#------------------------------------------------------------------------------
#$Date: 2021-01-07 08:18:02 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260749 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/57/7705716.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_7705716
loop_
_publ_author_name
'Koehne, Ingo'
'Lik, Artur'
'Gerstel, Miriam'
'Bruhn, Clemens'
'Reithmaier, Johann Peter'
'Benyoucef, Mohamed'
'Pietschnig, Rudolf'
_publ_section_title
;
 Functionalised phosphonate ester supported lanthanide (Ln = La, Nd, Dy,
 Er) complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16683
_journal_page_last               16692
_journal_paper_doi               10.1039/d0dt03047c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H54 Br2 Cl3 Dy O7 P2, 2(C2 H6 O)'
_chemical_formula_sum            'C48 H66 Br2 Cl3 Dy O9 P2'
_chemical_formula_weight         1277.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2020-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                101.357(3)
_cell_angle_beta                 98.671(3)
_cell_angle_gamma                111.903(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2192(4)
_cell_length_b                   13.3757(4)
_cell_length_c                   20.6992(7)
_cell_measurement_reflns_used    57069
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.53
_cell_measurement_theta_min      3.71
_cell_volume                     2738.39(18)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Mercury (P. A. Wood et al., 2020)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.83, Darmstadt 2018
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20943
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.152
_diffrn_reflns_theta_min         3.706
_exptl_absorpt_coefficient_mu    11.311
_exptl_absorpt_correction_T_max  0.2375
_exptl_absorpt_correction_T_min  0.0380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0470
_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)+(0.0942P)²+3.2911P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9981
_reflns_number_total             10129
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03047c2.cif
_cod_data_source_block           sv0796
_cod_depositor_comments
'Adding full bibliography for 7705708--7705721.cif.'
_cod_original_cell_volume        2738.39(17)
_cod_database_code               7705716
_shelx_shelxl_version_number     2017/1
_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   0.200
_shelx_estimated_absorpt_t_min   0.150
_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, All O(H,H) groups
2. Restrained distances
 O9-C47
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C43A \\sim C44A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C43, C44, C43A, C44A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O7, C43, C44} sigma for 1-2: 0.02, 1-3: 0.04
{O7, C43A, C44A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7, C43, C44}
{O8, C45, C46} sigma for 1-2: 0.02, 1-3: 0.04
{O8, C45A, C46A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O8, C45, C46}
6. Others
 Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Sof(H8B)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=1-FVAR(2)
 Sof(H8A)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C43(H43A,H43B), C43A(H43C,H43D), C45(H45A,H45B),
 C45A(H45C,H45D), C47(H47A,H47B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C25(H25), C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35)
7.d Tetrahedral OH refined with riding coordinates:
 O8(H8A), O8(H8B)
7.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C44(H44A,H44B,H44C), C44A(H44D,H44E,H44F), C46(H46A,H46B,H46C),
 C46A(H46D,H46E,H46F), C48(H48A,H48B,H48C)
7.f Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.28888(2) 0.75481(2) 0.75603(2) 0.03400(9) Uani 1 1 d . . . . .
C1 C 0.2058(4) 0.8953(3) 0.6085(2) 0.0356(8) Uani 1 1 d . . . . .
H1A H 0.135356 0.830273 0.615939 0.043 Uiso 1 1 calc R . . . .
H1B H 0.221878 0.962171 0.645171 0.043 Uiso 1 1 calc R . . . .
Br1 Br -0.01641(5) 0.95863(4) 0.33178(2) 0.04396(12) Uani 1 1 d . . . . .
P1 P 0.35433(9) 0.87263(8) 0.61686(5) 0.0323(2) Uani 1 1 d . . . . .
O1 O 0.3775(3) 0.8318(2) 0.67736(14) 0.0350(6) Uani 1 1 d . . . . .
Cl1 Cl 0.19410(13) 0.90351(9) 0.78679(5) 0.0494(3) Uani 1 1 d . . . . .
