 1 1 d . . . . .
C12 C 0.7537(16) 0.4282(15) 0.4010(11) 0.031(4) Uani 1 1 d . . . . .
C21 C 0.7062(16) 0.6074(16) 0.7009(11) 0.034(4) Uani 1 1 d . . . . .
C11 C 0.7839(18) 0.4033(17) 0.3371(12) 0.040(5) Uani 1 1 d . . . . .
H11 H 0.744755 0.349702 0.304520 0.049 Uiso 1 1 calc R . . . .
C9 C 0.9327(16) 0.5317(15) 0.3662(11) 0.032(4) Uani 1 1 d . . . . .
H9 H 0.995660 0.564917 0.354107 0.038 Uiso 1 1 calc R . . . .
C19 C 0.6036(17) 0.5774(15) 0.7960(11) 0.035(4) Uani 1 1 d . . . . .
H19 H 0.548417 0.539217 0.813591 0.042 Uiso 1 1 calc R . . . .
C16 C 0.7603(16) 0.6911(15) 0.7412(11) 0.034(4) Uani 1 1 d . . . . .
C7 C 0.9585(16) 0.6487(17) 0.4772(13) 0.039(5) Uani 1 1 d . . . . .
H7 H 1.027706 0.670976 0.467094 0.047 Uiso 1 1 calc R . . . .
C14 C 0.608(2) 0.2964(19) 0.3819(13) 0.056(7) Uani 1 1 d . . . . .
H14A H 0.576583 0.318903 0.329202 0.084 Uiso 1 1 calc GR . . . .
H14B H 0.546941 0.271926 0.403376 0.084 Uiso 1 1 calc GR . . . .
H14C H 0.662817 0.239490 0.383080 0.084 Uiso 1 1 calc GR . . . .
C22 C 0.4948(19) 0.4072(17) 0.7046(12) 0.042(5) Uani 1 1 d . . . . .
H22A H 0.473769 0.347237 0.670338 0.063 Uiso 1 1 calc GR . . . .
H22B H 0.426262 0.446998 0.705333 0.063 Uiso 1 1 calc GR . . . .
H22C H 0.531402 0.382357 0.756162 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.872(2) 0.4566(18) 0.3191(12) 0.046(5) Uani 1 1 d . . . . .
H10 H 0.891970 0.440709 0.273026 0.055 Uiso 1 1 calc R . . . .
C17 C 0.736(2) 0.7143(16) 0.8113(14) 0.046(6) Uani 1 1 d . . . . .
H17 H 0.774264 0.771299 0.840715 0.056 Uiso 1 1 calc R . . . .
C15 C 0.845(2) 0.7588(16) 0.7173(12) 0.044(5) Uani 1 1 d . . . . .
H15 H 0.887291 0.807900 0.752815 0.053 Uiso 1 1 calc R . . . .
C18 C 0.6598(18) 0.6567(16) 0.8383(12) 0.037(5) Uani 1 1 d . . . . .
H18 H 0.646478 0.672613 0.886296 0.044 Uiso 1 1 calc R . . . .
C4A C 1.057(4) 0.990(3) 0.639(2) 0.047(9) Uani 0.53(4) 1 d D U P A 1
H4AA H 1.103385 1.039105 0.676154 0.056 Uiso 0.53(4) 1 calc R . P A 1
H4AB H 0.998423 1.029317 0.600925 0.056 Uiso 0.53(4) 1 calc R . P A 1
C3A C 1.130(4) 0.923(3) 0.601(3) 0.050(13) Uani 0.53(4) 1 d D U P A 1
H3AA H 1.172085 0.970843 0.575129 0.059 Uiso 0.53(4) 1 calc R . P A 1
H3AB H 1.187641 0.887421 0.641896 0.059 Uiso 0.53(4) 1 calc R . P A 1
C6A C 0.925(3) 0.833(2) 0.6230(19) 0.032(7) Uani 0.53(4) 1 d D U P A 1
H6A H 0.868532 0.875199 0.584836 0.038 Uiso 0.53(4) 1 calc R . P A 1
C1A C 1.000(3) 0.774(2) 0.581(2) 0.031(8) Uani 0.53(4) 1 d D U P A 1
H1A H 1.052842 0.730562 0.620569 0.038 Uiso 0.53(4) 1 calc R . P A 1
C6B C 0.981(4) 0.799(2) 0.6411(18) 0.037(9) Uani 0.47(4) 1 d D U P A 2
H6B H 1.045683 0.750461 0.664107 0.044 Uiso 0.47(4) 1 calc R . P A 2
C1B C 0.962(3) 0.804(4) 0.5551(19) 0.035(9) Uani 0.47(4) 1 d D U P A 2
H1B H 0.901378 0.856067 0.533222 0.041 Uiso 0.47(4) 1 calc R . P A 2
C4B C 1.114(3) 0.942(4) 0.661(2) 0.038(9) Uani 0.47(4) 1 d D U P A 2
H4BA H 1.134593 1.011996 0.683293 0.046 Uiso 0.47(4) 1 calc R . P A 2
H4BB H 1.175642 0.893245 0.685814 0.046 Uiso 0.47(4) 1 calc R . P A 2
C3B C 1.109(6) 0.947(3) 0.576(2) 0.050(14) Uani 0.47(4) 1 d D U P A 2
H3BA H 1.053154 1.000178 0.550623 0.060 Uiso 0.47(4) 1 calc R . P A 2
H3BB H 1.184775 0.966164 0.569129 0.060 Uiso 0.47(4) 1 calc R . P A 2
C5 C 1.0027(18) 0.9068(14) 0.6780(12) 0.041(4) Uani 1 1 d D U . . .
H5AA H 0.958431 0.941581 0.709681 0.049 Uiso 0.5 1 calc R . P A 1
H5AB H 1.063968 0.865841 0.712437 0.049 Uiso 0.5 1 calc R . P A 1
H5BC H 1.011355 0.902609 0.733595 0.049 Uiso 0.5 1 calc R . P A 2
H5BD H 0.939670 0.955320 0.655283 0.049 Uiso 0.5 1 calc R . P A 2
C2 C 1.0742(18) 0.8398(17) 0.5432(14) 0.050(5) Uani 1 1 d D U . . .
H2AA H 1.132766 0.795683 0.529509 0.060 Uiso 0.5 1 calc R . P A 1
H2AB H 1.027239 0.872868 0.496259 0.060 Uiso 0.5 1 calc R . P A 1
H2BC H 1.068546 0.841200 0.487869 0.060 Uiso 0.5 1 calc R . P A 2
H2BD H 1.134047 0.788839 0.566963 0.060 Uiso 0.5 1 calc R . P A 2


_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 Zn1 3.377(2) 3_666 ?
Dy1 O3 2.310(12) 3_666 ?
Dy1 O6 2.368(12) . ?
Dy1 O6 2.400(12) 3_666 ?
Dy1 O1 2.311(12) 3_666 ?
Dy1 O2 2.607(12) 3_666 ?
Dy1 O4 2.556(14) 3_666 ?
Dy1 O7 2.405(12) . ?
Dy1 O8 2.448(13) . ?
Dy1 O9 2.508(15) . ?
Dy1 N3 2.894(15) . ?
Dy1 C23 2.817(19) . ?
Zn1 O3 2.021(12) . ?
Zn1 O1 2.021(13) . ?
Zn1 O5 1.951(13) . ?
Zn1 N1 2.028(16) . ?
Zn1 N2 2.000(16) . ?
O3 C21 1.33(2) . ?
O6 C23 1.29(2) . ?
O1 C13 1.33(2) . ?
O2 C12 1.39(2) . ?
O2 C14 1.45(2) . ?
O4 C20 1.38(2) . ?
O4 C22 1.44(2) . ?
O7 C23 1.30(2) . ?
O5 C23 1.26(2) . ?
O8 N3 1.29(2) . ?
O9 N3 1.24(2) . ?
N1 C7 1.27(3) . ?
N1 C1A 1.51(4) . ?
N1 C1B 1.48(5) . ?
O10 N3 1.24(2) . ?
N2 C15 1.26(3) . ?
N2 C6A 1.44(4) . ?
N2 C6B 1.61(5) . ?
C13 C8 1.36(3) . ?
C13 C12 1.43(3) . ?
C20 C21 1.40(3) . ?
C20 C19 1.38(3) . ?
C8 C9 1.45(3) . ?
C8 C7 1.45(3) . ?
C12 C11 1.34(3) . ?
C21 C16 1.37(3) . ?
C11 H11 0.9500 . ?
C11 C10 1.38(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.37(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.35(3) . ?
C16 C17 1.41(3) . ?
C16 C15 1.49(3) . ?
C7 H7 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C10 H10 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.37(3) . ?
C15 H15 0.9500 . ?
C18 H18 0.9500 . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C4A C3A 1.53(2) . ?
C4A C5 1.52(2) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C2 1.53(2) . ?
C6A H6A 1.0000 . ?
C6A C1A 1.52(2) . ?
C6A C5 1.52(2) . ?
C1A H1A 1.0000 . ?
C1A C2 1.53(2) . ?
C6B H6B 1.0000 . ?
C6B C1B 1.52(2) . ?
C6B C5 1.53(2) . ?
C1B H1B 1.0000 . ?
C1B C2 1.51(2) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
C4B C3B 1.52(2) . ?
C4B C5 1.54(2) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3B C2 1.52(2) . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C2 H2AA 0.9900 . ?
C2 H2AB 0.9900 . ?
C2 H2BC 0.9900 . ?
C2 H2BD 0.9900 . ?

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
O3 Dy1 Zn1 35.8(3) 3_666 3_666 ?
O3 Dy1 O6 75.6(4) 3_666 3_666 ?
O3 Dy1 O6 126.4(4) 3_666 . ?
O3 Dy1 O1 67.1(4) 3_666 3_666 ?
O3 Dy1 O2 128.5(4) 3_666 3_666 ?
O3 Dy1 O4 62.5(4) 3_666 3_666 ?
O3 Dy1 O7 146.6(5) 3_666 . ?
O3 Dy1 O8 106.1(5) 3_666 . ?
O3 Dy1 O9 80.8(4) 3_666 . ?
O3 Dy1 N3 93.4(4) 3_666 . ?
O3 Dy1 C23 143.4(5) 3_666 . ?
O6 Dy1 Zn1 122.4(3) . 3_666 ?
O6 Dy1 Zn1 58.8(3) 3_666 3_666 ?
O6 Dy1 O6 63.6(4) . 3_666 ?
O6 Dy1 O2 84.9(4) 3_666 3_666 ?
O6 Dy1 O2 82.2(4) . 3_666 ?
O6 Dy1 O4 83.3(4) . 3_666 ?
O6 Dy1 O4 89.8(4) 3_666 3_666 ?
O6 Dy1 O7 118.0(4) 3_666 . ?
O6 Dy1 O7 54.5(4) . . ?
O6 Dy1 O8 148.8(5) 3_666 . ?
O6 Dy1 O8 126.9(4) . . ?
O6 Dy1 O9 124.3(5) . . ?
O6 Dy1 O9 153.0(5) 3_666 . ?
O6 Dy1 N3 166.0(4) 3_666 . ?
O6 Dy1 N3 130.3(4) . . ?
O6 Dy1 C23 27.1(4) . . ?
O6 Dy1 C23 90.7(4) 3_666 . ?
O1 Dy1 Zn1 35.8(3) 3_666 3_666 ?
O1 Dy1 O6 126.7(4) 3_666 . ?
O1 Dy1 O6 74.6(4) 3_666 3_666 ?
O1 Dy1 O2 61.8(4) 3_666 3_666 ?
O1 Dy1 O4 129.4(4) 3_666 3_666 ?
O1 Dy1 O7 143.7(5) 3_666 . ?
O1 Dy1 O8 77.6(5) 3_666 . ?
O1 Dy1 O9 108.1(5) 3_666 . ?
O1 Dy1 N3 93.3(5) 3_666 . ?
O1 Dy1 C23 142.1(5) 3_666 . ?
O2 Dy1 Zn1 93.6(3) 3_666 3_666 ?
O2 Dy1 N3 95.6(4) 3_666 . ?
O2 Dy1 C23 82.5(5) 3_666 . ?
O4 Dy1 Zn1 95.1(3) 3_666 3_666 ?
O4 Dy1 O2 165.5(4) 3_666 3_666 ?
O4 Dy1 N3 92.9(5) 3_666 . ?
O4 Dy1 C23 84.1(5) 3_666 . ?
O7 Dy1 Zn1 176.5(3) . 3_666 ?
O7 Dy1 O2 84.5(4) . 3_666 ?
O7 Dy1 O4 86.2(5) . 3_666 ?
O7 Dy1 O8 78.1(5) . . ?
O7 Dy1 O9 76.4(5) . . ?
O7 Dy1 N3 75.9(4) . . ?
O7 Dy1 C23 27.4(5) . . ?
O8 Dy1 Zn1 104.0(3) . 3_666 ?
O8 Dy1 O2 69.6(4) . 3_666 ?
O8 Dy1 O4 119.1(5) . 3_666 ?
O8 Dy1 O9 51.7(5) . . ?
O8 Dy1 N3 26.3(5) . . ?
O8 Dy1 C23 102.9(5) . . ?
O9 Dy1 Zn1 107.1(4) . 3_666 ?
O9 Dy1 O2 120.6(4) . 3_666 ?
O9 Dy1 O4 67.6(5) . 3_666 ?
O9 Dy1 N3 25.3(5) . . ?
O9 Dy1 C23 100.7(5) . . ?
N3 Dy1 Zn1 107.3(3) . 3_666 ?
C23 Dy1 Zn1 149.5(3) . 3_666 ?
C23 Dy1 N3 103.2(5) . . ?
O3 Zn1 Dy1 41.9(3) . 3_666 ?
O3 Zn1 N1 143.3(6) . . ?
O1 Zn1 Dy1 42.0(4) . 3_666 ?
O1 Zn1 O3 78.4(5) . . ?
O1 Zn1 N1 89.0(6) . . ?
O5 Zn1 Dy1 92.7(4) . 3_666 ?
O5 Zn1 O3 104.0(5) . . ?
O5 Zn1 O1 105.4(5) . . ?
O5 Zn1 N1 112.6(6) . . ?
O5 Zn1 N2 107.7(6) . . ?
N1 Zn1 Dy1 130.2(5) . 3_666 ?
N2 Zn1 Dy1 131.1(5) . 3_666 ?
N2 Zn1 O3 89.4(6) . . ?
N2 Zn1 O1 146.6(7) . . ?
N2 Zn1 N1 82.4(7) . . ?
Zn1 O3 Dy1 102.3(5) . 3_666 ?
C21 O3 Dy1 129.1(11) . 3_666 ?
C21 O3 Zn1 122.3(12) . . ?
Dy1 O6 Dy1 116.4(4) . 3_666 ?
C23 O6 Dy1 96.2(11) . . ?
C23 O6 Dy1 147.3(12) . 3_666 ?
Zn1 O1 Dy1 102.3(5) . 3_666 ?
C13 O1 Dy1 130.9(12) . 3_666 ?
C13 O1 Zn1 121.7(11) . . ?
C12 O2 Dy1 118.6(11) . 3_666 ?
C12 O2 C14 115.8(16) . . ?
C14 O2 Dy1 124.4(13) . 3_666 ?
C20 O4 Dy1 119.0(11) . 3_666 ?
C20 O4 C22 116.0(15) . . ?
C22 O4 Dy1 123.9(11) . 3_666 ?
C23 O7 Dy1 94.3(10) . . ?
C23 O5 Zn1 119.5(11) . . ?
N3 O8 Dy1 96.5(10) . . ?
