#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:53:54 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223886 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/03/7700395.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7700395
loop_
_publ_author_name
'Athanasopoulou, Angeliki A.'
'Baldoví, José J'
'Carrella, Luca M.'
'Rentschler, Eva'
_publ_section_title
;
 Field-induced slow magnetic relaxation in the first Dy(iii)-centered
 12-metallacrown-4 double-decker.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15381
_journal_page_last               15385
_journal_paper_doi               10.1039/c9dt02432h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C56 H36 Dy Ga8 N8 O28, 5(C H4 O), 3(O1), 2(C8 H18 N0.5)'
_chemical_formula_sum            'C77 H92 Dy Ga8 N9 O36'
_chemical_formula_weight         2439.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-15 deposited with the CCDC.    2019-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.093(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6911(4)
_cell_length_b                   18.1247(5)
_cell_length_c                   19.8116(5)
_cell_measurement_reflns_used    55634
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.54
_cell_volume                     4916.2(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 177 frames, detector distance = 115 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24260
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.886
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    2.990
_exptl_absorpt_correction_T_max  0.5866
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             2438
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.550
_refine_diff_density_min         -1.872
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10530
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0973
_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)+(0.1051P)²+66.3057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2554
_refine_ls_wR_factor_ref         0.2648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9052
_reflns_number_total             10530
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02432h2.cif
_cod_data_source_block           ata245c
_cod_depositor_comments          'Adding full bibliography for 7700395.cif.'
_cod_database_code               7700395
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.396
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H13 of O13, H14 of O14, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H16A of O16, H15 of O15, H18A of O18, H19A of O19
2. Restrained distances
 C53-C54 = C61-C62 = C65-C66
 1.54 with sigma of 0.01
 N5-C51 = C51-C52 = C52-C53 = N5-C59 = C59-C60 = C60-C61 = N5-C63 = C63-C64 =
 C64-C65
 1.52 with sigma of 0.01
 O19-C32
 1.45 with sigma of 0.02
 C31-O18
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C62 \\sim C61 \\sim C60 \\sim C59: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C51 \\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C32 \\sim O19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim O18: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O17(0.7) O17A(0.3) O15(0.5) H15(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) N5(0.5) C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5)
 C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) O19(0.5) H19A(0.5) O18(0.5) H18A(0.5)
 O20(0.5) C32(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 H31C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C59(H59A,H59B), C60(H60A,
 H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
5.b Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C)
5.c Aromatic/amide H refined with riding coordinates:
 O13(H13), O14(H14), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10),
 C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26)
5.d Tetrahedral OH refined with riding coordinates:
 O15(H15)
5.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C)
5.f Idealised tetrahedral OH refined as rotating group:
 O16(H16A), O19(H19A), O18(H18A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.500000 0.74920(3) 0.750000 0.03067(18) Uani 1 2 d S T P . .
Ga1 Ga 0.46004(8) 0.61314(6) 0.61110(5) 0.0334(2) Uani 1 1 d . . . . .
Ga2 Ga 0.31080(8) 0.62454(6) 0.82505(5) 0.0343(3) Uani 1 1 d . . . . .
Ga3 Ga 0.32146(9) 0.88440(6) 0.81810(6) 0.0422(3) Uani 1 1 d . . . . .
Ga4 Ga 0.45868(10) 0.87169(6) 0.60071(6) 0.0446(3) Uani 1 1 d . . . . .
O1 O 0.4056(5) 0.5292(4) 0.5713(3) 0.0378(14) Uani 1 1 d . . . . .
O2 O 0.2782(6) 0.5437(4) 0.7663(3) 0.0453(16) Uani 1 1 d . . . . .
O3 O 0.3899(5) 0.6513(3) 0.7466(3) 0.0359(14) Uani 1 1 d . . . . .
O4 O 0.1964(5) 0.6056(4) 0.8735(4) 0.0442(16) Uani 1 1 d . . . . .
O5 O 0.2265(5) 0.8374(4) 0.8780(4) 0.0457(17) Uani 1 1 d . . . . .
O6 O 0.3503(5) 0.7817(4) 0.7987(3) 0.0369(14) Uani 1 1 d . . . . .
O7 O 0.2372(7) 0.9630(4) 0.8105(4) 0.058(2) Uani 1 1 d . . . . .
O8 O 0.3853(6) 0.9578(4) 0.6241(4) 0.0499(18) Uani 1 1 d . . . . .
O9 O 0.4297(5) 0.8478(4) 0.6945(3) 0.0401(15) Uani 1 1 d . . . . .
