#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:53:39 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/23/7232379.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_7232379
loop_
_publ_author_name
'Tiihonen, Antti'
'Lahtinen, Manu'
_publ_section_title
;
 In-depth structural analysis of lanthanoid coordination networks based on
 a flexible tripodal zwitterionic isonicotinate ligand
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2286
_journal_paper_doi               10.1039/C8CE01015C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'C30.57 H28.7 F1.72 N3 Nd O8.57 S0.57, 2(Br), 0.43(C1 F3 O3 S1), 1.15(H2 O)'
_chemical_formula_sum            'C31 H31 Br2 F3 N3 Nd O11 S'
_chemical_formula_weight         1014.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                105.103(2)
_cell_angle_beta                 98.057(2)
_cell_angle_gamma                99.489(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4141(3)
_cell_length_b                   12.0776(3)
_cell_length_c                   18.7454(5)
_cell_measurement_reflns_used    8785
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.8660
_cell_volume                     1991.70(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    2.00    --  -41.65 -37.00  90.00   99
  2  ω   -114.00 -15.00   1.00    2.00    --  -41.65 -57.00-150.00   99
  3  ω    -62.00  23.00   1.00    2.00    --  -41.65  57.00   0.00   85
  4  ω      1.00  83.00   1.00    2.00    --   41.65 -99.00  90.00   82
  5  ω     41.00 141.00   1.00    8.00    --  112.00 -61.00-150.00  100
  6  ω     58.00 116.00   1.00    8.00    --  112.00-111.00 150.00   58
  7  ω     35.00  61.00   1.00    8.00    --  112.00 -94.00 -30.00   26
  8  ω     39.00  90.00   1.00    8.00    --  112.00 -45.00 150.00   51
  9  ω     43.00 129.00   1.00    8.00    --  112.00 -45.00   0.00   86
 10  ω     30.00 106.00   1.00    8.00    --  112.00 -94.00  30.00   76
 11  ω     91.00 176.00   1.00    8.00    --  112.00  30.00 -60.00   85
 12  ω     70.00 101.00   1.00    8.00    --  112.00 -94.00 -30.00   31
 13  ω     30.00  96.00   1.00    8.00    --  112.00 -94.00-180.00   66
 14  ω    114.00 141.00   1.00    8.00    --  112.00 111.00 -60.00   27
 15  ω     77.00 114.00   1.00    8.00    --  112.00-111.00 -90.00   37
 16  ω     60.00 178.00   1.00    8.00    --  112.00  15.00  60.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1497051000
_diffrn_orient_matrix_UB_12      0.0250949000
_diffrn_orient_matrix_UB_13      -0.0234399000
_diffrn_orient_matrix_UB_21      -0.0751209000
_diffrn_orient_matrix_UB_22      0.0258400000
_diffrn_orient_matrix_UB_23      -0.0705738000
_diffrn_orient_matrix_UB_31      0.0230132000
_diffrn_orient_matrix_UB_32      0.1302635000
_diffrn_orient_matrix_UB_33      0.0446568000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12783
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.989
_diffrn_reflns_theta_min         3.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.409
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       prism
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0477P)²+3.4615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7009
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_nd_otf_h2o_acet_evac_ii_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        1991.69(9)
_cod_database_code               7232379
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C33 H30 N3 O12 S1 F3 Nd1'
_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   0.637
_shelx_estimated_absorpt_t_min   0.259
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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,H) groups
2. Shared sites
{O1WB, O51A}
{O2WB, O50A}
3. Restrained distances
 H4WA-Br2B
 2.55 with sigma of 0.04
 H4WB-Br1B
 2.55 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(O41A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1WB) = Uanis(O51A)
Uanis(O2WB) = Uanis(O50A)
5. Others
 Sof(S40A)=Sof(F45A)=Sof(F47A)=Sof(F46A)=Sof(C44A)=Sof(Br1B)=Sof(O42A)=
 Sof(O41A)=Sof(H1WA)=Sof(H1WB)=Sof(O2WB)=Sof(H2WA)=Sof(H2WB)=Sof(O43A)=
 Sof(O1WB)=1-FVAR(1)
 Sof(Br2B)=Sof(S48A)=Sof(O49A)=Sof(F54A)=Sof(F53A)=Sof(F55A)=Sof(C52A)=
 Sof(O3WA)=Sof(H3WA)=Sof(H3WB)=Sof(O51A)=Sof(O4WB)=Sof(H4WA)=Sof(H4WB)=
 Sof(O50A)=FVAR(1)
6.a Free rotating group:
 O3WA(H3WA,H3WB), O4WB(H4WA,H4WB)
6.b Rotating group:
 O51A(H1WA,H1WB), O2WB(H2WA,H2WB)
6.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
6.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C35(H35), C32(H32), C33(H33), C22(H22), C25(H25), C23(H23),
 C36(H36), C13(H13), C16(H16), C12(H12), C15(H15)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_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 3.216
_oxdiff_exptl_absorpt_empirical_full_min 0.806
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
Nd1 Nd 0.23859(2) 0.51295(2) 0.50295(2) 0.02854(9) Uani 1 1 d . . . . .