P2 P 0.20216(9) 0.60734(8) 0.88644(5) 0.0303(2) Uani 1 1 d . . . . .
Br2 Br 0.29260(6) 0.16259(4) 1.00291(3) 0.05952(16) Uani 1 1 d . . . . .
C2 C 0.1544(4) 0.9117(3) 0.5412(2) 0.0325(7) Uani 1 1 d . . . . .
O2 O 0.3553(3) 0.7951(2) 0.54997(14) 0.0365(6) Uani 1 1 d . . . . .
Cl2 Cl 0.42322(10) 0.62924(8) 0.74467(5) 0.0409(2) Uani 1 1 d . . . . .
O3 O 0.4616(3) 0.9895(2) 0.62063(14) 0.0343(6) Uani 1 1 d . . . . .
Cl3 Cl 0.08158(9) 0.62274(8) 0.65885(5) 0.0372(2) Uani 1 1 d . . . . .
C3 C 0.0584(4) 0.8186(3) 0.4898(2) 0.0335(8) Uani 1 1 d . . . . .
O5 O 0.0838(3) 0.4884(2) 0.86027(14) 0.0349(6) Uani 1 1 d . . . . .
C5 C -0.0818(4) 0.6183(4) 0.4480(2) 0.0430(9) Uani 1 1 d . . . . .
H5 H -0.112163 0.545797 0.455060 0.052 Uiso 1 1 calc R . . . .
O4 O 0.2116(3) 0.6716(2) 0.83476(13) 0.0338(5) Uani 1 1 d . . . . .
C4 C 0.0073(4) 0.7077(3) 0.4988(2) 0.0386(8) Uani 1 1 d . . . . .
H4 H 0.036845 0.696980 0.541290 0.046 Uiso 1 1 calc R . . . .
C7 C -0.0862(4) 0.7355(4) 0.3738(2) 0.0395(9) Uani 1 1 d . . . . .
H7 H -0.119335 0.743374 0.331009 0.047 Uiso 1 1 calc R . . . .
O6 O 0.1771(3) 0.6635(2) 0.95338(13) 0.0328(5) Uani 1 1 d . . . . .
C6 C -0.1305(4) 0.6314(4) 0.3842(2) 0.0450(10) Uani 1 1 d . . . . .
H6 H -0.193594 0.568128 0.349026 0.054 Uiso 1 1 calc R . . . .
C9 C 0.0535(4) 0.9401(4) 0.4166(2) 0.0361(8) Uani 1 1 d . . . . .
C8 C 0.0082(4) 0.8326(3) 0.4253(2) 0.0356(8) Uani 1 1 d . . . . .
C10 C 0.1474(4) 1.0343(3) 0.4665(2) 0.0364(8) Uani 1 1 d . . . . .
C11 C 0.1926(4) 1.1446(4) 0.4580(2) 0.0404(9) Uani 1 1 d . . . . .
H11 H 0.157899 1.155459 0.416417 0.048 Uiso 1 1 calc R . . . .
C12 C 0.2840(4) 1.2343(4) 0.5081(3) 0.0440(10) Uani 1 1 d . . . . .
H12 H 0.312494 1.306977 0.501340 0.053 Uiso 1 1 calc R . . . .
C13 C 0.3372(4) 1.2204(4) 0.5702(2) 0.0436(9) Uani 1 1 d . . . . .
H13 H 0.401803 1.283790 0.604820 0.052 Uiso 1 1 calc R . . . .
C14 C 0.2968(4) 1.1172(3) 0.5811(2) 0.0374(8) Uani 1 1 d . . . . .
H14 H 0.333668 1.109887 0.623372 0.045 Uiso 1 1 calc R . . . .
C16 C 0.3063(5) 0.6718(3) 0.5345(2) 0.0420(9) Uani 1 1 d . . . . .