O10 O 0.4506(6) 0.8940(4) 0.5087(4) 0.0500(18) Uani 1 1 d . . . . .
O11 O 0.4509(5) 0.6606(4) 0.5250(3) 0.0427(16) Uani 1 1 d . . . . .
O12 O 0.4751(5) 0.7161(3) 0.6386(3) 0.0339(13) Uani 1 1 d . . . . .
O13 O 0.5908(5) 0.5859(4) 0.6202(3) 0.0383(14) Uani 1 1 d . . . . .
H13 H 0.610452 0.545900 0.592407 0.046 Uiso 1 1 calc R . . . .
O14 O 0.5842(6) 0.9101(4) 0.6181(4) 0.0536(19) Uani 1 1 d . . . . .
H14 H 0.602629 0.949536 0.589181 0.064 Uiso 1 1 calc R . . . .
N1 N 0.3912(6) 0.5962(4) 0.6974(4) 0.0334(16) Uani 1 1 d . . . . .
N2 N 0.2976(6) 0.7322(4) 0.8410(4) 0.0369(17) Uani 1 1 d . . . . .
N3 N 0.3765(6) 0.9039(5) 0.7277(5) 0.0432(19) Uani 1 1 d . . . . .
N4 N 0.4762(6) 0.7661(4) 0.5833(4) 0.0382(17) Uani 1 1 d . . . . .
C1 C 0.3583(7) 0.4730(5) 0.6024(5) 0.038(2) Uani 1 1 d . . . . .
C2 C 0.3441(8) 0.4088(5) 0.5641(5) 0.042(2) Uani 1 1 d . . . . .
H2 H 0.370686 0.405416 0.519894 0.051 Uiso 1 1 calc R . . . .
C3 C 0.2918(10) 0.3504(6) 0.5904(7) 0.063(3) Uani 1 1 d . . . . .
H3 H 0.282339 0.307288 0.563843 0.075 Uiso 1 1 calc R . . . .
C4 C 0.2529(11) 0.3536(7) 0.6546(7) 0.061(3) Uani 1 1 d . . . . .
H4 H 0.217312 0.313073 0.672491 0.073 Uiso 1 1 calc R . . . .
C5 C 0.2669(10) 0.4173(6) 0.6925(6) 0.058(3) Uani 1 1 d . . . . .
H5 H 0.239699 0.420280 0.736506 0.069 Uiso 1 1 calc R . . . .
C6 C 0.3206(7) 0.4777(5) 0.6671(5) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.3306(7) 0.5417(5) 0.7120(5) 0.036(2) Uani 1 1 d . . . . .
C8 C 0.1570(8) 0.6486(7) 0.9209(5) 0.045(2) Uani 1 1 d . . . . .
C9 C 0.0929(9) 0.6135(8) 0.9686(6) 0.056(3) Uani 1 1 d . . . . .
H9 H 0.081560 0.561856 0.966176 0.067 Uiso 1 1 calc R . . . .
C10 C 0.0489(10) 0.6542(8) 1.0167(6) 0.066(3) Uani 1 1 d . . . . .
H10 H 0.007215 0.630386 1.048244 0.079 Uiso 1 1 calc R . . . .
C11 C 0.0625(11) 0.7293(9) 1.0215(7) 0.070(4) Uani 1 1 d . . . . .
H11 H 0.028543 0.756579 1.055044 0.085 Uiso 1 1 calc R . . . .
C12 C 0.1251(10) 0.7651(8) 0.9781(6) 0.061(3) Uani 1 1 d . . . . .
H12 H 0.136698 0.816568 0.982782 0.073 Uiso 1 1 calc R . . . .
C13 C 0.1715(8) 0.7248(7) 0.9269(5) 0.046(2) Uani 1 1 d . . . . .
C14 C 0.2349(8) 0.7656(6) 0.8803(5) 0.042(2) Uani 1 1 d . . . . .
C15 C 0.2454(10) 1.0213(6) 0.7689(7) 0.058(3) Uani 1 1 d . . . . .
C16 C 0.1910(12) 1.0840(8) 0.7861(9) 0.081(5) Uani 1 1 d . . . . .
H16 H 0.152129 1.084245 0.825803 0.098 Uiso 1 1 calc R . . . .
C17 C 0.1946(16) 1.1471(9) 0.7440(11) 0.110(7) Uani 1 1 d . . . . .
H17 H 0.156809 1.189314 0.755354 0.132 Uiso 1 1 calc R . . . .
C18 C 0.2510(17) 1.1485(9) 0.6875(12) 0.115(8) Uani 1 1 d . . . . .