Br3 Br 0.08760(5) 0.65925(4) 0.89392(3) 0.03173(12) Uani 1 1 d . . . . .
Br2B Br 0.50386(9) 1.32536(7) 0.83888(5) 0.0368(3) Uani 0.5743(17) 1 d D . P A
2
O18 O 0.1294(3) 0.4081(3) 0.58409(17) 0.0347(7) Uani 1 1 d . . . . .
N21 N 0.0459(4) -0.1060(3) 0.82843(18) 0.0213(6) Uani 1 1 d . . . . .
C6 C 0.2124(5) 0.3252(3) 0.9713(2) 0.0223(8) Uani 1 1 d . . . . .
C1 C 0.0747(4) 0.2777(3) 0.9251(2) 0.0215(7) Uani 1 1 d . . . . .
C5 C 0.2908(4) 0.2509(3) 0.99817(19) 0.0211(8) Uani 1 1 d . . . . .
N31 N 0.4385(4) 0.3485(3) 1.12973(17) 0.0192(6) Uani 1 1 d . . . . .
C4 C 0.2341(4) 0.1296(3) 0.9792(2) 0.0204(7) Uani 1 1 d . . . . .
C3 C 0.0970(4) 0.0836(3) 0.9310(2) 0.0204(7) Uani 1 1 d . . . . .
N11 N -0.0133(4) 0.3474(3) 0.81609(19) 0.0256(7) Uani 1 1 d . . . . .
C26 C -0.0735(5) -0.1699(4) 0.7784(2) 0.0274(8) Uani 1 1 d . . . . .
H26 H -0.167776 -0.167758 0.790663 0.033 Uiso 1 1 calc R . . . .
C2 C 0.0172(4) 0.1570(3) 0.9039(2) 0.0211(7) Uani 1 1 d . . . . .
C14 C -0.0028(5) 0.3574(4) 0.6727(2) 0.0280(9) Uani 1 1 d . . . . .
C35 C 0.5692(5) 0.4142(4) 1.2553(2) 0.0288(9) Uani 1 1 d . . . . .
H35 H 0.658641 0.429740 1.290190 0.035 Uiso 1 1 calc R . . . .
C24 C 0.0769(5) -0.2426(4) 0.6933(2) 0.0245(8) Uani 1 1 d . . . . .
C32 C 0.3138(4) 0.3687(3) 1.1528(2) 0.0211(7) Uani 1 1 d . . . . .
H32 H 0.225786 0.353036 1.116863 0.025 Uiso 1 1 calc R . . . .
C20 C 0.0310(5) -0.0473(3) 0.9068(2) 0.0240(8) Uani 1 1 d . . . . .
H20A H 0.080519 -0.084085 0.941865 0.029 Uiso 1 1 calc R . . . .
H20B H -0.074303 -0.059386 0.909988 0.029 Uiso 1 1 calc R . . . .
C33 C 0.3130(4) 0.4118(3) 1.2283(2) 0.0214(7) Uani 1 1 d . . . . .
H33 H 0.224758 0.426530 1.244335 0.026 Uiso 1 1 calc R . . . .
C22 C 0.1799(5) -0.1037(4) 0.8122(2) 0.0265(8) Uani 1 1 d . . . . .
H22 H 0.262888 -0.054695 0.847896 0.032 Uiso 1 1 calc R . . . .
C25 C -0.0615(5) -0.2390(4) 0.7092(2) 0.0286(9) Uani 1 1 d . . . . .
H25 H -0.146637 -0.283227 0.673135 0.034 Uiso 1 1 calc R . . . .
C23 C 0.1989(5) -0.1718(4) 0.7443(2) 0.0284(9) Uani 1 1 d . . . . .
H23 H 0.294200 -0.170039 0.732723 0.034 Uiso 1 1 calc R . . . .
C36 C 0.5659(4) 0.3723(3) 1.1797(2) 0.0232(8) Uani 1 1 d . . . . .
H36 H 0.653568 0.359953 1.162186 0.028 Uiso 1 1 calc R . . . .
C7 C 0.2780(6) 0.4549(4) 0.9915(3) 0.0403(11) Uani 1 1 d . . . . .
H7A H 0.273035 0.479648 0.945583 0.060 Uiso 1 1 calc GR . . . .