H16 H 0.229773 0.641833 0.555053 0.050 Uiso 1 1 calc R . . . .
C15 C 0.2002(4) 1.0194(3) 0.5303(2) 0.0344(8) Uani 1 1 d . . . . .
C17 C 0.2601(5) 0.6283(4) 0.4586(3) 0.0520(11) Uani 1 1 d . . . . .
H17A H 0.197903 0.658348 0.441926 0.078 Uiso 1 1 calc GR . . . .
H17B H 0.215783 0.546225 0.445677 0.078 Uiso 1 1 calc GR . . . .
H17C H 0.336484 0.651760 0.438673 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.4166(6) 0.6434(4) 0.5643(3) 0.0536(12) Uani 1 1 d . . . . .
H18A H 0.388408 0.562052 0.550055 0.080 Uiso 1 1 calc GR . . . .
H18B H 0.437806 0.669450 0.614060 0.080 Uiso 1 1 calc GR . . . .
H18C H 0.495261 0.680307 0.548315 0.080 Uiso 1 1 calc GR . . . .
C19 C 0.6008(4) 1.0128(4) 0.6212(2) 0.0416(9) Uani 1 1 d . . . . .
H19 H 0.605090 0.950818 0.587030 0.050 Uiso 1 1 calc R . . . .
C20 C 0.6528(5) 1.1196(4) 0.6008(3) 0.0507(11) Uani 1 1 d . . . . .
H20A H 0.745602 1.139734 0.599393 0.076 Uiso 1 1 calc GR . . . .
H20B H 0.646690 1.179768 0.633930 0.076 Uiso 1 1 calc GR . . . .
H20C H 0.600076 1.109121 0.555715 0.076 Uiso 1 1 calc GR . . . .
C21 C 0.6724(5) 1.0219(6) 0.6905(4) 0.0740(18) Uani 1 1 d . . . . .
H21A H 0.628985 0.952093 0.702542 0.111 Uiso 1 1 calc GR . . . .
H21B H 0.670786 1.084498 0.723598 0.111 Uiso 1 1 calc GR . . . .
H21C H 0.764517 1.035056 0.690810 0.111 Uiso 1 1 calc GR . . . .
C22 C 0.3544(4) 0.5955(3) 0.9153(2) 0.0325(8) Uani 1 1 d . . . . .
H22A H 0.401275 0.598643 0.878384 0.039 Uiso 1 1 calc R . . . .
H22B H 0.411059 0.661510 0.954295 0.039 Uiso 1 1 calc R . . . .
C23 C 0.3407(4) 0.4909(3) 0.9368(2) 0.0333(8) Uani 1 1 d . . . . .
C24 C 0.3335(4) 0.4873(4) 1.0036(2) 0.0363(8) Uani 1 1 d . . . . .
C25 C 0.3403(4) 0.5815(4) 1.0540(2) 0.0397(9) Uani 1 1 d . . . . .
H25 H 0.349022 0.648358 1.041953 0.048 Uiso 1 1 calc R . . . .
C26 C 0.3344(4) 0.5768(4) 1.1187(2) 0.0460(10) Uani 1 1 d . . . . .
H26 H 0.338923 0.640257 1.150934 0.055 Uiso 1 1 calc R . . . .
C27 C 0.3218(5) 0.4791(5) 1.1382(2) 0.0517(11) Uani 1 1 d . . . . .
H27 H 0.317886 0.477298 1.183541 0.062 Uiso 1 1 calc R . . . .
C28 C 0.3153(4) 0.3878(4) 1.0935(2) 0.0469(10) Uani 1 1 d . . . . .
H28 H 0.307481 0.322900 1.107785 0.056 Uiso 1 1 calc R . . . .
C29 C 0.3200(4) 0.3875(4) 1.0247(2) 0.0387(8) Uani 1 1 d . . . . .