H18 H 0.254753 1.191811 0.660666 0.138 Uiso 1 1 calc R . . . .
C19 C 0.3023(13) 1.0867(7) 0.6699(9) 0.084(5) Uani 1 1 d . . . . .
H19 H 0.339870 1.087050 0.629657 0.101 Uiso 1 1 calc R . . . .
C20 C 0.3006(9) 1.0223(6) 0.7102(7) 0.056(3) Uani 1 1 d . . . . .
C21 C 0.3574(9) 0.9592(6) 0.6858(6) 0.049(2) Uani 1 1 d . . . . .
C22 C 0.4509(8) 0.8482(6) 0.4567(5) 0.044(2) Uani 1 1 d . . . . .
C23 C 0.4409(9) 0.8804(7) 0.3917(6) 0.053(3) Uani 1 1 d . . . . .
H23 H 0.436705 0.932505 0.387353 0.064 Uiso 1 1 calc R . . . .
C24 C 0.4372(10) 0.8365(8) 0.3349(6) 0.063(3) Uani 1 1 d . . . . .
H24 H 0.430949 0.858797 0.291743 0.076 Uiso 1 1 calc R . . . .
C25 C 0.4424(12) 0.7609(8) 0.3397(6) 0.068(4) Uani 1 1 d . . . . .
H25 H 0.440173 0.731221 0.300200 0.081 Uiso 1 1 calc R . . . .
C26 C 0.4508(10) 0.7286(8) 0.4026(6) 0.060(3) Uani 1 1 d . . . . .
H26 H 0.453415 0.676373 0.406041 0.072 Uiso 1 1 calc R . . . .
C27 C 0.4556(8) 0.7714(6) 0.4616(5) 0.044(2) Uani 1 1 d . . . . .
C28 C 0.4617(8) 0.7304(5) 0.5253(5) 0.038(2) Uani 1 1 d . . . . .
O16 O 0.6317(6) 0.4614(4) 0.5657(4) 0.0525(19) Uani 1 1 d . . . . .
H16A H 0.609835 0.456996 0.526226 0.079 Uiso 1 1 calc GR . . . .
C30 C 0.7238(11) 0.4306(9) 0.5693(9) 0.086(5) Uani 1 1 d . . . . .
H30A H 0.769274 0.459719 0.542037 0.130 Uiso 1 1 calc GR . . . .
H30B H 0.721544 0.379885 0.552115 0.130 Uiso 1 1 calc GR . . . .
H30C H 0.745896 0.430146 0.616388 0.130 Uiso 1 1 calc GR . . . .
O17 O 0.6653(9) 0.9835(8) 0.5205(7) 0.072(4) Uani 0.7 1 d . . . A 1
O17A O 0.742(3) 0.983(2) 0.5050(18) 0.094(10) Uani 0.3 1 d . U . B 2
O15 O 0.2901(12) 0.8348(9) 0.5857(8) 0.051(4) Uani 0.5 1 d . . . C 1
H15 H 0.313309 0.831410 0.546653 0.076 Uiso 0.5 1 calc R . . C 1
C29 C 0.2481(19) 0.7648(14) 0.6053(14) 0.053(6) Uani 0.5 1 d . . . C 1
H29A H 0.176954 0.769597 0.608140 0.080 Uiso 0.5 1 calc GR . . C 1
H29B H 0.274158 0.750167 0.649440 0.080 Uiso 0.5 1 calc GR . . C 1
H29C H 0.264860 0.727296 0.571673 0.080 Uiso 0.5 1 calc GR . . C 1
N5 N 0.0252(15) 0.8271(16) 0.7337(10) 0.088(10) Uani 0.5 1 d D . . D -2
C51 C 0.0243(17) 0.8666(14) 0.8023(10) 0.157(9) Uani 1 1 d D U . D -2
H51A H 0.023604 0.826632 0.836278 0.189 Uiso 1 1 calc R . . D -2
H51B H 0.089255 0.890250 0.806082 0.189 Uiso 1 1 calc R . . D -2
C52 C -0.0478(18) 0.9241(15) 0.8285(13) 0.169(8) Uani 1 1 d D U . D -2
H52A H -0.109437 0.898776 0.840651 0.203 Uiso 1 1 calc R . . D -2
H52B H -0.062756 0.959127 0.791595 0.203 Uiso 1 1 calc R . . D -2
C53 C -0.012(2) 0.9679(17) 0.8899(15) 0.180(9) Uani 1 1 d D U . D -2