N3 O9 Dy1 95.0(11) . . ?
C7 N1 Zn1 126.2(14) . . ?
C7 N1 C1A 121.5(18) . . ?
C7 N1 C1B 124.5(19) . . ?
C1A N1 Zn1 110.4(13) . . ?
C1B N1 Zn1 108.2(15) . . ?
O8 N3 Dy1 57.2(8) . . ?
O9 N3 Dy1 59.7(9) . . ?
O9 N3 O8 116.9(14) . . ?
O10 N3 Dy1 176.3(14) . . ?
O10 N3 O8 119.2(17) . . ?
O10 N3 O9 123.9(17) . . ?
C15 N2 Zn1 127.7(15) . . ?
C15 N2 C6A 122.8(18) . . ?
C15 N2 C6B 118.3(19) . . ?
C6A N2 Zn1 107.9(14) . . ?
C6B N2 Zn1 111.7(13) . . ?
O1 C13 C8 123.8(17) . . ?
O1 C13 C12 115.7(17) . . ?
C8 C13 C12 120.4(17) . . ?
O6 C23 Dy1 56.7(9) . . ?
O6 C23 O7 115.0(16) . . ?
O7 C23 Dy1 58.4(9) . . ?
O5 C23 Dy1 178.1(13) . . ?
O5 C23 O6 121.6(16) . . ?
O5 C23 O7 123.3(15) . . ?
O4 C20 C21 113.0(16) . . ?
C19 C20 O4 126.9(18) . . ?
C19 C20 C21 120.1(19) . . ?
C13 C8 C9 117.9(17) . . ?
C13 C8 C7 125.1(18) . . ?
C9 C8 C7 116.9(17) . . ?
O2 C12 C13 112.5(16) . . ?
C11 C12 O2 126.4(19) . . ?
C11 C12 C13 121.1(19) . . ?
O3 C21 C20 115.9(17) . . ?
O3 C21 C16 124.0(18) . . ?
C16 C21 C20 120.0(19) . . ?
C12 C11 H11 120.3 . . ?
C12 C11 C10 119(2) . . ?
C10 C11 H11 120.3 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.7(19) . . ?
C10 C9 H9 120.1 . . ?
C20 C19 H19 119.6 . . ?
C18 C19 C20 121(2) . . ?
C18 C19 H19 119.6 . . ?
C21 C16 C17 118(2) . . ?
C21 C16 C15 124.8(19) . . ?
C17 C16 C15 117.3(18) . . ?
N1 C7 C8 124.3(18) . . ?
N1 C7 H7 117.8 . . ?
C8 C7 H7 117.8 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 122(2) . . ?
C9 C10 H10 119.2 . . ?
C16 C17 H17 119.1 . . ?
C18 C17 C16 122(2) . . ?
C18 C17 H17 119.1 . . ?
N2 C15 C16 122.8(19) . . ?
N2 C15 H15 118.6 . . ?
C16 C15 H15 118.6 . . ?
C19 C18 C17 119(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
H4AA C4A H4AB 109.4 . . ?
C3A C4A H4AA 111.6 . . ?
C3A C4A H4AB 111.6 . . ?
C5 C4A H4AA 111.6 . . ?
C5 C4A H4AB 111.6 . . ?
C5 C4A C3A 101(3) . . ?
C4A C3A H3AA 107.4 . . ?
C4A C3A H3AB 107.4 . . ?
H3AA C3A H3AB 107.0 . . ?
C2 C3A C4A 120(3) . . ?
C2 C3A H3AA 107.4 . . ?
C2 C3A H3AB 107.4 . . ?
N2 C6A H6A 108.2 . . ?
N2 C6A C1A 106(2) . . ?
N2 C6A C5 120(2) . . ?
C1A C6A H6A 108.2 . . ?
C5 C6A H6A 108.2 . . ?
C5 C6A C1A 106(2) . . ?
N1 C1A C6A 107(2) . . ?
N1 C1A H1A 106.2 . . ?
N1 C1A C2 113(2) . . ?
C6A C1A H1A 106.2 . . ?
C6A C1A C2 117(3) . . ?
C2 C1A H1A 106.2 . . ?
N2 C6B H6B 110.6 . . ?
C1B C6B N2 104(3) . . ?
C1B C6B H6B 110.6 . . ?
C1B C6B C5 112(3) . . ?
C5 C6B N2 109(3) . . ?
C5 C6B H6B 110.6 . . ?
N1 C1B C6B 105(3) . . ?
N1 C1B H1B 109.8 . . ?
N1 C1B C2 117(3) . . ?
C6B C1B H1B 109.8 . . ?
C2 C1B C6B 105(3) . . ?
C2 C1B H1B 109.8 . . ?
H4BA C4B H4BB 107.6 . . ?
C3B C4B H4BA 108.7 . . ?
C3B C4B H4BB 108.7 . . ?
C3B C4B C5 114(4) . . ?
C5 C4B H4BA 108.7 . . ?
C5 C4B H4BB 108.7 . . ?
C4B C3B H3BA 110.3 . . ?
C4B C3B H3BB 110.3 . . ?
H3BA C3B H3BB 108.5 . . ?
C2 C3B C4B 107(3) . . ?
C2 C3B H3BA 110.3 . . ?
C2 C3B H3BB 110.3 . . ?
C4A C5 C6A 114(3) . . ?
C4A C5 H5AA 108.8 . . ?
C4A C5 H5AB 108.8 . . ?
C6A C5 H5AA 108.8 . . ?
C6A C5 H5AB 108.8 . . ?
C6B C5 C4B 104(3) . . ?
C6B C5 H5BC 111.1 . . ?
C6B C5 H5BD 111.1 . . ?
C4B C5 H5BC 111.1 . . ?
C4B C5 H5BD 111.1 . . ?
H5AA C5 H5AB 107.7 . . ?
H5BC C5 H5BD 109.0 . . ?
C3A C2 C1A 106(3) . . ?
C3A C2 H2AA 110.4 . . ?
C3A C2 H2AB 110.4 . . ?
C1A C2 H2AA 110.4 . . ?
C1A C2 H2AB 110.4 . . ?
C1B C2 C3B 113(4) . . ?
C1B C2 H2BC 109.0 . . ?
C1B C2 H2BD 109.0 . . ?
C3B C2 H2BC 109.0 . . ?
C3B C2 H2BD 109.0 . . ?
H2AA C2 H2AB 108.6 . . ?
H2BC C2 H2BD 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O3 C21 C20 6(2) 3_666 . . . ?
Dy1 O3 C21 C16 -178.4(14) 3_666 . . . ?
Dy1 O6 C23 Dy1 -175(2) 3_666 . . . ?
Dy1 O6 C23 O7 -174.7(14) 3_666 . . . ?
Dy1 O6 C23 O7 0.1(19) . . . . ?
Dy1 O6 C23 O5 4(4) 3_666 . . . ?
Dy1 O6 C23 O5 179.1(17) . . . . ?
Dy1 O1 C13 C8 -174.1(13) 3_666 . . . ?
Dy1 O1 C13 C12 2(2) 3_666 . . . ?
Dy1 O2 C12 C13 -7.5(19) 3_666 . . . ?
Dy1 O2 C12 C11 172.5(16) 3_666 . . . ?
Dy1 O4 C20 C21 7(2) 3_666 . . . ?
Dy1 O4 C20 C19 -174.3(14) 3_666 . . . ?
Dy1 O7 C23 O6 -0.1(18) . . . . ?
Dy1 O7 C23 O5 -179.1(18) . . . . ?
Dy1 O8 N3 O9 -0.4(16) . . . . ?
Dy1 O8 N3 O10 -178.8(13) . . . . ?
Dy1 O9 N3 O8 0.4(16) . . . . ?
Dy1 O9 N3 O10 178.7(15) . . . . ?
Zn1 O3 C21 C20 152.7(13) . . . . ?
Zn1 O3 C21 C16 -31(2) . . . . ?
Zn1 O1 C13 C8 36(2) . . . . ?
Zn1 O1 C13 C12 -148.1(13) . . . . ?
Zn1 O5 C23 O6 1(3) . . . . ?
Zn1 O5 C23 O7 179.5(15) . . . . ?
Zn1 N1 C7 C8 4(3) . . . . ?
Zn1 N1 C1A C6A -25(3) . . . . ?
Zn1 N1 C1A C2 -155.4(18) . . . . ?
Zn1 N1 C1B C6B 55(3) . . . . ?
Zn1 N1 C1B C2 171(2) . . . . ?
Zn1 N2 C15 C16 2(3) . . . . ?
Zn1 N2 C6A C1A -54(3) . . . . ?
Zn1 N2 C6A C5 -173.6(19) . . . . ?
Zn1 N2 C6B C1B 29(3) . . . . ?
Zn1 N2 C6B C5 148.4(18) . . . . ?
O3 C21 C16 C17 -172.4(18) . . . . ?
O3 C21 C16 C15 6(3) . . . . ?
O1 C13 C8 C9 174.6(16) . . . . ?
O1 C13 C8 C7 -10(3) . . . . ?
O1 C13 C12 O2 4(2) . . . . ?
O1 C13 C12 C11 -175.9(17) . . . . ?
O2 C12 C11 C10 179.2(18) . . . . ?
O4 C20 C21 O3 -8(2) . . . . ?
O4 C20 C21 C16 176.1(17) . . . . ?
O4 C20 C19 C18 -179.0(18) . . . . ?
N1 C1A C2 C3A 171(3) . . . . ?
N1 C1B C2 C3B -178(3) . . . . ?
N2 C6A C1A N1 51(3) . . . . ?
N2 C6A C1A C2 179(3) . . . . ?
N2 C6A C5 C4A -177(3) . . . . ?
N2 C6B C1B N1 -53(3) . . . . ?
N2 C6B C1B C2 -177(3) . . . . ?
N2 C6B C5 C4B -178(2) . . . . ?
C13 C8 C9 C10 3(3) . . . . ?
C13 C8 C7 N1 -12(3) . . . . ?
C13 C12 C11 C10 -1(3) . . . . ?
C20 C21 C16 C17 3(3) . . . . ?
C20 C21 C16 C15 -177.9(19) . . . . ?
C20 C19 C18 C17 2(3) . . . . ?
C8 C13 C12 O2 -179.6(16) . . . . ?
C8 C13 C12 C11 0(3) . . . . ?
C8 C9 C10 C11 -3(3) . . . . ?
C12 C13 C8 C9 -1(3) . . . . ?
C12 C13 C8 C7 173.9(18) . . . . ?
C12 C11 C10 C9 2(3) . . . . ?
C21 C20 C19 C18 0(3) . . . . ?
C21 C16 C17 C18 -1(3) . . . . ?
C21 C16 C15 N2 10(4) . . . . ?
C9 C8 C7 N1 163(2) . . . . ?
C19 C20 C21 O3 173.3(16) . . . . ?
C19 C20 C21 C16 -3(3) . . . . ?
C16 C17 C18 C19 -2(3) . . . . ?
C7 N1 C1A C6A 170(3) . . . . ?
C7 N1 C1A C2 40(3) . . . . ?
C7 N1 C1B C6B -136(3) . . . . ?
C7 N1 C1B C2 -20(4) . . . . ?
C7 C8 C9 C10 -173.0(19) . . . . ?
C14 O2 C12 C13 -175.3(17) . . . . ?
C14 O2 C12 C11 5(3) . . . . ?
C22 O4 C20 C21 175.5(17) . . . . ?
C22 O4 C20 C19 -6(3) . . . . ?
C17 C16 C15 N2 -171(2) . . . . ?
C15 N2 C6A C1A 140(3) . . . . ?
C15 N2 C6A C5 20(4) . . . . ?
C15 N2 C6B C1B -167(3) . . . . ?
C15 N2 C6B C5 -47(3) . . . . ?
C15 C16 C17 C18 180(2) . . . . ?
C4A C3A C2 C1A -51(5) . . . . ?
C3A C4A C5 C6A -64(4) . . . . ?
C6A N2 C15 C16 166(2) . . . . ?
C6A C1A C2 C3A 46(4) . . . . ?
C1A N1 C7 C8 167(2) . . . . ?
C1A C6A C5 C4A 64(4) . . . . ?
C6B N2 C15 C16 -159(2) . . . . ?
C6B C1B C2 C3B -62(5) . . . . ?
C1B N1 C7 C8 -162(3) . . . . ?
C1B C6B C5 C4B -64(4) . . . . ?
C4B C3B C2 C1B 57(6) . . . . ?
C3B C4B C5 C6B 59(4) . . . . ?
C5 C4A C3A C2 60(5) . . . . ?
C5 C6A C1A N1 179(2) . . . . ?
C5 C6A C1A C2 -53(4) . . . . ?
C5 C6B C1B N1 -170(3) . . . . ?
C5 C6B C1B C2 66(5) . . . . ?