C30 C 0.3122(4) 0.2953(4) 0.9760(2) 0.0412(9) Uani 1 1 d . . . . .
C31 C 0.3187(4) 0.2951(3) 0.9087(2) 0.0389(9) Uani 1 1 d . . . . .
C32 C 0.3118(4) 0.2007(4) 0.8594(2) 0.0445(10) Uani 1 1 d . . . . .
H32 H 0.299790 0.133293 0.871564 0.053 Uiso 1 1 calc R . . . .
C33 C 0.3219(5) 0.2056(4) 0.7957(2) 0.0475(10) Uani 1 1 d . . . . .
H33 H 0.317637 0.141889 0.763759 0.057 Uiso 1 1 calc R . . . .
C34 C 0.3390(4) 0.3051(4) 0.7761(2) 0.0425(9) Uani 1 1 d . . . . .
H34 H 0.346949 0.307856 0.731319 0.051 Uiso 1 1 calc R . . . .
C35 C 0.3441(4) 0.3961(3) 0.8210(2) 0.0377(8) Uani 1 1 d . . . . .
H35 H 0.355015 0.461831 0.806900 0.045 Uiso 1 1 calc R . . . .
C36 C 0.3333(4) 0.3960(3) 0.88933(19) 0.0336(8) Uani 1 1 d . . . . .
C37 C 0.0269(4) 0.4250(4) 0.7879(2) 0.0406(9) Uani 1 1 d . . . . .
H37 H 0.096569 0.446086 0.761978 0.049 Uiso 1 1 calc R . . . .
C38 C -0.0161(5) 0.3039(4) 0.7869(3) 0.0537(12) Uani 1 1 d . . . . .
H38A H -0.057355 0.256642 0.740026 0.081 Uiso 1 1 calc GR . . . .
H38B H -0.080291 0.284849 0.814710 0.081 Uiso 1 1 calc GR . . . .
H38C H 0.061177 0.291351 0.805322 0.081 Uiso 1 1 calc GR . . . .
C39 C -0.0847(4) 0.4527(5) 0.7603(3) 0.0516(11) Uani 1 1 d . . . . .
H39A H -0.119231 0.415261 0.711509 0.077 Uiso 1 1 calc GR . . . .
H39B H -0.052320 0.533988 0.767796 0.077 Uiso 1 1 calc GR . . . .
H39C H -0.155499 0.426977 0.783689 0.077 Uiso 1 1 calc GR . . . .
C40 C 0.0530(4) 0.6781(4) 0.9570(2) 0.0416(9) Uani 1 1 d . . . . .
H40 H -0.023541 0.613654 0.923065 0.050 Uiso 1 1 calc R . . . .
C41 C 0.0372(4) 0.6755(4) 1.0273(2) 0.0463(10) Uani 1 1 d . . . . .
H41A H -0.046604 0.679739 1.031968 0.069 Uiso 1 1 calc GR . . . .
H41B H 0.111044 0.739516 1.060609 0.069 Uiso 1 1 calc GR . . . .
H41C H 0.036735 0.605634 1.035437 0.069 Uiso 1 1 calc GR . . . .
C42 C 0.0644(6) 0.7845(5) 0.9407(3) 0.0591(13) Uani 1 1 d . . . . .
H42A H 0.074770 0.780170 0.894211 0.089 Uiso 1 1 calc GR . . . .
H42B H 0.141733 0.847399 0.972627 0.089 Uiso 1 1 calc GR . . . .
H42C H -0.015838 0.795998 0.944635 0.089 Uiso 1 1 calc GR . . . .
O7 O 0.4818(4) 0.8824(3) 0.83964(17) 0.0509(8) Uani 1 1 d D . . . .