H53A H 0.059959 0.963257 0.889108 0.216 Uiso 1 1 calc R . . D -2
H53B H -0.034212 0.939280 0.929567 0.216 Uiso 1 1 calc R . . D -2
C54 C -0.032(2) 1.0491(17) 0.9081(18) 0.204(11) Uani 1 1 d D U . D -2
H54A H 0.001155 1.061101 0.950668 0.306 Uiso 1 1 calc R . . D -2
H54B H -0.006920 1.081079 0.872174 0.306 Uiso 1 1 calc R . . D -2
H54C H -0.102291 1.056796 0.913149 0.306 Uiso 1 1 calc R . . D -2
C59 C 0.1206(19) 0.791(2) 0.7123(16) 0.116(10) Uani 0.5 1 d D U . D -2
H59A H 0.148377 0.767401 0.753057 0.139 Uiso 0.5 1 calc R . . D -2
H59B H 0.165645 0.831437 0.699716 0.139 Uiso 0.5 1 calc R . . D -2
C60 C 0.126(3) 0.734(2) 0.6559(17) 0.123(10) Uani 0.5 1 d D U . D -2
H60A H 0.107458 0.685986 0.675934 0.147 Uiso 0.5 1 calc R . . D -2
H60B H 0.073733 0.746780 0.623062 0.147 Uiso 0.5 1 calc R . . D -2
C61 C 0.218(2) 0.721(3) 0.6155(19) 0.129(10) Uani 0.5 1 d D U . D -2
H61A H 0.219299 0.670905 0.596643 0.154 Uiso 0.5 1 calc R . . D -2
H61B H 0.276656 0.727801 0.644727 0.154 Uiso 0.5 1 calc R . . D -2
C62 C 0.219(3) 0.779(3) 0.558(2) 0.143(13) Uani 0.5 1 d D U . D -2
H62A H 0.277778 0.772809 0.530877 0.215 Uiso 0.5 1 calc R . . D -2
H62B H 0.160900 0.772116 0.529843 0.215 Uiso 0.5 1 calc R . . D -2
H62C H 0.217989 0.828746 0.577703 0.215 Uiso 0.5 1 calc R . . D -2
C63 C -0.0467(19) 0.7629(14) 0.7361(14) 0.071(8) Uani 0.5 1 d D . . D -2
H63A H -0.113414 0.782723 0.742540 0.085 Uiso 0.5 1 calc R . . D -2
H63B H -0.045401 0.736846 0.692217 0.085 Uiso 0.5 1 calc R . . D -2
C64 C -0.0253(16) 0.7075(12) 0.7921(12) 0.060(6) Uani 0.5 1 d D . . D -2
H64A H 0.040863 0.686590 0.786124 0.071 Uiso 0.5 1 calc R . . D -2
H64B H -0.027873 0.732414 0.836536 0.071 Uiso 0.5 1 calc R . . D -2
C65 C -0.101(2) 0.6462(13) 0.7893(14) 0.074(8) Uani 0.5 1 d D . . D -2
H65A H -0.096899 0.620993 0.745073 0.088 Uiso 0.5 1 calc R . . D -2
H65B H -0.167197 0.668045 0.793107 0.088 Uiso 0.5 1 calc R . . D -2
C66 C -0.087(3) 0.5892(17) 0.8460(15) 0.090(10) Uani 0.5 1 d D . . D -2
H66A H -0.136935 0.550877 0.842320 0.135 Uiso 0.5 1 calc R . . D -2
H66B H -0.021954 0.566749 0.841865 0.135 Uiso 0.5 1 calc R . . D -2
H66C H -0.092236 0.613791 0.889889 0.135 Uiso 0.5 1 calc R . . D -2
O19 O 0.0693(12) 0.4764(12) 0.8425(12) 0.076(6) Uani 0.5 1 d D U . E 1
H19A H 0.071488 0.453407 0.879251 0.114 Uiso 0.5 1 calc GR . . E 1
O18 O 0.2025(18) 0.8710(14) 0.4703(11) 0.082(6) Uani 0.5 1 d D U . F 1
H18A H 0.235246 0.902619 0.449198 0.123 Uiso 0.5 1 calc GR . . F 1
O20 O 0.081(2) 0.3278(15) 0.8134(16) 0.128(11) Uani 0.5 1 d . . . . .