C5 C4B C3B C2 -57(6) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id KG0210052016
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.544
_oxdiff_exptl_absorpt_empirical_full_min 0.482
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.560(3) 10322 17862 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.440(3) 10252 17862 nmt -0.3705 -0.0025 -0.6880 -0.0021 -1.0000 0.0017
-1.2501 0.0050 0.3718

_twin_special_details            
;
Component 2 rotated by 179.9722° 
 around [-0.45 0.00 0.89] (reciprocal) or [-0.67 0.00 0.74] (direct)
;
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1820464'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2017-11-21
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H35 N4 O14 Y Zn, C H4 O'
_chemical_formula_sum            'C32 H39 N4 O15 Y Zn'
_chemical_formula_weight         873.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zn Y C30 H30 N2 O10'
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0130(15)
_cell_length_b                   12.9690(15)
_cell_length_c                   13.1459(14)
_cell_angle_alpha                99.823(9)
_cell_angle_beta                 98.676(10)
_cell_angle_gamma                95.680(10)
_cell_volume                     1813.8(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1690
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.7990
_cell_measurement_theta_min      4.4890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12577
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        63.150
_diffrn_reflns_theta_max         63.150
_diffrn_reflns_theta_min         4.429
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds): 
# Type Start End Width tₑₓₚ ω θ κ φ Frames 
#-------------------------------------------------------------------------- 
1 ω -43.00 98.00 1.00 1.50 -- 31.83 -19.00 60.00 141 
2 ω 43.00 74.00 1.00 1.50 -- 31.83 -99.00 0.00 31 
3 ω 25.00 89.00 1.00 4.00 -- 94.50-111.00 30.00 64 
4 ω 77.00 102.00 1.00 4.00 -- 94.50 -93.00 65.68 25 
5 ω 81.00 127.00 1.00 4.00 -- 94.50 -77.00 30.00 46 
6 ω 107.00 138.00 1.00 4.00 -- 94.50 -25.00 90.00 31 
7 ω 132.00 157.00 1.00 4.00 -- 94.50 25.00 90.00 25 
8 ω 138.00 164.00 1.00 4.00 -- 94.50 50.00 30.00 26 
9 ω 121.00 156.00 1.00 4.00 -- 94.50 77.00 120.00 35 
10 ω 98.00 139.00 1.00 4.00 -- 94.50 25.00 30.00 41 
11 ω 87.00 124.00 1.00 4.00 -- 94.50 -38.00 120.00 37 
12 ω 72.00 134.00 1.00 4.00 -- 94.50 -92.00 120.00 62 
13 ω 80.00 105.00 1.00 4.00 -- 94.50 -92.00 -30.00 25 
14 ω 83.00 128.00 1.00 4.00 -- 94.50 -92.00 -60.00 45 
15 ω 85.00 110.00 1.00 4.00 -- 94.50 -92.00-150.00 25 
16 ω 49.00 76.00 1.00 4.00 -- 94.50 -77.00-150.00 27 
17 ω 22.00 90.00 1.00 4.00 -- 94.50-111.00 -60.00 68 
18 ω 37.00 115.00 1.00 4.00 -- 94.50 -50.00 0.00 78 
19 ω 67.00 168.00 1.00 4.00 -- 94.50 38.00 120.00 101 
20 ω 81.00 134.00 1.00 4.00 -- 94.50 50.00 30.00 53 
21 ω 76.00 122.00 1.00 4.00 -- 94.50 64.00 -90.00 46 
22 ω 117.00 145.00 1.00 4.00 -- 94.50 50.00-120.00 28 
23 ω 131.00 158.00 1.00 4.00 -- 94.50 64.00-150.00 27 
24 ω 71.00 157.00 1.00 4.00 -- 94.50 25.00-180.00 86 
25 ω 69.00 104.00 1.00 4.00 -- 94.50 64.00-150.00 35 
26 ω 39.00 70.00 1.00 1.50 -- 31.83 178.00 -30.00 31 
27 ω 49.00 76.00 1.00 4.00 -- 94.50 -25.00 90.00 27 
28 ω 45.00 82.00 1.00 4.00 -- 94.50 -64.00 90.00 37 
29 ω 49.00 74.00 1.00 4.00 -- 94.50-111.00 60.00 25 
30 ω 44.00 88.00 1.00 4.00 -- 94.50 -64.00 120.00 44 
31 ω 30.00 57.00 1.00 4.00 -- 94.50-111.00 0.00 27 
32 ω 22.00 78.00 1.00 4.00 -- 94.50 -92.00 -30.00 56 
33 ω 21.00 73.00 1.00 4.00 -- 94.50-111.00 -30.00 52 
34 ω 21.00 86.00 1.00 4.00 -- 94.50-111.00 90.00 65 
35 ω -11.00 38.00 1.00 1.50 -- 31.83 -99.00 0.00 49 
36 ω -88.00 -57.00 1.00 1.50 -- -31.83-178.00-180.00 31 
37 ω -100.00 -59.00 1.00 1.50 -- -31.83 -38.00 30.00 41 

;

_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1388662000
_diffrn_orient_matrix_UB_12      -0.0334319000
_diffrn_orient_matrix_UB_13      -0.0029696000
_diffrn_orient_matrix_UB_21      -0.0278356000
_diffrn_orient_matrix_UB_22      0.0146255000
_diffrn_orient_matrix_UB_23      -0.1147076000
_diffrn_orient_matrix_UB_31      0.0173866000
_diffrn_orient_matrix_UB_32      -0.1159585000
_diffrn_orient_matrix_UB_33      -0.0375038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3832
_reflns_number_total             5627
_reflns_odcompleteness_completeness 84.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5627
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0653
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0880P)²+3.1130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1957
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O13-H13
 0.85 with sigma of 0.01
 C25-H13
 1.867934 with sigma of 0.02
 Y1-H13
 2.869091 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C9(H9), C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C15(H15), C17(H17), C18(H18), C19(H19),
 C27(H27), C29(H29), C30(H30), C31(H31)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C34(H34A,H34B,
 H34C), C26(H26A,H26B,H26C)
3.e Idealised tetrahedral OH refined as rotating group:
 O14(H14A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.29597(6) 0.71249(5) 0.76351(5) 0.0533(3) Uani 1 1 d D . . . .
Zn1 Zn 0.39266(9) 0.76772(7) 0.53700(7) 0.0496(3) Uani 1 1 d . . . . .
O1 O 0.1416(5) 0.5514(4) 0.6595(4) 0.0552(13) Uani 1 1 d . . . . .
O2 O 0.3162(5) 0.6480(4) 0.5946(4) 0.0544(13) Uani 1 1 d . . . . .
O3 O 0.3998(5) 0.8331(4) 0.6887(4) 0.0547(13) Uani 1 1 d . . . . .
O4 O 0.3301(5) 0.9178(4) 0.8560(4) 0.0554(13) Uani 1 1 d . . . . .
O5 O 0.2827(5) 0.8572(4) 0.4645(4) 0.0604(13) Uani 1 1 d . . . . .
O6 O 0.1482(7) 0.7210(6) 0.4087(6) 0.088(2) Uani 1 1 d . . . . .
O7 O 0.3249(6) 0.5535(5) 0.8334(5) 0.0688(15) Uani 1 1 d . . . . .
O8 O 0.1798(5) 0.7105(4) 0.8887(4) 0.0587(13) Uani 1 1 d . . . . .
O9 O 0.0474(7) 0.7935(6) 1.0261(5) 0.084(2) Uani 1 1 d . . . . .
O10 O 0.5187(7) 0.6626(6) 0.7742(6) 0.087(2) Uani 1 1 d . . . . .
O11 O 0.4665(6) 0.7556(5) 0.9060(5) 0.0716(16) Uani 1 1 d . . . . .
O12 O 0.6471(8) 0.7022(8) 0.9214(8) 0.124(3) Uani 1 1 d . . . . .
O13 O 0.1210(6) 0.7905(5) 0.7053(4) 0.0697(16) Uani 1 1 d D . . . .
H13 H 0.064(4) 0.790(5) 0.744(5) 0.105 Uiso 1 1 d DR . . . .
O24 O 0.1082(7) 0.8696(6) 0.3690(6) 0.0851(19) Uani 1 1 d . . . . .
N1 N 0.4527(6) 0.6628(5) 0.4282(5) 0.0542(16) Uani 1 1 d . . . . .
N2 N 0.5601(6) 0.8511(5) 0.5398(4) 0.0491(14) Uani 1 1 d . . . . .
N3 N 0.1784(7) 0.8149(6) 0.4134(5) 0.0631(19) Uani 1 1 d . . . . .
N4 N 0.5473(9) 0.7050(7) 0.8689(7) 0.081(2) Uani 1 1 d . . . . .
C1 C 0.0488(8) 0.4955(6) 0.7043(6) 0.058(2) Uani 1 1 d . . . . .
H1A H 0.0780 0.4307 0.7217 0.086 Uiso 1 1 calc GR . . . .
H1B H -0.0285 0.4777 0.6534 0.086 Uiso 1 1 calc GR . . . .
H1C H 0.0340 0.5404 0.7680 0.086 Uiso 1 1 calc GR . . . .
C2 C 0.1718(7) 0.4986(6) 0.5677(5) 0.0492(17) Uani 1 1 d . . . . .
C3 C 0.1136(7) 0.4029(6) 0.5113(6) 0.0508(17) Uani 1 1 d . . . . .
H3 H 0.0458 0.3669 0.5335 0.061 Uiso 1 1 calc R . . . .
C4 C 0.1566(7) 0.3591(6) 0.4198(6) 0.0546(19) Uani 1 1 d . . . . .
H4 H 0.1182 0.2925 0.3803 0.066 Uiso 1 1 calc R . . . .
C5 C 0.2532(7) 0.4115(5) 0.3875(5) 0.0502(17) Uani 1 1 d . . . . .
H5 H 0.2829 0.3792 0.3272 0.060 Uiso 1 1 calc R . . . .
C6 C 0.3100(7) 0.5126(5) 0.4413(5) 0.0488(17) Uani 1 1 d . . . . .
C7 C 0.2684(7) 0.5568(5) 0.5343(5) 0.0481(17) Uani 1 1 d . . . . .
C8 C 0.4103(7) 0.5642(5) 0.4013(5) 0.0530(19) Uani 1 1 d . . . . .
H8 H 0.4477 0.5221 0.3514 0.064 Uiso 1 1 calc R . . . .
C9 C 0.5560(13) 0.7115(8) 0.3885(9) 0.107(5) Uani 1 1 d . . . . .
H9 H 0.6175 0.6755 0.4291 0.128 Uiso 1 1 calc R . . . .
C10 C 0.5888(8) 0.6665(7) 0.2893(6) 0.063(2) Uani 1 1 d . . . . .
H10A H 0.5167 0.6637 0.2335 0.075 Uiso 1 1 calc R . . . .
H10B H 0.6042 0.5929 0.2914 0.075 Uiso 1 1 calc R . . . .
C11 C 0.6992(11) 0.7229(7) 0.2593(8) 0.085(3) Uani 1 1 d . . . . .
H11A H 0.7648 0.6759 0.2613 0.102 Uiso 1 1 calc R . . . .
H11B H 0.6758 0.7300 0.1853 0.102 Uiso 1 1 calc R . . . .
C12 C 0.7537(12) 0.8242(9) 0.3167(9) 0.102(4) Uani 1 1 d . . . . .
H12A H 0.7371 0.8757 0.2703 0.122 Uiso 1 1 calc R . . . .
H12B H 0.8445 0.8233 0.3296 0.122 Uiso 1 1 calc R . . . .
C13 C 0.7182(9) 0.8664(7) 0.4177(7) 0.067(2) Uani 1 1 d . . . . .
H13A H 0.7889 0.8662 0.4739 0.080 Uiso 1 1 calc R . . . .
H13B H 0.7051 0.9410 0.4183 0.080 Uiso 1 1 calc R . . . .
C14 C 0.6089(9) 0.8123(7) 0.4441(7) 0.078(3) Uani 1 1 d . . . . .
H14 H 0.5514 0.8487 0.4000 0.094 Uiso 1 1 calc R . . . .
C15 C 0.6149(7) 0.9300(6) 0.6088(6) 0.0534(18) Uani 1 1 d . . . . .
H15 H 0.6920 0.9625 0.5983 0.064 Uiso 1 1 calc R . . . .
C16 C 0.5676(7) 0.9737(5) 0.7026(5) 0.0496(17) Uani 1 1 d . . . . .
C17 C 0.6288(8) 1.0719(6) 0.7623(6) 0.0564(19) Uani 1 1 d . . . . .
H17 H 0.6998 1.1047 0.7418 0.068 Uiso 1 1 calc R . . . .
C18 C 0.5865(8) 1.1195(6) 0.8489(6) 0.064(2) Uani 1 1 d . . . . .
H18 H 0.6262 1.1867 0.8858 0.077 Uiso 1 1 calc R . . . .
C19 C 0.4880(8) 1.0720(6) 0.8835(6) 0.0563(19) Uani 1 1 d . . . . .
H19 H 0.4604 1.1060 0.9442 0.068 Uiso 1 1 calc R . . . .
C20 C 0.4285(7) 0.9747(6) 0.8300(5) 0.0505(17) Uani 1 1 d . . . . .
C21 C 0.4648(7) 0.9260(6) 0.7363(5) 0.0490(17) Uani 1 1 d . . . . .
C22 C 0.2628(8) 0.9730(7) 0.9288(6) 0.065(2) Uani 1 1 d . . . . .
H22A H 0.1871 0.9278 0.9319 0.097 Uiso 1 1 calc GR . . . .
H22B H 0.2408 1.0377 0.9056 0.097 Uiso 1 1 calc GR . . . .
H22C H 0.3144 0.9911 0.9984 0.097 Uiso 1 1 calc GR . . . .
C25 C 0.1053(10) 0.8750(8) 0.6528(8) 0.079(3) Uani 1 1 d D . . . .
H25A H 0.0481 0.8502 0.5864 0.119 Uiso 1 1 calc GR . . . .
H25B H 0.1856 0.9036 0.6387 0.119 Uiso 1 1 calc GR . . . .
H25C H 0.0715 0.9303 0.6965 0.119 Uiso 1 1 calc GR . . . .
C27 C 0.3094(9) 0.5320(7) 0.9188(7) 0.071(2) Uani 1 1 d . . . . .
H27 H 0.3449 0.4724 0.9369 0.085 Uiso 1 1 calc R . . . .
C28 C 0.2451(9) 0.5853(7) 0.9934(7) 0.069(2) Uani 1 1 d . . . . .
C29 C 0.2450(11) 0.5486(8) 1.0895(8) 0.080(3) Uani 1 1 d . . . . .
H29 H 0.2885 0.4909 1.1017 0.096 Uiso 1 1 calc R . . . .
C30 C 0.1847(11) 0.5939(9) 1.1633(8) 0.086(3) Uani 1 1 d . . . . .
H30 H 0.1882 0.5701 1.2280 0.103 Uiso 1 1 calc R . . . .
C31 C 0.1160(10) 0.6772(9) 1.1444(7) 0.081(3) Uani 1 1 d . . . . .
H31 H 0.0726 0.7084 1.1964 0.097 Uiso 1 1 calc R . . . .
C32 C 0.1112(9) 0.7140(8) 1.0506(7) 0.068(2) Uani 1 1 d . . . . .
C33 C 0.1824(7) 0.6689(6) 0.9747(6) 0.054(2) Uani 1 1 d . . . . .
C34 C -0.0208(15) 0.8383(15) 1.1024(10) 0.148(7) Uani 1 1 d . . . . .
H34A H -0.0452 0.9052 1.0864 0.222 Uiso 1 1 calc GR . . . .
H34B H 0.0308 0.8510 1.1719 0.222 Uiso 1 1 calc GR . . . .
H34C H -0.0951 0.7895 1.1013 0.222 Uiso 1 1 calc GR . . . .
O14 O -0.0475(8) 0.8181(11) 0.8250(7) 0.127(4) Uani 1 1 d . . . . .
H14A H -0.0264 0.8027 0.8841 0.191 Uiso 1 1 calc GR . . A 1
C26 C -0.1571(13) 0.8604(13) 0.8224(11) 0.126(5) Uani 1 1 d . . . . .
H26A H -0.1744 0.8895 0.7584 0.189 Uiso 1 1 calc GR . . . .
H26B H -0.1508 0.9168 0.8837 0.189 Uiso 1 1 calc GR . . . .
H26C H -0.2244 0.8053 0.8232 0.189 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 Zn1 3.4708(11) . ?
Y1 O1 2.597(5) . ?
Y1 O2 2.288(4) . ?
Y1 O3 2.287(5) . ?
Y1 O4 2.696(5) . ?
Y1 O7 2.426(6) . ?
Y1 O8 2.233(5) . ?
Y1 O10 2.588(8) . ?
Y1 O11 2.392(6) . ?
Y1 O13 2.351(7) . ?
Y1 N4 2.921(10) . ?
Zn1 O2 2.006(5) . ?
Zn1 O3 2.016(4) . ?
Zn1 O5 2.007(6) . ?
Zn1 N1 2.034(6) . ?
Zn1 N2 2.036(6) . ?
O1 C1 1.448(9) . ?
O1 C2 1.387(8) . ?
O2 C7 1.318(8) . ?
O3 C21 1.339(8) . ?
O4 C20 1.370(9) . ?
O4 C22 1.436(9) . ?
O5 N3 1.260(9) . ?
O6 N3 1.219(10) . ?
O7 C27 1.234(11) . ?
O8 C33 1.331(10) . ?
O9 C32 1.360(12) . ?
O9 C34 1.421(12) . ?
O10 N4 1.251(11) . ?
O11 N4 1.264(11) . ?
O12 N4 1.214(12) . ?
O13 H13 0.863(10) . ?
O13 C25 1.404(12) . ?
O24 N3 1.247(10) . ?
N1 C8 1.286(10) . ?
N1 C9 1.454(11) . ?
N2 C14 1.472(9) . ?
N2 C15 1.276(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.374(10) . ?
C2 C7 1.409(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.409(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.413(10) . ?
C6 C7 1.420(10) . ?
C6 C8 1.447(11) . ?
C8 H8 0.9500 . ?
C9 H9 1.0000 . ?
C9 C10 1.447(11) . ?
C9 C14 1.407(12) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.495(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.424(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.472(12) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.450(11) . ?
C14 H14 1.0000 . ?
C15 H15 0.9500 . ?
C15 C16 1.458(10) . ?
C16 C17 1.421(10) . ?