C43 C 0.514(5) 0.983(2) 0.8937(16) 0.087(11) Uani 0.33(5) 1 d D U P A 1
H43A H 0.572959 0.985515 0.935028 0.104 Uiso 0.33(5) 1 calc R . P A 1
H43B H 0.431817 0.985103 0.905186 0.104 Uiso 0.33(5) 1 calc R . P A 1
C44 C 0.581(4) 1.080(2) 0.867(2) 0.088(9) Uani 0.33(5) 1 d D U P A 1
H44A H 0.665505 1.080980 0.860525 0.131 Uiso 0.33(5) 1 calc GR . P A 1
H44B H 0.595960 1.149571 0.900379 0.131 Uiso 0.33(5) 1 calc GR . P A 1
H44C H 0.524258 1.072320 0.824120 0.131 Uiso 0.33(5) 1 calc GR . P A 1
H7A H 0.560(6) 0.884(4) 0.836(3) 0.046(14) Uiso 1 1 d . . . . .
C43A C 0.487(2) 0.9605(13) 0.9007(6) 0.053(3) Uani 0.67(5) 1 d D U P A 2
H43C H 0.531620 0.946564 0.940871 0.064 Uiso 0.67(5) 1 calc R . P A 2
H43D H 0.395853 0.947217 0.904139 0.064 Uiso 0.67(5) 1 calc R . P A 2
C44A C 0.5593(13) 1.0785(9) 0.9012(18) 0.091(8) Uani 0.67(5) 1 d D U P A 2
H44D H 0.510623 1.094864 0.864245 0.136 Uiso 0.67(5) 1 calc GR . P A 2
H44E H 0.648020 1.090823 0.894818 0.136 Uiso 0.67(5) 1 calc GR . P A 2
H44F H 0.567110 1.128038 0.944833 0.136 Uiso 0.67(5) 1 calc GR . P A 2
O8 O 0.7280(4) 0.9022(4) 0.8410(2) 0.0712(11) Uani 1 1 d D . . . .
H8A H 0.731167 0.843913 0.818697 0.107 Uiso 0.555(15) 1 calc R . P B 1
H8B H 0.733320 0.845508 0.817949 0.107 Uiso 0.445(15) 1 calc R . P B 2
C45 C 0.8558(8) 0.9759(8) 0.8832(5) 0.054(3) Uani 0.555(15) 1 d D . P B 1
H45A H 0.896721 0.931813 0.903643 0.065 Uiso 0.555(15) 1 calc R . P B 1
H45B H 0.846399 1.029013 0.920710 0.065 Uiso 0.555(15) 1 calc R . P B 1
C46 C 0.9442(10) 1.0400(9) 0.8457(6) 0.059(3) Uani 0.555(15) 1 d D . P B 1
H46A H 0.974443 0.990871 0.817634 0.089 Uiso 0.555(15) 1 calc GR . P B 1
H46B H 1.020892 1.102822 0.878037 0.089 Uiso 0.555(15) 1 calc GR . P B 1
H46C H 0.895766 1.068926 0.816406 0.089 Uiso 0.555(15) 1 calc GR . P B 1
C45A C 0.8396(10) 1.0059(9) 0.8389(6) 0.052(3) Uani 0.445(15) 1 d D . P B 2
H45C H 0.850968 1.000015 0.792024 0.062 Uiso 0.445(15) 1 calc R . P B 2
H45D H 0.820941 1.072279 0.854063 0.062 Uiso 0.445(15) 1 calc R . P B 2
C46A C 0.9621(12) 1.0172(13) 0.8853(8) 0.067(4) Uani 0.445(15) 1 d D . P B 2
H46D H 0.985012 0.955168 0.867110 0.101 Uiso 0.445(15) 1 calc GR . P B 2
H46E H 0.946655 1.015166 0.930441 0.101 Uiso 0.445(15) 1 calc GR . P B 2
H46F H 1.035119 1.088561 0.888699 0.101 Uiso 0.445(15) 1 calc GR . P B 2
O9 O 0.7352(5) 0.7185(5) 0.7704(3) 0.0853(13) Uiso 1 1 d D . . . .