C32 C -0.0266(18) 0.511(2) 0.835(2) 0.108(13) Uani 0.5 1 d D U . E 1
H32A H -0.065445 0.483318 0.802007 0.162 Uiso 0.5 1 calc GR . . E 1
H32B H -0.018333 0.561945 0.819112 0.162 Uiso 0.5 1 calc GR . . E 1
H32C H -0.060169 0.511258 0.878553 0.162 Uiso 0.5 1 calc GR . . E 1
C31 C 0.192(4) 0.8041(18) 0.4288(17) 0.137(18) Uani 0.5 1 d D U . F 1
H31A H 0.201440 0.816749 0.381164 0.206 Uiso 0.5 1 calc GR . . F 1
H31B H 0.127006 0.783090 0.435217 0.206 Uiso 0.5 1 calc GR . . F 1
H31C H 0.241683 0.767867 0.442460 0.206 Uiso 0.5 1 calc GR . . F 1
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'
Ga Ga 0.2307 1.6083 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0940
-1 0 0 0.0940
0 -1 1 0.1636
0 1 -1 0.1505
0 -1 -1 0.1966
0 1 1 0.1784
0 1 0 0.1799
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
O3 Dy1 O3 80.7(3) 2_656 .
O3 Dy1 O6 138.3(2) . 2_656
O3 Dy1 O6 68.7(2) . .
O3 Dy1 O6 68.7(2) 2_656 2_656
O3 Dy1 O6 138.3(2) 2_656 .
O6 Dy1 O6 150.9(3) . 2_656
O9 Dy1 O3 107.9(2) . .
O9 Dy1 O3 150.8(2) . 2_656
O9 Dy1 O3 150.8(2) 2_656 .
O9 Dy1 O3 107.9(2) 2_656 2_656
O9 Dy1 O6 88.5(2) 2_656 .
O9 Dy1 O6 88.5(2) . 2_656
O9 Dy1 O6 68.7(2) 2_656 2_656
O9 Dy1 O6 68.7(2) . .
O9 Dy1 O9 78.5(3) . 2_656
O9 Dy1 O12 135.8(2) 2_656 .
O9 Dy1 O12 135.8(2) . 2_656
O9 Dy1 O12 71.7(2) . .
O9 Dy1 O12 71.7(2) 2_656 2_656
O12 Dy1 O3 71.4(2) . .
O12 Dy1 O3 71.4(2) 2_656 2_656
O12 Dy1 O3 85.7(2) 2_656 .
O12 Dy1 O3 85.7(2) . 2_656
O12 Dy1 O6 109.3(2) 2_656 2_656
O12 Dy1 O6 78.5(2) . 2_656
O12 Dy1 O6 109.3(2) . .
O12 Dy1 O6 78.5(2) 2_656 .
O12 Dy1 O12 149.9(3) 2_656 .
O1 Ga1 O11 87.9(3) . .
O1 Ga1 O12 159.5(3) . .
O1 Ga1 N1 92.8(3) . .
O11 Ga1 O12 80.0(3) . .
O11 Ga1 N1 144.0(3) . .
O12 Ga1 N1 87.6(3) . .
O13 Ga1 O1 102.0(3) . .
O13 Ga1 O11 105.4(3) . .
O13 Ga1 O12 97.2(3) . .
O13 Ga1 N1 109.5(3) . .
O2 Ga2 O3 80.6(3) . .
O2 Ga2 N2 145.5(3) . .
O3 Ga2 N2 86.2(3) . .
O4 Ga2 O2 88.7(3) . .
O4 Ga2 O3 156.7(3) . .
O4 Ga2 N2 91.3(3) . .
O13 Ga2 O2 103.5(3) 2_656 .
O13 Ga2 O3 98.9(3) 2_656 .
O13 Ga2 O4 103.8(3) 2_656 .
O13 Ga2 N2 110.0(3) 2_656 .
O5 Ga3 N3 151.9(3) . .
O6 Ga3 O5 80.7(3) . .
O6 Ga3 N3 85.1(3) . .
O7 Ga3 O5 88.3(4) . .
O7 Ga3 O6 148.6(4) . .
O7 Ga3 O14 107.2(4) . 2_656
O7 Ga3 N3 91.6(4) . .
O14 Ga3 O5 99.1(3) 2_656 .
O14 Ga3 O6 103.5(3) 2_656 .
O14 Ga3 N3 107.8(4) 2_656 .
O8 Ga4 O9 80.9(3) . .
O8 Ga4 N4 154.6(4) . .
O9 Ga4 N4 88.6(3) . .
O10 Ga4 O8 91.7(3) . .
O10 Ga4 O9 164.9(3) . .
O10 Ga4 O14 98.6(4) . .
O10 Ga4 N4 92.7(3) . .
O14 Ga4 O8 97.7(4) . .
O14 Ga4 O9 95.5(3) . .