C16 C21 1.403(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.369(12) . ?
C18 H18 0.9500 . ?
C18 C19 1.369(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.382(10) . ?
C20 C21 1.417(10) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 H27 0.9500 . ?
C27 C28 1.420(13) . ?
C28 C29 1.425(14) . ?
C28 C33 1.379(13) . ?
C29 H29 0.9500 . ?
C29 C30 1.344(15) . ?
C30 H30 0.9500 . ?
C30 C31 1.413(16) . ?
C31 H31 0.9500 . ?
C31 C32 1.392(14) . ?
C32 C33 1.442(11) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O14 H14A 0.8400 . ?
O14 C26 1.374(15) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 Zn1 92.12(11) . . ?
O1 Y1 O4 147.34(18) . . ?
O1 Y1 N4 125.9(2) . . ?
O2 Y1 Zn1 33.42(12) . . ?
O2 Y1 O1 61.90(16) . . ?
O2 Y1 O4 125.76(17) . . ?
O2 Y1 O7 97.75(19) . . ?
O2 Y1 O10 74.5(2) . . ?
O2 Y1 O11 123.5(2) . . ?
O2 Y1 O13 91.1(2) . . ?
O2 Y1 N4 99.5(2) . . ?
O3 Y1 Zn1 33.67(11) . . ?
O3 Y1 O1 124.55(16) . . ?
O3 Y1 O2 66.81(16) . . ?
O3 Y1 O4 60.82(15) . . ?
O3 Y1 O7 140.5(2) . . ?
O3 Y1 O10 74.9(2) . . ?
O3 Y1 O11 86.1(2) . . ?
O3 Y1 O13 84.3(2) . . ?
O3 Y1 N4 81.2(2) . . ?
O4 Y1 Zn1 92.72(11) . . ?
O4 Y1 N4 86.0(2) . . ?
O7 Y1 Zn1 125.12(14) . . ?
O7 Y1 O1 67.85(19) . . ?
O7 Y1 O4 131.79(18) . . ?
O7 Y1 O10 65.8(2) . . ?
O7 Y1 N4 65.2(2) . . ?
O8 Y1 Zn1 159.08(15) . . ?
O8 Y1 O1 85.56(17) . . ?
O8 Y1 O2 146.95(19) . . ?
O8 Y1 O3 138.70(18) . . ?
O8 Y1 O4 78.61(17) . . ?
O8 Y1 O7 73.0(2) . . ?
O8 Y1 O10 125.6(2) . . ?
O8 Y1 O11 84.7(2) . . ?
O8 Y1 O13 75.1(2) . . ?
O8 Y1 N4 104.6(2) . . ?
O10 Y1 Zn1 74.79(16) . . ?
O10 Y1 O1 108.9(2) . . ?
O10 Y1 O4 103.6(2) . . ?
O10 Y1 N4 25.3(2) . . ?
O11 Y1 Zn1 109.50(17) . . ?
O11 Y1 O1 140.2(2) . . ?
O11 Y1 O4 66.79(19) . . ?
O11 Y1 O7 72.4(2) . . ?
O11 Y1 O10 50.3(2) . . ?
O11 Y1 N4 25.1(2) . . ?
O13 Y1 Zn1 84.07(15) . . ?
O13 Y1 O1 77.2(2) . . ?
O13 Y1 O4 71.21(19) . . ?
O13 Y1 O7 133.8(2) . . ?
O13 Y1 O10 158.1(2) . . ?
O13 Y1 O11 136.2(2) . . ?
O13 Y1 N4 156.9(2) . . ?
N4 Y1 Zn1 93.58(17) . . ?
O2 Zn1 Y1 38.91(12) . . ?
O2 Zn1 O3 77.53(19) . . ?
O2 Zn1 O5 119.4(2) . . ?
O2 Zn1 N1 90.0(2) . . ?
O2 Zn1 N2 140.8(3) . . ?
O3 Zn1 Y1 38.96(14) . . ?
O3 Zn1 N1 148.9(3) . . ?
O3 Zn1 N2 89.4(2) . . ?
O5 Zn1 Y1 112.42(17) . . ?
O5 Zn1 O3 101.4(2) . . ?
O5 Zn1 N1 109.5(3) . . ?
O5 Zn1 N2 99.2(3) . . ?
N1 Zn1 Y1 125.47(19) . . ?
N1 Zn1 N2 82.5(2) . . ?
N2 Zn1 Y1 122.07(17) . . ?
C1 O1 Y1 123.9(4) . . ?
C2 O1 Y1 117.1(4) . . ?
C2 O1 C1 116.5(5) . . ?
Zn1 O2 Y1 107.67(19) . . ?
C7 O2 Y1 129.1(4) . . ?
C7 O2 Zn1 122.1(4) . . ?
Zn1 O3 Y1 107.37(19) . . ?
C21 O3 Y1 127.7(4) . . ?
C21 O3 Zn1 124.6(4) . . ?
C20 O4 Y1 113.4(4) . . ?
C20 O4 C22 117.2(6) . . ?
C22 O4 Y1 129.4(5) . . ?
N3 O5 Zn1 118.8(5) . . ?
C27 O7 Y1 130.3(6) . . ?
C33 O8 Y1 136.0(5) . . ?
C32 O9 C34 116.0(9) . . ?
N4 O10 Y1 92.4(6) . . ?
N4 O11 Y1 101.6(5) . . ?
Y1 O13 H13 115.5(18) . . ?
C25 O13 Y1 132.7(6) . . ?
C25 O13 H13 105.4(19) . . ?
C8 N1 Zn1 124.9(5) . . ?
C8 N1 C9 123.5(6) . . ?
C9 N1 Zn1 111.4(5) . . ?
C14 N2 Zn1 109.8(5) . . ?
C15 N2 Zn1 127.2(5) . . ?
C15 N2 C14 122.8(6) . . ?
O6 N3 O5 119.0(8) . . ?
O6 N3 O24 121.4(8) . . ?
O24 N3 O5 119.6(7) . . ?
O10 N4 Y1 62.3(5) . . ?
O10 N4 O11 115.2(9) . . ?
O11 N4 Y1 53.3(4) . . ?
O12 N4 Y1 173.8(8) . . ?
O12 N4 O10 123.1(10) . . ?
O12 N4 O11 121.6(9) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C7 112.1(6) . . ?
C3 C2 O1 125.6(7) . . ?
C3 C2 C7 122.3(6) . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.5(7) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.8(6) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C7 118.0(7) . . ?
C5 C6 C8 118.7(6) . . ?
C7 C6 C8 123.2(6) . . ?
O2 C7 C2 116.8(6) . . ?
O2 C7 C6 124.6(7) . . ?
C2 C7 C6 118.6(6) . . ?
N1 C8 C6 125.0(6) . . ?
N1 C8 H8 117.5 . . ?
C6 C8 H8 117.5 . . ?
N1 C9 H9 92.8 . . ?
C10 C9 N1 121.7(7) . . ?
C10 C9 H9 92.8 . . ?
C14 C9 N1 115.5(7) . . ?
C14 C9 H9 92.8 . . ?
C14 C9 C10 122.1(8) . . ?
C9 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
C9 C10 C11 116.2(7) . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
C10 C11 H11A 107.2 . . ?
C10 C11 H11B 107.2 . . ?
H11A C11 H11B 106.8 . . ?
C12 C11 C10 120.6(7) . . ?
C12 C11 H11A 107.2 . . ?
C12 C11 H11B 107.2 . . ?
C11 C12 H12A 107.2 . . ?
C11 C12 H12B 107.2 . . ?
C11 C12 C13 120.5(8) . . ?
H12A C12 H12B 106.8 . . ?
C13 C12 H12A 107.2 . . ?
C13 C12 H12B 107.2 . . ?
C12 C13 H13A 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C14 C13 C12 117.1(8) . . ?
C14 C13 H13A 108.0 . . ?
C14 C13 H13B 108.0 . . ?
N2 C14 H14 92.9 . . ?
C9 C14 N2 116.1(7) . . ?
C9 C14 C13 121.2(7) . . ?
C9 C14 H14 92.9 . . ?
C13 C14 N2 121.9(7) . . ?
C13 C14 H14 92.9 . . ?
N2 C15 H15 117.6 . . ?
N2 C15 C16 124.7(7) . . ?
C16 C15 H15 117.6 . . ?
C17 C16 C15 117.6(7) . . ?
C21 C16 C15 124.2(6) . . ?
C21 C16 C17 118.3(6) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.7(8) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 119.4 . . ?
C17 C18 C19 121.2(7) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(7) . . ?
C20 C19 H19 120.0 . . ?
O4 C20 C19 126.3(6) . . ?
O4 C20 C21 113.3(6) . . ?
C19 C20 C21 120.4(7) . . ?
O3 C21 C16 124.6(6) . . ?
O3 C21 C20 116.0(7) . . ?
C16 C21 C20 119.3(6) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O13 C25 H25A 109.5 . . ?
O13 C25 H25B 109.5 . . ?
O13 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O7 C27 H27 116.0 . . ?
O7 C27 C28 128.1(10) . . ?
C28 C27 H27 116.0 . . ?
C27 C28 C29 117.8(9) . . ?
C33 C28 C27 122.3(9) . . ?
C33 C28 C29 120.0(9) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 C28 121.3(10) . . ?
C30 C29 H29 119.4 . . ?
C29 C30 H30 120.1 . . ?
C29 C30 C31 119.8(10) . . ?
C31 C30 H30 120.1 . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.8(9) . . ?
C32 C31 H31 119.6 . . ?
O9 C32 C31 124.6(8) . . ?
O9 C32 C33 116.6(8) . . ?
C31 C32 C33 118.8(9) . . ?
O8 C33 C28 124.3(7) . . ?
O8 C33 C32 116.5(8) . . ?
C28 C33 C32 119.2(8) . . ?
O9 C34 H34A 109.5 . . ?
O9 C34 H34B 109.5 . . ?
O9 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C26 O14 H14A 109.5 . . ?
O14 C26 H26A 109.5 . . ?
O14 C26 H26B 109.5 . . ?
O14 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_olex2_date_sample_data_collection 2017-11-17
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.644
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1820466'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2017-07-27
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 Cl Dy N4 O11 Zn'
_chemical_formula_sum            'C24 H30 Cl Dy N4 O11 Zn'
_chemical_formula_weight         813.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C92 H108 Cl4 Dy4 N12 O44 Zn4 '
_chemical_oxdiff_usercomment     SS419
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'
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'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   16.1433(4)
_cell_length_b                   8.2376(2)
_cell_length_c                   24.0684(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.819(2)
_cell_angle_gamma                90
_cell_volume                     3193.56(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3310
_cell_measurement_theta_min      3.2130
_shelx_estimated_absorpt_T_max   0.669
_shelx_estimated_absorpt_T_min   0.323
_exptl_absorpt_coefficient_mu    14.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_recrystallization_method 
'The material was recrystallised from ethanol by slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.056
_diffrn_reflns_theta_min         3.200
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  27.00   0.50    3.00    --    0.00  60.00-150.00  130
  2  ω    -84.00 -54.00   0.50    3.00    --    0.00  60.00-150.00   60
  3  ω    -68.00  88.00   0.50    3.00    --    0.00  60.00 -90.00  312
  4  ω   -174.00-103.00   0.50   12.00    --  -90.00  20.00 -94.27  142
  5  ω   -164.00-119.00   0.50   12.00    --  -90.00  60.00-150.00   90
  6  ω    -89.00  -6.00   0.50   12.00    --  -90.00  60.00-150.00  166
  7  ω   -178.00  -2.00   0.50   12.00    --  -90.00   0.00  60.00  352
  8  ω    -26.00  -1.00   0.50   12.00    --  -90.00  60.00 -30.00   50
  9  ω   -178.00-115.00   0.50   12.00    --  -90.00  57.00-120.00  126
 10  ω    -30.00  -3.00   0.50   12.00    --  -90.00  29.00  30.00   54
 11  ω   -178.00-136.00   0.50   12.00    --  -90.00  60.00 120.00   84
 12  ω   -129.00 -91.00   0.50   12.00    --  -90.00  60.00 120.00   76
 13  ω    -40.00 -15.00   0.50   12.00    --  -90.00  60.00 120.00   50
 14  ω   -173.00 -27.00   0.50   12.00    --  -90.00  60.00 -90.00  292
 15  ω    -61.00 -30.00   0.50   12.00    --  -90.00  57.00 150.00   62
 16  ω   -170.00-134.00   0.50   12.00    --  -90.00  60.00   0.00   72
 17  ω   -161.00-123.00   0.50   12.00    --  -90.00  59.00   5.98   76
 18  ω    -84.00 -41.00   0.50   12.00    --  -90.00  59.00   5.98   86
 19  ω   -110.00 -85.00   0.50   12.00    --  -90.00  57.00-120.00   50
 20  ω   -118.00 -76.00   0.50   12.00    --  -90.00  29.00  30.00   84
 21  ω   -144.00 -77.00   0.50   12.00    --  -90.00  57.00 -60.00  134
 22  ω   -177.00-151.00   0.50   12.00    --  -90.00  60.00 -60.00   52
 23  ω   -143.00-118.00   0.50   12.00    --  -90.00  60.00 -60.00   50
 24  ω    -55.00 -28.00   0.50   12.00    --  -90.00  60.00 -60.00   54
 25  ω   -169.00 -84.00   0.50   12.00    --  -90.00  60.00-180.00  170
 26  ω    -76.00 -51.00   0.50   12.00    --  -90.00  60.00-180.00   50
 27  ω   -171.00-138.00   0.50   12.00    --  -90.00  43.00  90.00   66
 28  ω   -102.00 -62.00   0.50   12.00    --  -90.00  43.00  90.00   80
 29  ω    -44.00 -13.00   0.50   12.00    --  -90.00  43.00  90.00   62
 30  ω   -175.00-131.00   0.50   12.00    --  -90.00  14.00  90.00   88
 31  ω   -115.00 -88.00   0.50   12.00    --  -90.00  14.00  90.00   54
 32  ω   -173.00 -74.00   0.50   12.00    --  -90.00  57.00 150.00  198
 33  ω    -44.00 -19.00   0.50   12.00    --  -90.00  60.00   0.00   50
 34  ω   -134.00-103.00   0.50   12.00    --  -90.00  43.00-150.00   62
 35  ω    -53.00 -12.00   0.50   12.00    --  -90.00  43.00-150.00   82
 36  ω   -177.00-150.00   0.50   12.00    --  -90.00  57.00-180.00   54
 37  ω   -132.00-107.00   0.50   12.00    --  -90.00  57.00-180.00   50
 38  ω    -35.00 -10.00   0.50   12.00    --  -90.00  57.00-180.00   50
 39  ω   -170.00 -84.00   0.50   12.00    --  -90.00  60.00 -30.00  172
 40  ω    -40.00 -13.00   0.50   12.00    --  -90.00  20.00 -94.27   54
 41  ω    -54.00 -27.00   0.50   12.00    --  -90.00   0.00 -90.00   54
 42  ω   -168.00-102.00   0.50   12.00    --  -90.00  60.00  60.00  132
 43  ω   -110.00 -85.00   0.50   12.00    --  -90.00  59.00  44.92   50
 44  ω   -151.00  -1.00   0.50   12.00    --  -90.00  43.00 120.00  300
 45  ω   -136.00-109.00   0.50   12.00    --  -90.00  57.00   0.00   54
 46  ω   -155.00-128.00   0.50   12.00    --  -90.00  57.00  90.00   54
 47  ω   -103.00 -78.00   0.50   12.00    --  -90.00  57.00  90.00   50
 48  ω   -124.00 -97.00   0.50   12.00    --  -90.00  43.00 -30.00   54
 49  ω    -43.00 -18.00   0.50   12.00    --  -90.00  43.00 -30.00   50
 50  ω   -104.00 -75.00   0.50   12.00    --  -90.00  43.00   0.00   58
 51  ω    -40.00 -15.00   0.50   12.00    --  -90.00  43.00   0.00   50
 52  ω   -167.00-142.00   0.50   12.00    --  -90.00  59.00  44.92   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0793248000
_diffrn_orient_matrix_UB_12      -0.0650390000
_diffrn_orient_matrix_UB_13      0.0244687000
_diffrn_orient_matrix_UB_21      0.0455927000
_diffrn_orient_matrix_UB_22      -0.1587580000
_diffrn_orient_matrix_UB_23      0.0166340000
_diffrn_orient_matrix_UB_31      0.0279970000
_diffrn_orient_matrix_UB_32      0.0743398000
_diffrn_orient_matrix_UB_33      0.0569067000
_diffrn_oxdiff_ac3_digest_frames 
;
01f9e576944edae6512df99d104723c5230500274eb
;
_diffrn_oxdiff_ac3_digest_hkl    
;
01bd4d5c64dd6d7b408b38c65f77f4d2f63024
;
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4957
_reflns_number_total             6046
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.716
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     630
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      1.079
_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)+(0.0996P)²+1.3153P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1601
_refine_special_details          
'Distance and angle restraints applied to O5-H5. Cyclohexane moiety of ligand disordered over two positions, approx. ratio 68:32. Electronic contribution from unknown solvent (likely EtOH or H2O) accounted for with SMTBX solvent masking routine as implemented within Olex2.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C23-H5
 1.925921 with sigma of 0.02
 Dy1-H5
 2.817452 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(H4BC)=Sof(H4BD)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6B)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C6A(H6A), C6B(H6B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), C5A(H5AA,H5AB), C5B(H5BA,H5BB), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C10(H10), C11(H11), C15(H15), C17(H17), C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.22246(2) 0.24906(4) 0.50114(2) 0.04828(15) Uani 1 1 d D U . . .