H9 H 0.657342 0.713866 0.761993 0.128 Uiso 1 1 calc GR . . . .
C48 C 0.7455(8) 0.6304(7) 0.6586(4) 0.089(2) Uiso 1 1 d . . . . .
H48A H 0.781392 0.644326 0.619298 0.134 Uiso 1 1 calc GR . . . .
H48B H 0.648430 0.596991 0.644576 0.134 Uiso 1 1 calc GR . . . .
H48C H 0.775420 0.578938 0.676529 0.134 Uiso 1 1 calc GR . . . .
C47 C 0.7916(8) 0.7351(7) 0.7107(4) 0.087(2) Uiso 1 1 d D . . . .
H47A H 0.765583 0.788456 0.691713 0.105 Uiso 1 1 calc R . . . .
H47B H 0.889539 0.767919 0.725488 0.105 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 Cl1 92.18(7) . . ?
O1 Dy1 Cl2 88.94(7) . . ?
O1 Dy1 Cl3 87.41(8) . . ?
O1 Dy1 O7 88.97(12) . . ?
Cl1 Dy1 Cl2 169.12(4) . . ?
Cl3 Dy1 Cl1 93.28(3) . . ?
Cl3 Dy1 Cl2 97.57(3) . . ?
O4 Dy1 O1 175.51(9) . . ?
O4 Dy1 Cl1 92.03(7) . . ?
O4 Dy1 Cl2 86.63(7) . . ?
O4 Dy1 Cl3 93.91(8) . . ?
O4 Dy1 O7 89.77(12) . . ?
O7 Dy1 Cl1 85.86(10) . . ?
O7 Dy1 Cl2 83.35(9) . . ?
O7 Dy1 Cl3 176.25(9) . . ?
H1A C1 H1B 107.4 . . ?
P1 C1 H1A 108.3 . . ?
P1 C1 H1B 108.3 . . ?
C2 C1 H1A 108.3 . . ?
C2 C1 H1B 108.3 . . ?
C2 C1 P1 116.1(3) . . ?
O1 P1 C1 111.02(18) . . ?
O1 P1 O2 112.88(16) . . ?
O1 P1 O3 114.44(16) . . ?
O2 P1 C1 111.80(18) . . ?
O3 P1 C1 102.65(17) . . ?
O3 P1 O2 103.41(15) . . ?
P1 O1 Dy1 146.40(17) . . ?
O5 P2 C22 110.26(17) . . ?
O4 P2 O5 112.36(16) . . ?
O4 P2 O6 114.16(15) . . ?
O4 P2 C22 112.01(18) . . ?
O6 P2 O5 104.18(15) . . ?
O6 P2 C22 103.26(16) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C15 120.1(4) . . ?
C15 C2 C1 120.8(3) . . ?
C16 O2 P1 124.6(3) . . ?
C19 O3 P1 124.2(2) . . ?
C2 C3 C4 122.2(4) . . ?
C2 C3 C8 120.0(4) . . ?
C4 C3 C8 117.8(4) . . ?
C37 O5 P2 124.1(3) . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.9(4) . . ?
C6 C5 H5 119.6 . . ?
P2 O4 Dy1 159.65(17) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 H4 119.3 . . ?
C6 C7 H7 119.0 . . ?
C6 C7 C8 122.0(4) . . ?
C8 C7 H7 119.0 . . ?
C40 O6 P2 123.6(2) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
C8 C9 Br1 118.4(3) . . ?
C10 C9 Br1 118.5(3) . . ?
C10 C9 C8 123.1(4) . . ?
C7 C8 C3 118.1(4) . . ?
C9 C8 C3 118.6(4) . . ?
C9 C8 C7 123.3(4) . . ?
C9 C10 C11 123.2(4) . . ?
C9 C10 C15 118.1(4) . . ?
C11 C10 C15 118.7(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.2(4) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(4) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(4) . . ?