O14 Ga4 N4 106.3(4) . .
C1 O1 Ga1 127.6(6) . .
C7 O2 Ga2 113.3(6) . .
Ga2 O3 Dy1 121.7(3) . .
N1 O3 Dy1 123.8(5) . .
N1 O3 Ga2 112.7(5) . .
C8 O4 Ga2 126.4(7) . .
C14 O5 Ga3 113.3(7) . .
Ga3 O6 Dy1 120.0(3) . .
N2 O6 Dy1 121.9(5) . .
N2 O6 Ga3 112.6(5) . .
C15 O7 Ga3 127.3(8) . .
C21 O8 Ga4 113.9(7) . .
Ga4 O9 Dy1 122.7(3) . .
N3 O9 Dy1 123.4(5) . .
N3 O9 Ga4 112.9(5) . .
C22 O10 Ga4 128.5(6) . .
C28 O11 Ga1 115.8(6) . .
Ga1 O12 Dy1 121.9(3) . .
N4 O12 Dy1 124.6(5) . .
N4 O12 Ga1 113.3(5) . .
Ga1 O13 H13 114.7 . .
Ga2 O13 Ga1 130.5(4) 2_656 .
Ga2 O13 H13 114.7 2_656 .
Ga3 O14 Ga4 131.4(4) 2_656 .
Ga3 O14 H14 114.3 2_656 .
Ga4 O14 H14 114.3 . .
O3 N1 Ga1 120.0(5) . .
C7 N1 Ga1 127.2(6) . .
C7 N1 O3 111.9(8) . .
O6 N2 Ga2 118.6(6) . .
C14 N2 Ga2 127.6(8) . .
C14 N2 O6 113.1(8) . .
O9 N3 Ga3 119.3(6) . .
C21 N3 Ga3 128.8(8) . .
C21 N3 O9 110.7(9) . .
O12 N4 Ga4 119.1(6) . .
C28 N4 Ga4 127.4(6) . .
C28 N4 O12 110.7(7) . .
O1 C1 C2 116.3(9) . .
O1 C1 C6 123.6(9) . .
C6 C1 C2 120.0(9) . .
C1 C2 H2 119.9 . .
C3 C2 C1 120.2(10) . .
C3 C2 H2 119.9 . .
C2 C3 H3 119.4 . .
C2 C3 C4 121.1(11) . .
C4 C3 H3 119.4 . .
C3 C4 H4 120.7 . .
C3 C4 C5 118.6(11) . .
C5 C4 H4 120.7 . .
C4 C5 H5 119.2 . .
C4 C5 C6 121.5(11) . .
C6 C5 H5 119.2 . .
C1 C6 C5 118.5(9) . .
C1 C6 C7 125.1(9) . .
C5 C6 C7 116.4(9) . .
O2 C7 N1 120.6(9) . .
O2 C7 C6 118.3(8) . .
N1 C7 C6 121.0(9) . .
O4 C8 C9 116.8(11) . .
O4 C8 C13 125.3(10) . .
C13 C8 C9 117.9(10) . .
C8 C9 H9 120.1 . .
C10 C9 C8 119.7(13) . .
C10 C9 H9 120.1 . .
C9 C10 H10 119.0 . .
C9 C10 C11 121.9(12) . .
C11 C10 H10 119.0 . .
C10 C11 H11 119.8 . .
C10 C11 C12 120.5(12) . .
C12 C11 H11 119.8 . .
C11 C12 H12 120.4 . .
C11 C12 C13 119.2(14) . .
C13 C12 H12 120.4 . .
C8 C13 C12 120.7(11) . .
C8 C13 C14 121.8(9) . .
C12 C13 C14 117.5(11) . .
O5 C14 C13 118.1(9) . .
N2 C14 O5 119.9(10) . .
N2 C14 C13 122.0(10) . .
O7 C15 C16 116.3(13) . .
O7 C15 C20 124.8(10) . .
C20 C15 C16 118.9(12) . .
C15 C16 H16 120.2 . .
C15 C16 C17 119.5(16) . .
C17 C16 H16 120.2 . .
C16 C17 H17 119.4 . .
C18 C17 C16 121.2(15) . .
C18 C17 H17 119.4 . .
C17 C18 H18 120.4 . .
C17 C18 C19 119.2(17) . .
C19 C18 H18 120.4 . .
C18 C19 H19 119.2 . .
C18 C19 C20 121.6(16) . .
C20 C19 H19 119.2 . .
C15 C20 C19 119.5(11) . .
C15 C20 C21 123.7(11) . .
C19 C20 C21 116.7(12) . .