Zn1 Zn 0.32616(4) 0.32334(9) 0.38119(3) 0.0509(2) Uani 1 1 d . U . . .
Cl1 Cl 0.32480(8) 0.07073(17) 0.34258(5) 0.0573(3) Uani 1 1 d . U . . .
O1 O 0.3462(2) 0.2821(5) 0.46425(15) 0.0473(8) Uani 1 1 d . U . . .
O2 O 0.3483(2) 0.1106(4) 0.55220(14) 0.0496(8) Uani 1 1 d . U . . .
O3 O 0.2136(2) 0.3570(5) 0.41306(14) 0.0556(9) Uani 1 1 d . U . . .
O4 O 0.0783(2) 0.2805(5) 0.45470(18) 0.0569(9) Uani 1 1 d . U . . .
O5 O 0.2260(2) 0.0090(5) 0.44686(16) 0.0601(9) Uani 1 1 d D U . . .
H5 H 0.249(4) 0.024(4) 0.4163(14) 0.090 Uiso 1 1 d DR . . . .
O6 O 0.1469(3) 0.0407(6) 0.54520(18) 0.0681(11) Uani 1 1 d . U . . .
O7 O 0.1745(6) 0.2422(6) 0.5965(3) 0.114(3) Uani 1 1 d . U . . .
O8 O 0.1031(3) 0.0426(7) 0.6275(2) 0.0975(17) Uani 1 1 d . U . . .
O9 O 0.1695(3) 0.5127(6) 0.5234(2) 0.0795(13) Uani 1 1 d . U . . .
O10 O 0.2902(2) 0.4541(6) 0.56117(19) 0.0724(11) Uani 1 1 d . U . . .
O11 O 0.2279(4) 0.6746(7) 0.5844(3) 0.0963(16) Uani 1 1 d . U . . .
N1 N 0.4370(3) 0.4422(6) 0.38300(19) 0.0625(12) Uani 1 1 d . U . . .
N2 N 0.2938(3) 0.4980(6) 0.3241(2) 0.0658(12) Uani 1 1 d . U . . .
N3 N 0.1385(3) 0.1067(8) 0.5917(2) 0.0744(13) Uani 1 1 d . U . . .
N4 N 0.2291(3) 0.5527(7) 0.5573(2) 0.0686(12) Uani 1 1 d . U . . .
C1A C 0.4290(8) 0.5925(15) 0.3412(4) 0.066(2) Uani 0.667(8) 1 d . U P A 1
H1A H 0.410813 0.688824 0.362582 0.079 Uiso 0.667(8) 1 calc R . P A 1
C1B C 0.3798(13) 0.612(2) 0.3218(9) 0.053(3) Uani 0.333(8) 1 d . U P A 2
H1B H 0.377086 0.701267 0.349707 0.064 Uiso 0.333(8) 1 calc R . P A 2
C2A C 0.5112(6) 0.6361(13) 0.3163(4) 0.070(2) Uani 0.667(8) 1 d . U P A 1
H2AA H 0.504999 0.741790 0.296853 0.084 Uiso 0.667(8) 1 calc R . P A 1
H2AB H 0.555022 0.648128 0.346776 0.084 Uiso 0.667(8) 1 calc R . P A 1
C2B C 0.3826(11) 0.686(2) 0.2652(7) 0.058(4) Uani 0.333(8) 1 d . U P A 2
H2BA H 0.328678 0.739814 0.255507 0.069 Uiso 0.333(8) 1 calc R . P A 2
H2BB H 0.425878 0.771791 0.266918 0.069 Uiso 0.333(8) 1 calc R . P A 2
C3A C 0.5378(6) 0.5082(15) 0.2756(4) 0.078(3) Uani 0.667(8) 1 d . U P A 1
H3AA H 0.589611 0.544073 0.259509 0.094 Uiso 0.667(8) 1 calc R . P A 1
H3AB H 0.549674 0.405507 0.295899 0.094 Uiso 0.667(8) 1 calc R . P A 1
C3B C 0.3999(11) 0.572(2) 0.2201(6) 0.060(4) Uani 0.333(8) 1 d . U P A 2
H3BA H 0.352425 0.496525 0.214332 0.072 Uiso 0.333(8) 1 calc R . P A 2
H3BB H 0.404165 0.634182 0.185184 0.072 Uiso 0.333(8) 1 calc R . P A 2
C4 C 0.4747(4) 0.4785(9) 0.2306(3) 0.0704(16) Uani 1 1 d . U . . .
H4AA H 0.493506 0.389614 0.206773 0.084 Uiso 0.667(8) 1 calc R . P A 1
H4AB H 0.468004 0.577316 0.207250 0.084 Uiso 0.667(8) 1 calc R . P A 1
H4BC H 0.523555 0.550469 0.228813 0.084 Uiso 0.333(8) 1 calc R . P A 2
H4BD H 0.477861 0.394313 0.201439 0.084 Uiso 0.333(8) 1 calc R . P A 2
C5A C 0.3876(6) 0.4314(13) 0.2528(3) 0.066(2) Uani 0.667(8) 1 d . U P A 1
H5AA H 0.345584 0.422823 0.221035 0.079 Uiso 0.667(8) 1 calc R . P A 1
H5AB H 0.391916 0.324245 0.271405 0.079 Uiso 0.667(8) 1 calc R . P A 1
C5B C 0.4763(10) 0.393(2) 0.2909(6) 0.054(4) Uani 0.333(8) 1 d . U P A 2
H5BA H 0.433831 0.306385 0.290056 0.065 Uiso 0.333(8) 1 calc R . P A 2
H5BB H 0.531223 0.341920 0.299113 0.065 Uiso 0.333(8) 1 calc R . P A 2
C6A C 0.3601(6) 0.5572(13) 0.2935(4) 0.060(2) Uani 0.667(8) 1 d . U P A 1
H6A H 0.343402 0.659767 0.273505 0.072 Uiso 0.667(8) 1 calc R . P A 1
C6B C 0.4601(11) 0.510(3) 0.3366(7) 0.052(3) Uani 0.333(8) 1 d . U P A 2
H6B H 0.509041 0.582939 0.344574 0.063 Uiso 0.333(8) 1 calc R . P A 2
C7 C 0.4979(4) 0.4215(8) 0.4199(2) 0.0609(13) Uani 1 1 d . U . . .
H7 H 0.547635 0.480603 0.415737 0.073 Uiso 1 1 calc R . . . .
C8 C 0.4952(3) 0.3141(7) 0.4672(2) 0.0533(11) Uani 1 1 d . U . . .
C9 C 0.5716(4) 0.2757(7) 0.4966(3) 0.0628(15) Uani 1 1 d . U . . .
H9 H 0.621948 0.319332 0.484675 0.075 Uiso 1 1 calc R . . . .
C10 C 0.5733(4) 0.1761(8) 0.5423(3) 0.0662(14) Uani 1 1 d . U . . .
H10 H 0.625390 0.145617 0.559914 0.079 Uiso 1 1 calc R . . . .
C11 C 0.5007(3) 0.1180(7) 0.5636(3) 0.0578(12) Uani 1 1 d . U . . .
H11 H 0.502805 0.052198 0.596085 0.069 Uiso 1 1 calc R . . . .
C12 C 0.4257(3) 0.1587(6) 0.5363(2) 0.0506(11) Uani 1 1 d . U . . .
C13 C 0.4217(3) 0.2544(6) 0.4879(3) 0.0472(12) Uani 1 1 d . U . . .
C14 C 0.3473(4) 0.0100(7) 0.6013(2) 0.0604(13) Uani 1 1 d . U . . .
H14A H 0.368969 0.071909 0.633832 0.091 Uiso 1 1 calc GR . . . .
H14B H 0.382015 -0.085964 0.596662 0.091 Uiso 1 1 calc GR . . . .
H14C H 0.290200 -0.024080 0.606589 0.091 Uiso 1 1 calc GR . . . .
C15 C 0.2201(4) 0.5407(8) 0.3077(3) 0.0715(16) Uani 1 1 d . U . . .
H15 H 0.213786 0.618275 0.278555 0.086 Uiso 1 1 calc R . . . .
C16 C 0.1463(4) 0.4797(9) 0.3303(3) 0.0702(16) Uani 1 1 d . U . . .
C17 C 0.0678(5) 0.5145(12) 0.3025(3) 0.099(3) Uani 1 1 d . U . . .
H17 H 0.066026 0.569599 0.267784 0.119 Uiso 1 1 calc R . . . .
C18 C -0.0038(5) 0.4721(13) 0.3238(4) 0.106(3) Uani 1 1 d . U . . .
H18 H -0.054618 0.497144 0.303413 0.127 Uiso 1 1 calc R . . . .
C19 C -0.0060(4) 0.3927(11) 0.3745(3) 0.084(2) Uani 1 1 d . U . . .
H19 H -0.057173 0.363841 0.389128 0.101 Uiso 1 1 calc R . . . .
C20 C 0.0689(3) 0.3572(8) 0.4030(2) 0.0614(14) Uani 1 1 d . U . . .
C21 C 0.1452(3) 0.3973(8) 0.3820(2) 0.0583(13) Uani 1 1 d . U . . .
C22 C 0.0018(5) 0.2520(9) 0.4803(4) 0.087(3) Uani 1 1 d . U . . .
H22A H 0.013593 0.202833 0.517040 0.131 Uiso 1 1 calc GR . . . .
H22B H -0.033172 0.178458 0.456883 0.131 Uiso 1 1 calc GR . . . .
H22C H -0.027312 0.355282 0.484404 0.131 Uiso 1 1 calc GR . . . .
C23 C 0.1877(4) -0.1525(9) 0.4451(3) 0.0762(17) Uani 1 1 d D U . . .
H23A H 0.227892 -0.232892 0.432336 0.091 Uiso 1 1 calc R . . . .
H23B H 0.173597 -0.183719 0.483076 0.091 Uiso 1 1 calc R . . . .
C24 C 0.1127(5) -0.1550(12) 0.4077(3) 0.092(2) Uani 1 1 d . U . . .
H24A H 0.126803 -0.126491 0.369970 0.137 Uiso 1 1 calc GR . . . .
H24B H 0.072632 -0.076379 0.420584 0.137 Uiso 1 1 calc GR . . . .
H24C H 0.088247 -0.263968 0.407508 0.137 Uiso 1 1 calc GR . . . .


_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 Zn1 3.4865(7) . ?
Dy1 O1 2.255(4) . ?
Dy1 O2 2.570(3) . ?
Dy1 O3 2.294(3) . ?
Dy1 O4 2.527(4) . ?
Dy1 O5 2.373(4) . ?
Dy1 O6 2.394(4) . ?
Dy1 O7 2.470(6) . ?
Dy1 O9 2.408(4) . ?
Dy1 O10 2.434(4) . ?
Dy1 N3 2.890(5) . ?
Dy1 N4 2.842(5) . ?
Zn1 Cl1 2.2785(16) . ?
Zn1 O1 2.032(4) . ?
Zn1 O3 2.037(3) . ?
Zn1 N1 2.038(5) . ?
Zn1 N2 2.034(5) . ?
O1 C13 1.331(7) . ?
O2 C12 1.389(6) . ?
O2 C14 1.443(6) . ?
O3 C21 1.333(6) . ?
O4 C20 1.394(7) . ?
O4 C22 1.436(9) . ?
O5 H5 0.854(9) . ?
O5 C23 1.466(8) . ?
O6 N3 1.259(7) . ?
O7 N3 1.260(8) . ?
O8 N3 1.191(7) . ?
O9 N4 1.262(7) . ?
O10 N4 1.277(7) . ?
O11 N4 1.198(7) . ?
N1 C1A 1.595(13) . ?
N1 C6B 1.325(17) . ?
N1 C7 1.292(8) . ?
N2 C1B 1.68(2) . ?
N2 C6A 1.426(9) . ?
N2 C15 1.277(8) . ?
C1A H1A 1.0000 . ?
C1A C2A 1.535(15) . ?
C1A C6A 1.572(13) . ?
C1B H1B 1.0000 . ?
C1B C2B 1.50(2) . ?
C1B C6B 1.56(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A C3A 1.521(15) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C2B C3B 1.48(3) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C4 1.457(12) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3B C4 1.439(19) . ?
C4 H4AA 0.9900 . ?
C4 H4AB 0.9900 . ?
C4 H4BC 0.9900 . ?
C4 H4BD 0.9900 . ?
C4 C5A 1.586(10) . ?
C4 C5B 1.613(17) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
C5A C6A 1.512(14) . ?
C5B H5BA 0.9900 . ?
C5B H5BB 0.9900 . ?
C5B C6B 1.50(2) . ?
C6A H6A 1.0000 . ?
C6B H6B 1.0000 . ?
C7 H7 0.9500 . ?
C7 C8 1.443(9) . ?
C8 C9 1.418(9) . ?
C8 C13 1.406(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.371(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.395(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(7) . ?
C12 C13 1.404(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C16 1.432(9) . ?
C16 C17 1.422(9) . ?
C16 C21 1.420(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.341(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(8) . ?
C20 C21 1.402(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.461(10) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 Zn1 33.52(9) . . ?
O1 Dy1 O2 63.23(12) . . ?
O1 Dy1 O3 65.91(12) . . ?
O1 Dy1 O4 128.83(13) . . ?
O1 Dy1 O5 80.17(13) . . ?
O1 Dy1 O6 138.72(15) . . ?
O1 Dy1 O7 135.1(2) . . ?
O1 Dy1 O9 108.40(16) . . ?
O1 Dy1 O10 77.02(14) . . ?
O1 Dy1 N3 144.85(15) . . ?
O1 Dy1 N4 94.29(14) . . ?