C15 C14 H14 119.2 . . ?
O2 C16 H16 109.5 . . ?
O2 C16 C17 105.9(4) . . ?
O2 C16 C18 108.8(4) . . ?
C17 C16 H16 109.5 . . ?
C17 C16 C18 113.5(4) . . ?
C18 C16 H16 109.5 . . ?
C2 C15 C10 120.2(4) . . ?
C2 C15 C14 122.5(4) . . ?
C14 C15 C10 117.3(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 H19 109.8 . . ?
O3 C19 C20 105.0(3) . . ?
O3 C19 C21 109.1(4) . . ?
C20 C19 H19 109.8 . . ?
C21 C19 H19 109.8 . . ?
C21 C19 C20 113.3(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P2 C22 H22A 108.3 . . ?
P2 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 P2 115.9(3) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 C36 119.9(4) . . ?
C36 C23 C22 119.8(4) . . ?
C23 C24 C25 122.2(4) . . ?
C23 C24 C29 120.8(4) . . ?
C25 C24 C29 116.9(4) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 C24 121.5(4) . . ?
C26 C25 H25 119.3 . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 120.7(4) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.9(4) . . ?
C28 C27 H27 119.6 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 121.0(4) . . ?
C29 C28 H28 119.5 . . ?
C28 C29 C24 119.1(4) . . ?
C30 C29 C24 117.4(4) . . ?
C30 C29 C28 123.5(4) . . ?
C29 C30 Br2 117.8(3) . . ?
C29 C30 C31 123.7(4) . . ?
C31 C30 Br2 118.5(3) . . ?
C30 C31 C32 123.3(4) . . ?
C30 C31 C36 117.7(4) . . ?
C32 C31 C36 119.1(4) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.1(4) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.6(4) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.2(4) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.1 . . ?
C34 C35 C36 121.8(4) . . ?
C36 C35 H35 119.1 . . ?
C23 C36 C31 120.5(4) . . ?
C23 C36 C35 122.2(4) . . ?
C35 C36 C31 117.2(4) . . ?
O5 C37 H37 109.8 . . ?
O5 C37 C38 105.2(4) . . ?
O5 C37 C39 108.7(3) . . ?
C38 C37 H37 109.8 . . ?
C39 C37 H37 109.8 . . ?
C39 C37 C38 113.5(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O6 C40 H40 109.3 . . ?
O6 C40 C41 105.5(3) . . ?
O6 C40 C42 109.1(4) . . ?
C41 C40 H40 109.3 . . ?
C42 C40 H40 109.3 . . ?
C42 C40 C41 114.1(4) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Dy1 O7 H7A 120(4) . . ?
C43 O7 Dy1 134(2) . . ?
C43 O7 H7A 104(4) . . ?
C43A O7 Dy1 126.1(9) . . ?
C43A O7 H7A 113(4) . . ?
O7 C43 H43A 110.4 . . ?
O7 C43 H43B 110.4 . . ?
O7 C43 C44 107(2) . . ?
H43A C43 H43B 108.6 . . ?
C44 C43 H43A 110.4 . . ?
C44 C43 H43B 110.4 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O7 C43A H43C 109.1 . . ?
O7 C43A H43D 109.1 . . ?
O7 C43A C44A 112.3(10) . . ?
H43C C43A H43D 107.9 . . ?
C44A C43A H43C 109.1 . . ?
C44A C43A H43D 109.1 . . ?
C43A C44A H44D 109.5 . . ?
C43A C44A H44E 109.5 . . ?
C43A C44A H44F 109.5 . . ?
H44D C44A H44E 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
C45 O8 H8A 109.5 . . ?
C45A O8 H8B 109.5 . . ?
O8 C45 H45A 109.1 . . ?
O8 C45 H45B 109.1 . . ?
O8 C45 C46 112.5(8) . . ?