O8 C21 N3 121.5(10) . .
O8 C21 C20 119.2(10) . .
N3 C21 C20 119.2(11) . .
O10 C22 C23 116.5(10) . .
O10 C22 C27 124.8(9) . .
C27 C22 C23 118.6(10) . .
C22 C23 H23 119.8 . .
C24 C23 C22 120.3(11) . .
C24 C23 H23 119.8 . .
C23 C24 H24 119.4 . .
C25 C24 C23 121.1(11) . .
C25 C24 H24 119.4 . .
C24 C25 H25 120.4 . .
C24 C25 C26 119.2(13) . .
C26 C25 H25 120.4 . .
C25 C26 H26 119.3 . .
C25 C26 C27 121.4(13) . .
C27 C26 H26 119.3 . .
C22 C27 C26 119.3(10) . .
C22 C27 C28 124.6(10) . .
C26 C27 C28 116.0(10) . .
O11 C28 N4 120.2(8) . .
O11 C28 C27 119.5(9) . .
N4 C28 C27 120.2(9) . .
C30 O16 H16A 109.5 . .
O16 C30 H30A 109.5 . .
O16 C30 H30B 109.5 . .
O16 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 O15 H15 109.5 . .
O15 C29 H29A 109.5 . .
O15 C29 H29B 109.5 . .
O15 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C59 N5 C51 117(2) . .
C59 N5 C63 104(2) . .
C63 N5 C51 109(2) . .
N5 C51 H51A 105.1 . .
N5 C51 H51B 105.1 . .
H51A C51 H51B 105.9 . .
C52 C51 N5 129(2) . .
C52 C51 H51A 105.1 . .
C52 C51 H51B 105.1 . .
C51 C52 H52A 108.6 . .
C51 C52 H52B 108.6 . .
C51 C52 C53 115(2) . .
H52A C52 H52B 107.6 . .
C53 C52 H52A 108.6 . .
C53 C52 H52B 108.6 . .
C52 C53 H53A 105.1 . .
C52 C53 H53B 105.1 . .
C52 C53 C54 129(3) . .
H53A C53 H53B 105.9 . .
C54 C53 H53A 105.1 . .
C54 C53 H53B 105.1 . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54B 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
N5 C59 H59A 106.7 . .
N5 C59 H59B 106.7 . .
N5 C59 C60 122(3) . .
H59A C59 H59B 106.6 . .
C60 C59 H59A 106.7 . .
C60 C59 H59B 106.7 . .
C59 C60 H60A 106.9 . .
C59 C60 H60B 106.9 . .
H60A C60 H60B 106.7 . .
C61 C60 C59 122(3) . .
C61 C60 H60A 106.9 . .
C61 C60 H60B 106.9 . .
C60 C61 H61A 110.4 . .
C60 C61 H61B 110.4 . .
C60 C61 C62 107(3) . .
H61A C61 H61B 108.6 . .
C62 C61 H61A 110.4 . .
C62 C61 H61B 110.4 . .
C61 C62 H62A 109.5 . .
C61 C62 H62B 109.5 . .
C61 C62 H62C 109.5 . .
H62A C62 H62B 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
N5 C63 H63A 108.8 . .
N5 C63 H63B 108.8 . .
H63A C63 H63B 107.7 . .
C64 C63 N5 114(2) . .
C64 C63 H63A 108.8 . .
C64 C63 H63B 108.8 . .
C63 C64 H64A 109.9 . .
C63 C64 H64B 109.9 . .
H64A C64 H64B 108.3 . .
C65 C64 C63 108.9(17) . .
C65 C64 H64A 109.9 . .
C65 C64 H64B 109.9 . .
C64 C65 H65A 109.2 . .
C64 C65 H65B 109.2 . .
C64 C65 C66 112(2) . .
H65A C65 H65B 107.9 . .
C66 C65 H65A 109.2 . .
C66 C65 H65B 109.2 . .
C65 C66 H66A 109.5 . .
C65 C66 H66B 109.5 . .
C65 C66 H66C 109.5 . .
H66A C66 H66B 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
C32 O19 H19A 109.5 . .
C31 O18 H18A 109.5 . .
O19 C32 H32A 109.5 . .
O19 C32 H32B 109.5 . .
O19 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
O18 C31 H31A 109.5 . .
O18 C31 H31B 109.5 . .
O18 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O3 2.329(6) .
Dy1 O3 2.329(6) 2_656
Dy1 O6 2.342(7) .
Dy1 O6 2.342(7) 2_656
Dy1 O9 2.308(6) 2_656
Dy1 O9 2.308(6) .