O2 Dy1 Zn1 93.80(8) . . ?
O2 Dy1 N3 81.63(14) . . ?
O2 Dy1 N4 99.18(14) . . ?
O3 Dy1 Zn1 33.97(9) . . ?
O3 Dy1 O2 127.77(11) . . ?
O3 Dy1 O4 63.44(12) . . ?
O3 Dy1 O5 79.43(14) . . ?
O3 Dy1 O6 133.23(14) . . ?
O3 Dy1 O7 149.6(2) . . ?
O3 Dy1 O9 81.68(16) . . ?
O3 Dy1 O10 106.11(16) . . ?
O3 Dy1 N3 148.26(15) . . ?
O3 Dy1 N4 95.55(16) . . ?
O4 Dy1 Zn1 95.42(10) . . ?
O4 Dy1 O2 158.78(12) . . ?
O4 Dy1 N3 84.89(15) . . ?
O4 Dy1 N4 97.17(15) . . ?
O5 Dy1 Zn1 70.11(9) . . ?
O5 Dy1 O2 81.13(13) . . ?
O5 Dy1 O4 84.10(14) . . ?
O5 Dy1 O6 71.21(15) . . ?
O5 Dy1 O7 120.85(15) . . ?
O5 Dy1 O9 153.71(15) . . ?
O5 Dy1 O10 151.46(14) . . ?
O5 Dy1 N3 96.12(16) . . ?
O5 Dy1 N4 173.67(14) . . ?
O6 Dy1 Zn1 141.22(11) . . ?
O6 Dy1 O2 83.08(13) . . ?
O6 Dy1 O4 77.76(14) . . ?
O6 Dy1 O7 51.08(17) . . ?
O6 Dy1 O9 110.44(16) . . ?
O6 Dy1 O10 117.17(16) . . ?
O6 Dy1 N3 25.42(16) . . ?
O6 Dy1 N4 115.12(16) . . ?
O7 Dy1 Zn1 166.05(18) . . ?
O7 Dy1 O2 80.3(2) . . ?
O7 Dy1 O4 94.4(3) . . ?
O7 Dy1 N3 25.69(17) . . ?
O7 Dy1 N4 65.32(16) . . ?
O9 Dy1 Zn1 102.91(13) . . ?
O9 Dy1 O2 125.08(14) . . ?
O9 Dy1 O4 71.11(15) . . ?
O9 Dy1 O7 71.08(19) . . ?
O9 Dy1 O10 52.69(15) . . ?
O9 Dy1 N3 90.39(18) . . ?
O9 Dy1 N4 26.19(15) . . ?
O10 Dy1 Zn1 98.53(11) . . ?
O10 Dy1 O2 73.41(14) . . ?
O10 Dy1 O4 123.76(14) . . ?
O10 Dy1 O7 67.7(2) . . ?
O10 Dy1 N3 92.79(17) . . ?
O10 Dy1 N4 26.59(15) . . ?
N3 Dy1 Zn1 166.08(13) . . ?
N4 Dy1 Zn1 103.57(11) . . ?
N4 Dy1 N3 90.17(17) . . ?
Cl1 Zn1 Dy1 100.68(4) . . ?
O1 Zn1 Dy1 37.79(10) . . ?
O1 Zn1 Cl1 104.19(12) . . ?
O1 Zn1 O3 74.91(14) . . ?
O1 Zn1 N1 88.70(17) . . ?
O1 Zn1 N2 143.12(19) . . ?
O3 Zn1 Dy1 38.99(10) . . ?
O3 Zn1 Cl1 107.05(13) . . ?
O3 Zn1 N1 136.92(18) . . ?
N1 Zn1 Dy1 122.41(13) . . ?
N1 Zn1 Cl1 115.60(15) . . ?
N2 Zn1 Dy1 124.59(14) . . ?
N2 Zn1 Cl1 112.04(16) . . ?
N2 Zn1 O3 87.86(17) . . ?
N2 Zn1 N1 82.0(2) . . ?
Zn1 O1 Dy1 108.69(16) . . ?
C13 O1 Dy1 128.4(3) . . ?
C13 O1 Zn1 122.0(3) . . ?
C12 O2 Dy1 116.0(3) . . ?
C12 O2 C14 116.6(4) . . ?
C14 O2 Dy1 126.5(3) . . ?
Zn1 O3 Dy1 107.04(15) . . ?
C21 O3 Dy1 127.7(3) . . ?
C21 O3 Zn1 123.3(3) . . ?
C20 O4 Dy1 118.9(3) . . ?
C20 O4 C22 114.2(5) . . ?
C22 O4 Dy1 125.9(5) . . ?
Dy1 O5 H5 112.6(14) . . ?
C23 O5 Dy1 138.3(4) . . ?
C23 O5 H5 108.1(14) . . ?
N3 O6 Dy1 99.9(4) . . ?
N3 O7 Dy1 96.1(4) . . ?
N4 O9 Dy1 96.5(3) . . ?
N4 O10 Dy1 94.8(3) . . ?
C1A N1 Zn1 108.9(5) . . ?
C6B N1 Zn1 118.7(8) . . ?
C7 N1 Zn1 125.3(4) . . ?
C7 N1 C1A 124.3(6) . . ?
C7 N1 C6B 113.1(9) . . ?
C1B N2 Zn1 103.9(8) . . ?
C6A N2 Zn1 115.0(5) . . ?
C15 N2 Zn1 126.5(4) . . ?
C15 N2 C1B 126.3(8) . . ?
C15 N2 C6A 117.6(6) . . ?
O6 N3 Dy1 54.7(3) . . ?
O6 N3 O7 112.8(5) . . ?
O7 N3 Dy1 58.2(4) . . ?
O8 N3 Dy1 177.2(5) . . ?
O8 N3 O6 122.5(6) . . ?
O8 N3 O7 124.6(7) . . ?
O9 N4 Dy1 57.3(3) . . ?
O9 N4 O10 115.6(5) . . ?
O10 N4 Dy1 58.6(3) . . ?
O11 N4 Dy1 174.3(5) . . ?
O11 N4 O9 122.1(6) . . ?
O11 N4 O10 122.3(6) . . ?
N1 C1A H1A 107.8 . . ?
C2A C1A N1 113.1(11) . . ?
C2A C1A H1A 107.8 . . ?
C2A C1A C6A 110.2(7) . . ?
C6A C1A N1 110.0(7) . . ?
C6A C1A H1A 107.8 . . ?
N2 C1B H1B 108.4 . . ?
C2B C1B N2 109.5(16) . . ?
C2B C1B H1B 108.4 . . ?
C2B C1B C6B 110.6(14) . . ?
C6B C1B N2 111.6(12) . . ?
C6B C1B H1B 108.4 . . ?
C1A C2A H2AA 109.2 . . ?
C1A C2A H2AB 109.2 . . ?
H2AA C2A H2AB 107.9 . . ?
C3A C2A C1A 112.2(8) . . ?
C3A C2A H2AA 109.2 . . ?
C3A C2A H2AB 109.2 . . ?
C1B C2B H2BA 108.5 . . ?
C1B C2B H2BB 108.5 . . ?
H2BA C2B H2BB 107.5 . . ?
C3B C2B C1B 115.2(16) . . ?
C3B C2B H2BA 108.5 . . ?
C3B C2B H2BB 108.5 . . ?
C2A C3A H3AA 109.1 . . ?
C2A C3A H3AB 109.1 . . ?
H3AA C3A H3AB 107.8 . . ?
C4 C3A C2A 112.5(9) . . ?
C4 C3A H3AA 109.1 . . ?
C4 C3A H3AB 109.1 . . ?
C2B C3B H3BA 108.7 . . ?
C2B C3B H3BB 108.7 . . ?
H3BA C3B H3BB 107.6 . . ?
C4 C3B C2B 114.2(13) . . ?
C4 C3B H3BA 108.7 . . ?
C4 C3B H3BB 108.7 . . ?
C3A C4 H4AA 109.1 . . ?
C3A C4 H4AB 109.1 . . ?
C3A C4 C5A 112.4(6) . . ?
C3B C4 H4BC 109.5 . . ?
C3B C4 H4BD 109.5 . . ?
C3B C4 C5B 110.7(9) . . ?
H4AA C4 H4AB 107.8 . . ?
H4BC C4 H4BD 108.1 . . ?
C5A C4 H4AA 109.1 . . ?
C5A C4 H4AB 109.1 . . ?
C5B C4 H4BC 109.5 . . ?
C5B C4 H4BD 109.5 . . ?
C4 C5A H5AA 109.5 . . ?
C4 C5A H5AB 109.5 . . ?
H5AA C5A H5AB 108.1 . . ?
C6A C5A C4 110.8(7) . . ?
C6A C5A H5AA 109.5 . . ?
C6A C5A H5AB 109.5 . . ?
C4 C5B H5BA 109.0 . . ?
C4 C5B H5BB 109.0 . . ?
H5BA C5B H5BB 107.8 . . ?
C6B C5B C4 112.8(14) . . ?
C6B C5B H5BA 109.0 . . ?
C6B C5B H5BB 109.0 . . ?
N2 C6A C1A 101.8(7) . . ?
N2 C6A C5A 111.3(8) . . ?
N2 C6A H6A 110.5 . . ?
C1A C6A H6A 110.5 . . ?
C5A C6A C1A 112.1(9) . . ?
C5A C6A H6A 110.5 . . ?
N1 C6B C1B 98.2(13) . . ?
N1 C6B C5B 114.8(16) . . ?
N1 C6B H6B 110.7 . . ?
C1B C6B H6B 110.7 . . ?
C5B C6B C1B 111.1(14) . . ?
C5B C6B H6B 110.7 . . ?
N1 C7 H7 117.9 . . ?
N1 C7 C8 124.1(5) . . ?
C8 C7 H7 117.9 . . ?
C9 C8 C7 117.3(5) . . ?
C13 C8 C7 124.4(5) . . ?
C13 C8 C9 118.1(6) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3(6) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.9(6) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 H11 120.9 . . ?
C12 C11 C10 118.3(6) . . ?
C12 C11 H11 120.9 . . ?
O2 C12 C13 113.4(4) . . ?
C11 C12 O2 125.2(5) . . ?
C11 C12 C13 121.4(5) . . ?
O1 C13 C8 124.0(5) . . ?
O1 C13 C12 116.2(5) . . ?
C12 C13 C8 119.9(5) . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15 117.7 . . ?
N2 C15 C16 124.6(6) . . ?
C16 C15 H15 117.7 . . ?
C17 C16 C15 119.3(6) . . ?
C21 C16 C15 124.0(6) . . ?
C21 C16 C17 116.4(6) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 C16 122.2(7) . . ?
C18 C17 H17 118.9 . . ?
C17 C18 H18 119.0 . . ?
C17 C18 C19 122.1(7) . . ?
C19 C18 H18 119.0 . . ?
C18 C19 H19 121.2 . . ?
C20 C19 C18 117.7(7) . . ?
C20 C19 H19 121.2 . . ?
O4 C20 C21 112.5(5) . . ?
C19 C20 O4 125.4(5) . . ?
C19 C20 C21 122.1(6) . . ?
O3 C21 C16 123.5(5) . . ?
O3 C21 C20 117.0(5) . . ?
C20 C21 C16 119.5(5) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 H23A 109.4 . . ?
O5 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C24 C23 O5 111.2(6) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_smtbx_masks_special_details     ?
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
_smtbx_masks_void_content
1 0.250 -0.914 0.750 200.7 40.7 ?
2 -0.250 -0.627 0.250 200.7 40.7 ?

_olex2_date_sample_data_collection 2017-07-24
_olex2_date_sample_submission    2017-06-29
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id SS419
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.476
_vrf_PLAT241_2017ncs0426za       
;
PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of O7 Check:
RESPONSE: Arises from minor disorder in coordinated NO3 which has not been
 modelled
;
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1820465'
_audit_update_record             
;
2018-01-30 deposited with the CCDC.
2018-02-23 downloaded from the CCDC.
;
_audit_creation_date             2017-08-01
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H30 Cl N4 O11 Y Zn'
_chemical_formula_sum            'C24 H30 Cl N4 O11 Y Zn'
_chemical_formula_weight         740.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         '(Zn2 Y2 (C22 H24 N2 O2)2 (N O3)4 )2 (N O3)'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2025(3)
_cell_length_b                   14.3533(5)
_cell_length_c                   14.4172(6)
_cell_angle_alpha                67.998(4)
_cell_angle_beta                 83.196(3)
_cell_angle_gamma                80.804(3)
_cell_volume                     1550.35(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7640
_cell_measurement_theta_min      2.5090
_shelx_estimated_absorpt_T_max   0.946
_shelx_estimated_absorpt_T_min   0.680
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18089
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.534
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00  73.00   1.00    5.00    --  -17.00   0.00 -60.00  180
  2  ω    -69.00  22.00   1.00    5.00    --  -17.00 -72.00 -90.00   91
  3  ω    -75.00  22.00   1.00    5.00    --  -17.00 -72.00 120.00   97
  4  ω    -27.00  68.00   1.00    5.00    --  -17.00  72.00  30.00   95
  5  ω    -49.00 -32.00   1.00    5.00    --  -17.00 -72.00  90.00   17
  6  ω   -107.00 -31.00   1.00    5.00    --  -17.00   0.00  30.00   76
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097895000
_diffrn_orient_matrix_UB_12      -0.0097090000
_diffrn_orient_matrix_UB_13      0.0522093000
_diffrn_orient_matrix_UB_21      0.0415843000
_diffrn_orient_matrix_UB_22      -0.0496807000
_diffrn_orient_matrix_UB_23      0.0097497000
_diffrn_orient_matrix_UB_31      0.0766824000
_diffrn_orient_matrix_UB_32      0.0179917000
_diffrn_orient_matrix_UB_33      -0.0025190000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5271
_reflns_number_total             6903
_reflns_odcompleteness_completeness 96.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6903
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0456
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0671P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1205
_refine_special_details          
'RIGU and SIMU restraints applied to disordered cyclohexane moiety. H-atom bonded to O atom of coordinated EtOH has been located in the difference map and refined with the reding model..Appropriate distance and angle restraints applied to coordinated EtOH O-H bond. The electron contribution from diffuse solvent which cannot be modelled is accounted for by the SMTBX solvent masking routine as implemented in Olex2.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 C23-H5
 1.91398 with sigma of 0.02
 Y1-H5
 2.80439 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4A \\sim C3B \\sim C3A \\sim C4B \\sim C1B \\sim C1A \\sim C6B \\sim C6A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C6A, C6B, C1A, C1B, C4B, C4A, C3A, C3B, C2, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H5bc)=Sof(H5bd)=Sof(H2bc)=Sof(H2bd)=Sof(C1B)=Sof(H1B)=Sof(C6A)=Sof(H6A)=
 Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(C4B)=Sof(H4Ba)=Sof(H4Bb)=1-FVAR(1)
 Sof(H5aa)=Sof(H5ab)=Sof(H2aa)=Sof(H2ab)=Sof(C6B)=Sof(H6B)=Sof(C1A)=Sof(H1A)=
 Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C6B(H6B), C1A(H1A), C1B(H1B), C6A(H6A)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5aa,H5ab), C5(H5bc,H5bd), C2(H2aa,H2ab), C2(H2bc,H2bd), C23(H23a,H23b),
 C3A(H3Aa,H3Ab), C4A(H4Aa,H4Ab), C3B(H3Ba,H3Bb), C4B(H4Ba,H4Bb)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C19(H19), C7(H7), C9(H9), C15(H15), C17(H17), C18(H18)
6.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.74909(4) 0.27499(2) 0.22342(2) 0.02040(11) Uani 1 1 d D . . . .