H45A C45 H45B 107.8 . . ?
C46 C45 H45A 109.1 . . ?
C46 C45 H45B 109.1 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O8 C45A H45C 110.2 . . ?
O8 C45A H45D 110.2 . . ?
H45C C45A H45D 108.5 . . ?
C46A C45A O8 107.7(9) . . ?
C46A C45A H45C 110.2 . . ?
C46A C45A H45D 110.2 . . ?
C45A C46A H46D 109.5 . . ?
C45A C46A H46E 109.5 . . ?
C45A C46A H46F 109.5 . . ?
H46D C46A H46E 109.5 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?
C47 O9 H9 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
O9 C47 H47A 109.4 . . ?
O9 C47 H47B 109.4 . . ?
C48 C47 O9 111.3(7) . . ?
C48 C47 H47A 109.4 . . ?
C48 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
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 O1 2.255(3) . ?
Dy1 Cl1 2.6030(10) . ?
Dy1 Cl2 2.6434(9) . ?
Dy1 Cl3 2.5885(10) . ?
Dy1 O4 2.251(3) . ?
Dy1 O7 2.354(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 P1 1.791(4) . ?
C1 C2 1.515(6) . ?
Br1 C9 1.913(4) . ?
P1 O1 1.487(3) . ?
P1 O2 1.562(3) . ?
P1 O3 1.555(3) . ?
P2 O5 1.567(3) . ?
P2 O4 1.490(3) . ?
P2 O6 1.558(3) . ?
P2 C22 1.798(4) . ?
Br2 C30 1.909(4) . ?
C2 C3 1.405(5) . ?
C2 C15 1.414(5) . ?
O2 C16 1.479(5) . ?
O3 C19 1.472(5) . ?
C3 C4 1.439(6) . ?
C3 C8 1.443(6) . ?
O5 C37 1.476(5) . ?
C5 H5 0.9500 . ?
C5 C4 1.353(6) . ?
C5 C6 1.419(7) . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.366(7) . ?
C7 C8 1.426(6) . ?
O6 C40 1.487(4) . ?
C6 H6 0.9500 . ?
C9 C8 1.394(6) . ?
C9 C10 1.391(6) . ?
C10 C11 1.427(6) . ?
C10 C15 1.447(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.356(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.410(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.359(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.431(6) . ?
C16 H16 1.0000 . ?
C16 C17 1.497(7) . ?
C16 C18 1.506(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.500(6) . ?
C19 C21 1.492(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.511(5) . ?
C23 C24 1.406(6) . ?
C23 C36 1.411(5) . ?
C24 C25 1.438(6) . ?
C24 C29 1.447(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.363(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.408(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.349(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.432(6) . ?
C29 C30 1.396(6) . ?
C30 C31 1.404(6) . ?
C31 C32 1.428(6) . ?
C31 C36 1.441(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.354(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.422(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.355(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.439(6) . ?
C37 H37 1.0000 . ?
C37 C38 1.501(7) . ?
C37 C39 1.499(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40 1.0000 . ?
C40 C41 1.499(6) . ?
C40 C42 1.491(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O7 C43 1.458(18) . ?
O7 H7A 0.88(6) . ?
O7 C43A 1.449(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.48(2) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C43A C44A 1.478(13) . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?
O8 H8A 0.8400 . ?
O8 H8B 0.8400 . ?
O8 C45 1.422(9) . ?
O8 C45A 1.496(10) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.478(12) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C45A H45C 0.9900 . ?
C45A H45D 0.9900 . ?
C45A C46A 1.490(14) . ?
C46A H46D 0.9800 . ?
C46A H46E 0.9800 . ?
C46A H46F 0.9800 . ?
O9 H9 0.8400 . ?
O9 C47 1.489(9) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 C47 1.445(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
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 0.427 0.670 0.291 44.4 2.6 ?
2 0.573 0.330 0.709 44.4 4.8 ?