Dy1 O12 2.312(6) 2_656
Dy1 O12 2.312(6) .
Ga1 O1 1.869(6) .
Ga1 O11 1.915(7) .
Ga1 O12 1.955(6) .
Ga1 O13 1.865(7) .
Ga1 N1 1.978(8) .
Ga2 O2 1.923(7) .
Ga2 O3 1.957(7) .
Ga2 O4 1.870(7) .
Ga2 O13 1.865(7) 2_656
Ga2 N2 1.985(8) .
Ga3 O5 1.956(8) .
Ga3 O6 1.942(7) .
Ga3 O7 1.840(8) .
Ga3 O14 1.866(8) 2_656
Ga3 N3 1.977(9) .
Ga4 O8 1.913(8) .
Ga4 O9 1.950(7) .
Ga4 O10 1.870(7) .
Ga4 O14 1.885(8) .
Ga4 N4 1.959(8) .
O1 C1 1.356(11) .
O2 C7 1.295(12) .
O3 N1 1.396(9) .
O4 C8 1.336(12) .
O5 C14 1.308(13) .
O6 N2 1.424(10) .
O7 C15 1.345(15) .
O8 C21 1.282(14) .
O9 N3 1.413(11) .
O10 C22 1.325(13) .
O11 C28 1.274(12) .
O12 N4 1.422(9) .
O13 H13 0.9500 .
O14 H14 0.9500 .
N1 C7 1.322(12) .
N2 C14 1.308(13) .
N3 C21 1.326(13) .
N4 C28 1.334(13) .
C1 C2 1.404(13) .
C1 C6 1.385(14) .
C2 H2 0.9500 .
C2 C3 1.381(16) .
C3 H3 0.9500 .
C3 C4 1.381(17) .
C4 H4 0.9500 .
C4 C5 1.391(16) .
C5 H5 0.9500 .
C5 C6 1.412(14) .
C6 C7 1.468(13) .
C8 C9 1.439(15) .
C8 C13 1.400(17) .
C9 H9 0.9500 .
C9 C10 1.348(17) .
C10 H10 0.9500 .
C10 C11 1.38(2) .
C11 H11 0.9500 .
C11 C12 1.378(19) .
C12 H12 0.9500 .
C12 C13 1.403(16) .
C13 C14 1.468(16) .
C15 C16 1.401(16) .
C15 C20 1.389(19) .
C16 H16 0.9500 .
C16 C17 1.42(2) .
C17 H17 0.9500 .
C17 C18 1.36(3) .
C18 H18 0.9500 .
C18 C19 1.367(19) .
C19 H19 0.9500 .
C19 C20 1.413(18) .
C20 C21 1.466(15) .
C22 C23 1.419(13) .
C22 C27 1.396(15) .
C23 H23 0.9500 .
C23 C24 1.380(18) .
C24 H24 0.9500 .
C24 C25 1.374(19) .
C25 H25 0.9500 .
C25 C26 1.382(16) .
C26 H26 0.9500 .
C26 C27 1.404(16) .
C27 C28 1.466(13) .
O16 H16A 0.8400 .
O16 C30 1.382(16) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
O15 H15 0.8400 .
O15 C29 1.45(3) .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
N5 C51 1.537(10) .
N5 C59 1.521(10) .
N5 C63 1.525(10) .
C51 H51A 0.9900 .
C51 H51B 0.9900 .
C51 C52 1.527(10) .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C52 C53 1.532(10) .
C53 H53A 0.9900 .
C53 H53B 0.9900 .
C53 C54 1.539(10) .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C59 H59A 0.9900 .
C59 H59B 0.9900 .
C59 C60 1.523(10) .
C60 H60A 0.9900 .
C60 H60B 0.9900 .
C60 C61 1.519(10) .
C61 H61A 0.9900 .
C61 H61B 0.9900 .
C61 C62 1.541(10) .
C62 H62A 0.9800 .
C62 H62B 0.9800 .
C62 H62C 0.9800 .
C63 H63A 0.9900 .
C63 H63B 0.9900 .
C63 C64 1.523(10) .
C64 H64A 0.9900 .
C64 H64B 0.9900 .
C64 C65 1.521(10) .
C65 H65A 0.9900 .
C65 H65B 0.9900 .
C65 C66 1.538(10) .
C66 H66A 0.9800 .
C66 H66B 0.9800 .
C66 H66C 0.9800 .
O19 H19A 0.8400 .
O19 C32 1.462(18) .
O18 H18A 0.8400 .
O18 C31 1.47(2) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