Zn1 Zn 0.62401(5) 0.28647(3) 0.45701(3) 0.02165(12) Uani 1 1 d . . . . .
Cl1 Cl 0.85790(11) 0.32722(7) 0.49821(7) 0.0307(2) Uani 1 1 d . . . . .
O1 O 0.7113(3) 0.18835(15) 0.38789(17) 0.0203(5) Uani 1 1 d . . . . .
O3 O 0.5987(3) 0.36787(16) 0.30902(17) 0.0247(5) Uani 1 1 d . . . . .
O2 O 0.9164(3) 0.10158(16) 0.29043(17) 0.0217(5) Uani 1 1 d . . . . .
O4 O 0.6815(3) 0.46450(16) 0.12646(17) 0.0230(5) Uani 1 1 d . . . . .
O6 O 0.9715(3) 0.31286(19) 0.0973(2) 0.0321(6) Uani 1 1 d . . . . .
O9 O 0.5735(3) 0.15092(17) 0.23186(19) 0.0309(6) Uani 1 1 d . . . . .
O5 O 0.9637(3) 0.31876(18) 0.28639(19) 0.0274(6) Uani 1 1 d D . . . .
H5 H 0.933(3) 0.327(3) 0.3419(15) 0.041 Uiso 1 1 d DR . . . .
O10 O 0.4914(3) 0.30679(18) 0.1487(2) 0.0340(6) Uani 1 1 d . . . . .
N2 N 0.4197(4) 0.3711(2) 0.4884(2) 0.0288(7) Uani 1 1 d . . . . .
O7 O 0.7979(4) 0.2288(3) 0.0733(2) 0.0504(8) Uani 1 1 d . . . . .
O8 O 1.0064(4) 0.2704(2) -0.0337(2) 0.0479(8) Uani 1 1 d . . . . .
N1 N 0.5170(4) 0.1734(2) 0.5670(2) 0.0302(7) Uani 1 1 d . . . . .
N4 N 0.4703(4) 0.2153(2) 0.1742(2) 0.0291(7) Uani 1 1 d . . . . .
C12 C 0.8629(4) 0.0380(2) 0.3842(3) 0.0200(7) Uani 1 1 d . . . . .
C11 C 0.9117(4) -0.0635(2) 0.4265(3) 0.0215(7) Uani 1 1 d . . . . .
H11 H 0.990942 -0.096826 0.391965 0.026 Uiso 1 1 calc R . . . .
N3 N 0.9271(4) 0.2716(2) 0.0415(2) 0.0340(8) Uani 1 1 d . . . . .
O11 O 0.3555(4) 0.1903(2) 0.1458(2) 0.0489(8) Uani 1 1 d . . . . .
C20 C 0.5653(4) 0.5180(2) 0.1717(3) 0.0220(7) Uani 1 1 d . . . . .
C8 C 0.6792(4) 0.0346(2) 0.5290(3) 0.0197(7) Uani 1 1 d . . . . .
C21 C 0.5245(4) 0.4621(2) 0.2727(3) 0.0223(7) Uani 1 1 d . . . . .
C13 C 0.7494(4) 0.0897(2) 0.4347(2) 0.0177(7) Uani 1 1 d . . . . .
C10 C 0.8436(4) -0.1176(2) 0.5213(3) 0.0261(8) Uani 1 1 d . . . . .
H10 H 0.877894 -0.188150 0.551709 0.031 Uiso 1 1 calc R . . . .
C16 C 0.4101(4) 0.5078(2) 0.3272(3) 0.0228(7) Uani 1 1 d . . . . .
C19 C 0.4913(4) 0.6152(2) 0.1252(3) 0.0277(8) Uani 1 1 d . . . . .
H19 H 0.518482 0.651405 0.056366 0.033 Uiso 1 1 calc R . . . .
C7 C 0.5530(4) 0.0787(2) 0.5844(3) 0.0270(8) Uani 1 1 d . . . . .
H7 H 0.491934 0.033745 0.637974 0.032 Uiso 1 1 calc R . . . .
C9 C 0.7290(4) -0.0706(2) 0.5705(3) 0.0227(7) Uani 1 1 d . . . . .
H9 H 0.681453 -0.109166 0.634073 0.027 Uiso 1 1 calc R . . . .
C15 C 0.3538(4) 0.4570(3) 0.4309(3) 0.0274(8) Uani 1 1 d . . . . .
H15 H 0.261637 0.490115 0.457875 0.033 Uiso 1 1 calc R . . . .
C17 C 0.3362(4) 0.6074(3) 0.2778(3) 0.0278(8) Uani 1 1 d . . . . .
H17 H 0.256340 0.638867 0.313856 0.033 Uiso 1 1 calc R . . . .
C14 C 1.0393(4) 0.0557(3) 0.2357(3) 0.0273(8) Uani 1 1 d . . . . .
H14A H 0.990815 0.007157 0.217635 0.041 Uiso 1 1 calc GR . . . .
H14B H 1.132490 0.020382 0.277460 0.041 Uiso 1 1 calc GR . . . .
H14C H 1.078498 0.108252 0.174619 0.041 Uiso 1 1 calc GR . . . .
C18 C 0.3769(4) 0.6597(2) 0.1797(3) 0.0302(8) Uani 1 1 d . . . . .
H18 H 0.326355 0.727147 0.148257 0.036 Uiso 1 1 calc R . . . .
C5 C 0.2106(5) 0.3688(3) 0.6346(3) 0.0316(8) Uani 1 1 d . U . . .
H5AA H 0.218224 0.440064 0.624944 0.038 Uiso 0.758(10) 1 calc R . P A 1
H5AB H 0.118646 0.368689 0.595980 0.038 Uiso 0.758(10) 1 calc R . P A 1
H5BC H 0.125507 0.418264 0.592371 0.038 Uiso 0.242(10) 1 calc R . P A 2
H5BD H 0.284375 0.405073 0.654985 0.038 Uiso 0.242(10) 1 calc R . P A 2
C2 C 0.3306(5) 0.1509(3) 0.7249(3) 0.0375(10) Uani 1 1 d . U . . .
H2AA H 0.322829 0.079419 0.735487 0.045 Uiso 0.758(10) 1 calc R . P A 1
H2AB H 0.423106 0.152869 0.762165 0.045 Uiso 0.758(10) 1 calc R . P A 1
H2BC H 0.244239 0.131976 0.695141 0.045 Uiso 0.242(10) 1 calc R . P A 2
H2BD H 0.399591 0.087761 0.763133 0.045 Uiso 0.242(10) 1 calc R . P A 2
C22 C 0.7368(5) 0.5201(3) 0.0254(3) 0.0364(10) Uani 1 1 d . . . . .
H22A H 0.826549 0.478205 0.002590 0.055 Uiso 1 1 calc GR . . . .
H22B H 0.777049 0.581891 0.022485 0.055 Uiso 1 1 calc GR . . . .
H22C H 0.644560 0.538193 -0.018129 0.055 Uiso 1 1 calc GR . . . .
C24 C 1.0804(5) 0.4758(3) 0.2122(3) 0.0390(10) Uani 1 1 d . . . . .
H24A H 0.999104 0.499830 0.161072 0.059 Uiso 1 1 calc GR . . . .
H24B H 1.183076 0.505404 0.183457 0.059 Uiso 1 1 calc GR . . . .
H24C H 1.036360 0.496299 0.268896 0.059 Uiso 1 1 calc GR . . . .
C23 C 1.1149(4) 0.3639(3) 0.2474(3) 0.0331(9) Uani 1 1 d D . . . .
H23A H 1.165250 0.343256 0.191024 0.040 Uiso 1 1 calc R . . . .
H23B H 1.194645 0.339372 0.300442 0.040 Uiso 1 1 calc R . . . .
C6B C 0.3686(7) 0.3255(4) 0.5945(4) 0.0251(12) Uani 0.758(10) 1 d . U P A 1
H6B H 0.459953 0.326512 0.634171 0.030 Uiso 0.758(10) 1 calc R . P A 1
C1A C 0.3571(8) 0.2144(4) 0.6111(4) 0.0253(13) Uani 0.758(10) 1 d . U P A 1
H1A H 0.262105 0.211438 0.575208 0.030 Uiso 0.758(10) 1 calc R . P A 1
C3A C 0.1650(10) 0.2012(4) 0.7603(5) 0.0401(17) Uani 0.758(10) 1 d . U P A 1
H3AA H 0.073888 0.196644 0.723474 0.048 Uiso 0.758(10) 1 calc R . P A 1
H3AB H 0.140632 0.163870 0.832616 0.048 Uiso 0.758(10) 1 calc R . P A 1
C4A C 0.1725(9) 0.3115(5) 0.7429(5) 0.0354(16) Uani 0.758(10) 1 d . U P A 1
H4AA H 0.065076 0.341380 0.765156 0.042 Uiso 0.758(10) 1 calc R . P A 1
H4AB H 0.259099 0.316178 0.782715 0.042 Uiso 0.758(10) 1 calc R . P A 1
C1B C 0.437(2) 0.2167(10) 0.6424(13) 0.022(3) Uani 0.242(10) 1 d . U P A 2
H1B H 0.516404 0.246023 0.668012 0.026 Uiso 0.242(10) 1 calc R . P A 2
C6A C 0.312(2) 0.2960(12) 0.5798(11) 0.019(3) Uani 0.242(10) 1 d . U P A 2
H6A H 0.235828 0.265071 0.553898 0.023 Uiso 0.242(10) 1 calc R . P A 2
C3B C 0.251(3) 0.2002(13) 0.7942(14) 0.033(4) Uani 0.242(10) 1 d . U P A 2
H3BA H 0.331754 0.230097 0.816620 0.040 Uiso 0.242(10) 1 calc R . P A 2
H3BB H 0.196694 0.151363 0.853648 0.040 Uiso 0.242(10) 1 calc R . P A 2
C4B C 0.126(3) 0.2801(16) 0.7340(14) 0.029(4) Uani 0.242(10) 1 d . U P A 2
H4BA H 0.059456 0.313317 0.777555 0.035 Uiso 0.242(10) 1 calc R . P A 2
H4BB H 0.050106 0.248040 0.709976 0.035 Uiso 0.242(10) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 Zn1 3.4589(5) . ?
Y1 O1 2.237(2) . ?
Y1 O3 2.273(2) . ?
Y1 O2 2.536(2) . ?
Y1 O4 2.552(2) . ?
Y1 O6 2.392(2) . ?
Y1 O9 2.424(2) . ?
Y1 O5 2.340(2) . ?
Y1 O10 2.387(2) . ?
Y1 O7 2.464(3) . ?
Y1 N4 2.816(3) . ?
Y1 N3 2.860(3) . ?
Zn1 Cl1 2.2944(10) . ?
Zn1 O1 2.012(2) . ?
Zn1 O3 2.030(2) . ?
Zn1 N2 2.017(3) . ?
Zn1 N1 2.028(3) . ?
O1 C13 1.323(3) . ?
O3 C21 1.325(4) . ?
O2 C12 1.385(4) . ?
O2 C14 1.436(4) . ?
O4 C20 1.385(4) . ?
O4 C22 1.433(4) . ?
O6 N3 1.275(4) . ?
O9 N4 1.266(4) . ?
O5 H5 0.856(9) . ?
O5 C23 1.447(4) . ?
O10 N4 1.259(4) . ?
N2 C15 1.275(4) . ?
N2 C6B 1.459(6) . ?
N2 C6A 1.623(15) . ?
O7 N3 1.261(4) . ?
O8 N3 1.201(4) . ?
N1 C7 1.278(4) . ?
N1 C1A 1.519(6) . ?
N1 C1B 1.485(15) . ?
N4 O11 1.222(4) . ?
C12 C11 1.363(4) . ?
C12 C13 1.404(4) . ?
C11 H11 0.9500 . ?
C11 C10 1.394(5) . ?
C20 C21 1.404(5) . ?
C20 C19 1.374(4) . ?
C8 C13 1.400(4) . ?
C8 C7 1.443(5) . ?
C8 C9 1.409(4) . ?
C21 C16 1.394(5) . ?
C10 H10 0.9500 . ?
C10 C9 1.357(5) . ?
C16 C15 1.451(5) . ?
C16 C17 1.408(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.384(5) . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C15 H15 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.360(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C18 H18 0.9500 . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C5 C6B 1.495(6) . ?
C5 C4A 1.488(7) . ?
C5 C6A 1.613(15) . ?
C5 C4B 1.68(2) . ?
C2 H2AA 0.9900 . ?
C2 H2AB 0.9900 . ?
C2 H2BC 0.9900 . ?
C2 H2BD 0.9900 . ?
C2 C1A 1.559(6) . ?
C2 C3A 1.557(7) . ?
C2 C1B 1.499(15) . ?
C2 C3B 1.468(17) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 C23 1.482(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C6B H6B 1.0000 . ?
C6B C1A 1.538(8) . ?
C1A H1A 1.0000 . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C4A 1.517(9) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C1B H1B 1.0000 . ?
C1B C6A 1.49(3) . ?
C6A H6A 1.0000 . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C3B C4B 1.48(3) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 Zn1 33.41(5) . . ?
O1 Y1 O3 66.26(8) . . ?
O1 Y1 O2 63.85(7) . . ?
O1 Y1 O4 128.92(7) . . ?
O1 Y1 O6 138.92(9) . . ?
O1 Y1 O9 76.39(8) . . ?
O1 Y1 O5 78.53(8) . . ?
O1 Y1 O10 108.76(9) . . ?
O1 Y1 O7 134.57(9) . . ?
O1 Y1 N4 94.17(8) . . ?
O1 Y1 N3 144.56(8) . . ?
O3 Y1 Zn1 34.17(6) . . ?
O3 Y1 O2 129.20(8) . . ?
O3 Y1 O4 63.23(8) . . ?
O3 Y1 O6 131.65(8) . . ?
O3 Y1 O9 104.65(9) . . ?
O3 Y1 O5 80.20(9) . . ?
O3 Y1 O10 80.81(9) . . ?
O3 Y1 O7 149.90(10) . . ?
O3 Y1 N4 94.44(9) . . ?
O3 Y1 N3 148.08(8) . . ?
O2 Y1 Zn1 95.04(5) . . ?
O2 Y1 O4 159.62(7) . . ?
O2 Y1 N4 98.00(8) . . ?
O2 Y1 N3 80.72(8) . . ?
O4 Y1 Zn1 95.57(5) . . ?
O4 Y1 N4 96.70(8) . . ?
O4 Y1 N3 84.93(8) . . ?
O6 Y1 Zn1 140.96(6) . . ?
O6 Y1 O2 84.40(8) . . ?
O6 Y1 O4 76.41(8) . . ?
O6 Y1 O9 119.85(9) . . ?
O6 Y1 O7 52.27(9) . . ?
O6 Y1 N4 116.60(9) . . ?
O6 Y1 N3 26.21(9) . . ?
O9 Y1 Zn1 96.72(6) . . ?
O9 Y1 O2 72.45(8) . . ?
O9 Y1 O4 123.31(8) . . ?
O9 Y1 O7 68.72(9) . . ?
O9 Y1 N4 26.63(8) . . ?
O9 Y1 N3 94.32(9) . . ?
O5 Y1 Zn1 70.23(6) . . ?
O5 Y1 O2 81.32(8) . . ?
O5 Y1 O4 85.98(8) . . ?
O5 Y1 O6 71.12(9) . . ?
O5 Y1 O9 149.65(8) . . ?
O5 Y1 O10 154.59(9) . . ?
O5 Y1 O7 120.95(9) . . ?
O5 Y1 N4 172.21(9) . . ?
O5 Y1 N3 96.29(9) . . ?
O10 Y1 Zn1 102.02(7) . . ?
O10 Y1 O2 123.97(8) . . ?
O10 Y1 O4 70.40(8) . . ?
O10 Y1 O6 110.56(9) . . ?
O10 Y1 O9 52.92(8) . . ?
O10 Y1 O7 71.92(10) . . ?
O10 Y1 N4 26.39(8) . . ?
O10 Y1 N3 90.98(10) . . ?
O7 Y1 Zn1 165.16(7) . . ?
O7 Y1 O2 78.21(10) . . ?
O7 Y1 O4 95.01(10) . . ?
O7 Y1 N4 66.22(9) . . ?
O7 Y1 N3 26.07(9) . . ?
N4 Y1 Zn1 102.17(6) . . ?
N4 Y1 N3 91.25(9) . . ?
N3 Y1 Zn1 166.39(7) . . ?
Cl1 Zn1 Y1 101.27(3) . . ?
O1 Zn1 Y1 37.74(6) . . ?
O1 Zn1 Cl1 103.96(7) . . ?
O1 Zn1 O3 75.17(9) . . ?
O1 Zn1 N2 144.39(11) . . ?
O1 Zn1 N1 88.66(10) . . ?
O3 Zn1 Y1 38.98(6) . . ?
O3 Zn1 Cl1 106.86(7) . . ?
N2 Zn1 Y1 125.33(9) . . ?
N2 Zn1 Cl1 111.11(9) . . ?
N2 Zn1 O3 88.76(11) . . ?
N2 Zn1 N1 82.04(12) . . ?
N1 Zn1 Y1 122.06(8) . . ?
N1 Zn1 Cl1 115.25(10) . . ?
N1 Zn1 O3 137.44(12) . . ?
Zn1 O1 Y1 108.86(9) . . ?
C13 O1 Y1 126.6(2) . . ?
C13 O1 Zn1 124.4(2) . . ?
Zn1 O3 Y1 106.85(9) . . ?
C21 O3 Y1 128.2(2) . . ?
C21 O3 Zn1 124.5(2) . . ?
C12 O2 Y1 115.82(18) . . ?
C12 O2 C14 116.0(2) . . ?
C14 O2 Y1 127.15(19) . . ?
C20 O4 Y1 116.94(18) . . ?
C20 O4 C22 115.7(3) . . ?
C22 O4 Y1 127.0(2) . . ?
N3 O6 Y1 97.8(2) . . ?
N4 O9 Y1 94.23(19) . . ?
Y1 O5 H5 111.7(13) . . ?
C23 O5 Y1 137.4(2) . . ?
C23 O5 H5 108.0(13) . . ?
N4 O10 Y1 96.17(19) . . ?
C15 N2 Zn1 127.3(3) . . ?
C15 N2 C6B 123.3(3) . . ?
C15 N2 C6A 121.5(6) . . ?
C6B N2 Zn1 108.9(3) . . ?
C6A N2 Zn1 107.5(5) . . ?
N3 O7 Y1 94.8(2) . . ?
C7 N1 Zn1 126.1(2) . . ?
C7 N1 C1A 121.0(3) . . ?
C7 N1 C1B 124.4(6) . . ?
C1A N1 Zn1 111.2(2) . . ?
C1B N1 Zn1 106.3(6) . . ?
O9 N4 Y1 59.14(16) . . ?
O10 N4 Y1 57.44(16) . . ?
O10 N4 O9 116.3(3) . . ?
O11 N4 Y1 175.1(3) . . ?
O11 N4 O9 121.9(3) . . ?
O11 N4 O10 121.8(3) . . ?
O2 C12 C13 112.3(3) . . ?
C11 C12 O2 126.0(3) . . ?
C11 C12 C13 121.7(3) . . ?
C12 C11 H11 120.5 . . ?
C12 C11 C10 119.0(3) . . ?
C10 C11 H11 120.5 . . ?
O6 N3 Y1 55.94(17) . . ?
O7 N3 Y1 59.17(19) . . ?
O7 N3 O6 115.1(3) . . ?
O8 N3 Y1 177.9(3) . . ?
O8 N3 O6 122.1(3) . . ?
O8 N3 O7 122.7(4) . . ?
O4 C20 C21 113.2(3) . . ?
C19 C20 O4 125.4(3) . . ?
C19 C20 C21 121.4(3) . . ?
C13 C8 C7 123.6(3) . . ?
C13 C8 C9 118.4(3) . . ?
C9 C8 C7 117.9(3) . . ?
O3 C21 C20 116.4(3) . . ?
O3 C21 C16 124.7(3) . . ?
C16 C21 C20 118.9(3) . . ?
O1 C13 C12 117.2(3) . . ?
O1 C13 C8 123.9(3) . . ?
C8 C13 C12 118.9(3) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 C11 120.7(3) . . ?
C9 C10 H10 119.6 . . ?
C21 C16 C15 124.1(3) . . ?
C21 C16 C17 118.5(3) . . ?
C17 C16 C15 117.2(3) . . ?
C20 C19 H19 120.4 . . ?
C20 C19 C18 119.3(3) . . ?
C18 C19 H19 120.4 . . ?
N1 C7 C8 125.2(3) . . ?
N1 C7 H7 117.4 . . ?
C8 C7 H7 117.4 . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 H9 119.4 . . ?
N2 C15 C16 124.5(3) . . ?
N2 C15 H15 117.7 . . ?
C16 C15 H15 117.7 . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C19 C18 H18 119.8 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18 119.8 . . ?
H5AA C5 H5AB 107.8 . . ?
H5BC C5 H5BD 109.7 . . ?
C6B C5 H5AA 109.0 . . ?
C6B C5 H5AB 109.0 . . ?
C4A C5 H5AA 109.0 . . ?
C4A C5 H5AB 109.0 . . ?
C4A C5 C6B 112.7(4) . . ?
C6A C5 H5BC 112.0 . . ?
C6A C5 H5BD 112.0 . . ?
C6A C5 C4B 98.7(9) . . ?
C4B C5 H5BC 112.0 . . ?
C4B C5 H5BD 112.0 . . ?
H2AA C2 H2AB 108.8 . . ?
H2BC C2 H2BD 107.8 . . ?
C1A C2 H2AA 110.7 . . ?
C1A C2 H2AB 110.7 . . ?
C3A C2 H2AA 110.7 . . ?
C3A C2 H2AB 110.7 . . ?
C3A C2 C1A 105.2(4) . . ?
C1B C2 H2BC 109.0 . . ?
C1B C2 H2BD 109.0 . . ?
C3B C2 H2BC 109.0 . . ?
C3B C2 H2BD 109.0 . . ?
C3B C2 C1B 113.0(10) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
O5 C23 C24 110.4(3) . . ?
O5 C23 H23A 109.6 . . ?
O5 C23 H23B 109.6 . . ?
C24 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
N2 C6B C5 119.3(4) . . ?
N2 C6B H6B 107.9 . . ?
N2 C6B C1A 104.6(5) . . ?
C5 C6B H6B 107.9 . . ?
C5 C6B C1A 108.8(5) . . ?
C1A C6B H6B 107.9 . . ?
N1 C1A C2 110.7(4) . . ?
N1 C1A C6B 107.6(4) . . ?
N1 C1A H1A 109.2 . . ?
C2 C1A H1A 109.2 . . ?
C6B C1A C2 110.8(4) . . ?
C6B C1A H1A 109.2 . . ?
C2 C3A H3AA 109.3 . . ?
C2 C3A H3AB 109.3 . . ?
H3AA C3A H3AB 107.9 . . ?
C4A C3A C2 111.7(5) . . ?
C4A C3A H3AA 109.3 . . ?
C4A C3A H3AB 109.3 . . ?
C5 C4A C3A 110.2(6) . . ?
C5 C4A H4AA 109.6 . . ?
C5 C4A H4AB 109.6 . . ?
C3A C4A H4AA 109.6 . . ?
C3A C4A H4AB 109.6 . . ?
H4AA C4A H4AB 108.1 . . ?
N1 C1B C2 116.1(11) . . ?
N1 C1B H1B 112.5 . . ?
N1 C1B C6A 99.6(14) . . ?
C2 C1B H1B 112.5 . . ?
C6A C1B C2 102.6(14) . . ?
C6A C1B H1B 112.5 . . ?
N2 C6A H6A 111.0 . . ?
C5 C6A N2 103.9(9) . . ?
C5 C6A H6A 111.0 . . ?
C1B C6A N2 105.4(13) . . ?
C1B C6A C5 114.1(14) . . ?
C1B C6A H6A 111.0 . . ?
C2 C3B H3BA 111.0 . . ?
C2 C3B H3BB 111.0 . . ?
C2 C3B C4B 104.0(17) . . ?
H3BA C3B H3BB 109.0 . . ?
C4B C3B H3BA 111.0 . . ?
C4B C3B H3BB 111.0 . . ?
C5 C4B H4BA 108.9 . . ?
C5 C4B H4BB 108.9 . . ?
C3B C4B C5 113.3(17) . . ?
C3B C4B H4BA 108.9 . . ?
C3B C4B H4BB 108.9 . . ?
H4BA C4B H4BB 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C13 C12 18.6(4) . . . . ?
Y1 O1 C13 C8 -159.2(2) . . . . ?
Y1 O3 C21 C20 -11.8(4) . . . . ?
Y1 O3 C21 C16 167.7(2) . . . . ?
Y1 O2 C12 C11 166.4(3) . . . . ?
Y1 O2 C12 C13 -13.9(3) . . . . ?
Y1 O4 C20 C21 10.9(3) . . . . ?
Y1 O4 C20 C19 -167.8(3) . . . . ?
Y1 O6 N3 O7 -1.6(3) . . . . ?
Y1 O6 N3 O8 -178.9(3) . . . . ?
Y1 O9 N4 O10 -6.4(3) . . . . ?
Y1 O9 N4 O11 174.4(3) . . . . ?
Y1 O5 C23 C24 86.8(4) . . . . ?
Y1 O10 N4 O9 6.5(3) . . . . ?
Y1 O10 N4 O11 -174.2(3) . . . . ?
Y1 O7 N3 O6 1.5(3) . . . . ?
Y1 O7 N3 O8 178.9(3) . . . . ?
Zn1 O1 C13 C12 -156.6(2) . . . . ?
Zn1 O1 C13 C8 25.6(4) . . . . ?
Zn1 O3 C21 C20 159.1(2) . . . . ?
Zn1 O3 C21 C16 -21.4(5) . . . . ?
Zn1 N2 C15 C16 4.3(5) . . . . ?
Zn1 N2 C6B C5 -174.4(4) . . . . ?
Zn1 N2 C6B C1A -52.6(5) . . . . ?
Zn1 N2 C6A C5 153.1(7) . . . . ?
Zn1 N2 C6A C1B 32.8(15) . . . . ?
Zn1 N1 C7 C8 0.8(6) . . . . ?
Zn1 N1 C1A C2 -146.6(3) . . . . ?
Zn1 N1 C1A C6B -25.4(6) . . . . ?
Zn1 N1 C1B C2 172.4(11) . . . . ?
Zn1 N1 C1B C6A 63.2(15) . . . . ?
O3 C21 C16 C15 -1.6(5) . . . . ?
O3 C21 C16 C17 -177.7(3) . . . . ?
O2 C12 C11 C10 -178.7(3) . . . . ?
O2 C12 C13 O1 -0.4(4) . . . . ?
O2 C12 C13 C8 177.5(3) . . . . ?
O4 C20 C21 O3 -1.1(4) . . . . ?
O4 C20 C21 C16 179.3(3) . . . . ?
O4 C20 C19 C18 -180.0(3) . . . . ?
N2 C6B C1A N1 49.9(6) . . . . ?
N2 C6B C1A C2 171.1(4) . . . . ?
N1 C1B C6A N2 -60.7(16) . . . . ?
N1 C1B C6A C5 -174.0(9) . . . . ?
C12 C11 C10 C9 0.8(5) . . . . ?
C11 C12 C13 O1 179.2(3) . . . . ?
C11 C12 C13 C8 -2.9(5) . . . . ?
C11 C10 C9 C8 -2.0(5) . . . . ?
C20 C21 C16 C15 178.0(3) . . . . ?
C20 C21 C16 C17 1.9(5) . . . . ?
C20 C19 C18 C17 -0.9(5) . . . . ?
C21 C20 C19 C18 1.5(5) . . . . ?
C21 C16 C15 N2 11.1(6) . . . . ?
C21 C16 C17 C18 -1.3(5) . . . . ?
C13 C12 C11 C10 1.7(5) . . . . ?
C13 C8 C7 N1 -16.6(6) . . . . ?
C13 C8 C9 C10 0.8(5) . . . . ?
C16 C17 C18 C19 0.8(5) . . . . ?
C19 C20 C21 O3 177.6(3) . . . . ?
C19 C20 C21 C16 -2.0(5) . . . . ?
C7 N1 C1A C2 47.2(6) . . . . ?
C7 N1 C1A C6B 168.5(4) . . . . ?
C7 N1 C1B C2 -27(2) . . . . ?
C7 N1 C1B C6A -135.9(10) . . . . ?
C7 C8 C13 O1 2.2(5) . . . . ?
C7 C8 C13 C12 -175.6(3) . . . . ?
C7 C8 C9 C10 178.1(3) . . . . ?
C9 C8 C13 O1 179.4(3) . . . . ?
C9 C8 C13 C12 1.6(5) . . . . ?
C9 C8 C7 N1 166.2(3) . . . . ?
C15 N2 C6B C5 13.3(8) . . . . ?
C15 N2 C6B C1A 135.2(4) . . . . ?
C15 N2 C6A C5 -46.9(13) . . . . ?
C15 N2 C6A C1B -167.2(10) . . . . ?
C15 C16 C17 C18 -177.7(3) . . . . ?
C17 C16 C15 N2 -172.7(3) . . . . ?
C14 O2 C12 C11 -2.7(5) . . . . ?
C14 O2 C12 C13 177.0(3) . . . . ?
C5 C6B C1A N1 178.4(4) . . . . ?
C5 C6B C1A C2 -60.5(7) . . . . ?
C2 C3A C4A C5 58.4(9) . . . . ?
C2 C1B C6A N2 179.7(8) . . . . ?
C2 C1B C6A C5 66.3(18) . . . . ?
C2 C3B C4B C5 -63(2) . . . . ?
C22 O4 C20 C21 -175.8(3) . . . . ?
C22 O4 C20 C19 5.6(5) . . . . ?
C6B N2 C15 C16 175.1(4) . . . . ?
C6B C5 C4A C3A -57.1(9) . . . . ?
C1A N1 C7 C8 164.8(4) . . . . ?
C1A C2 C3A C4A -59.1(8) . . . . ?
C3A C2 C1A N1 179.5(4) . . . . ?
C3A C2 C1A C6B 60.2(7) . . . . ?
C4A C5 C6B N2 177.6(4) . . . . ?
C4A C5 C6B C1A 57.9(8) . . . . ?
C1B N1 C7 C8 -156.2(11) . . . . ?
C1B C2 C3B C4B 70(2) . . . . ?
C6A N2 C15 C16 -151.4(9) . . . . ?
C6A C5 C4B C3B 57(2) . . . . ?
C3B C2 C1B N1 -177.7(12) . . . . ?
C3B C2 C1B C6A -70(2) . . . . ?
C4B C5 C6A N2 -173.3(10) . . . . ?
C4B C5 C6A C1B -59.1(19) . . . . ?

_smtbx_masks_special_details     ?
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
_smtbx_masks_void_content
1 -0.119 0.000 0.000 199.5 38.4 ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id Zn-Y_CC
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.626
_oxdiff_exptl_absorpt_empirical_full_min 0.366