H7B H 0.380719 0.470233 1.016811 0.060 Uiso 1 1 calc GR . . . .
H7C H 0.222875 0.498970 1.025268 0.060 Uiso 1 1 calc GR . . . .
C13 C -0.1337(5) 0.3541(4) 0.6985(3) 0.0334(10) Uani 1 1 d . . . . .
H13 H -0.221089 0.354348 0.666397 0.040 Uiso 1 1 calc R . . . .
C30 C 0.4421(4) 0.3018(4) 1.0473(2) 0.0259(8) Uani 1 1 d . . . . .
H30A H 0.500767 0.240265 1.040832 0.031 Uiso 1 1 calc R . . . .
H30B H 0.491808 0.366175 1.030087 0.031 Uiso 1 1 calc R . . . .
C10 C -0.0148(5) 0.3559(4) 0.8972(2) 0.0272(8) Uani 1 1 d . . . . .
H10A H -0.117328 0.333706 0.903404 0.033 Uiso 1 1 calc R . . . .
H10B H 0.024791 0.438192 0.928152 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1142(5) 0.3455(4) 0.7907(2) 0.0287(9) Uani 1 1 d . . . . .
H16 H 0.198949 0.340333 0.822758 0.034 Uiso 1 1 calc R . . . .
C17 C 0.0044(5) 0.3767(4) 0.5955(2) 0.0309(9) Uani 1 1 d . . . . .
C9 C 0.3235(5) 0.0533(4) 1.0101(2) 0.0328(9) Uani 1 1 d . . . . .
H9A H 0.410456 0.049828 0.987056 0.049 Uiso 1 1 calc GR . . . .
H9B H 0.263728 -0.025977 0.998515 0.049 Uiso 1 1 calc GR . . . .
H9C H 0.354084 0.086718 1.064813 0.049 Uiso 1 1 calc GR . . . .
C34 C 0.4412(4) 0.4338(4) 1.2808(2) 0.0257(8) Uani 1 1 d . . . . .
C8 C -0.1285(5) 0.1076(4) 0.8510(3) 0.0373(11) Uani 1 1 d . . . . .
H8A H -0.190722 0.165553 0.858918 0.056 Uiso 1 1 calc GR . . . .
H8B H -0.176368 0.036089 0.860774 0.056 Uiso 1 1 calc GR . . . .
H8C H -0.113256 0.089054 0.798918 0.056 Uiso 1 1 calc GR . . . .
C12 C -0.1363(5) 0.3504(4) 0.7714(3) 0.0311(9) Uani 1 1 d . . . . .
H12 H -0.225262 0.349985 0.789882 0.037 Uiso 1 1 calc R . . . .
C15 C 0.1223(5) 0.3511(4) 0.7188(2) 0.0298(9) Uani 1 1 d . . . . .
H15 H 0.212060 0.350681 0.701179 0.036 Uiso 1 1 calc R . . . .
O38 O 0.3163(4) 0.4864(4) 1.38113(16) 0.0414(9) Uani 1 1 d . . . . .
O28 O 0.2244(3) -0.3332(3) 0.61388(16) 0.0354(7) Uani 1 1 d . . . . .
C27 C 0.0956(5) -0.3287(4) 0.6225(2) 0.0275(9) Uani 1 1 d . . . . .
O39 O 0.5537(4) 0.4872(4) 1.40923(17) 0.0517(11) Uani 1 1 d . . . . .
C37 C 0.4374(5) 0.4731(5) 1.3642(2) 0.0361(11) Uani 1 1 d . . . . .
O29 O -0.0176(3) -0.3939(3) 0.57794(15) 0.0327(7) Uani 1 1 d . . . . .
O19 O -0.1168(3) 0.3617(3) 0.55311(17) 0.0352(7) Uani 1 1 d . . . . .
S48A S 0.4178(2) 0.26255(16) 0.44108(10) 0.0292(4) Uani 0.5743(17) 1 d . . P A
1
O49A O 0.4084(7) 0.2239(6) 0.3619(3) 0.0479(16) Uani 0.5743(17) 1 d . . P A 1
F54A F 0.3831(11) 0.1501(8) 0.5393(4) 0.089(3) Uani 0.5743(17) 1 d . . P A 1
F53A F 0.4773(12) 0.0642(8) 0.4487(6) 0.105(3) Uani 0.5743(17) 1 d . . P A 1
F55A F 0.2410(11) 0.0668(7) 0.4300(6) 0.103(3) Uani 0.5743(17) 1 d . . P A 1
C52A C 0.3772(15) 0.1295(10) 0.4675(7) 0.064(3) Uani 0.5743(17) 1 d . . P A 1
S40A S 0.5131(3) -0.1972(3) 0.17126(15) 0.0372(6) Uani 0.4257(17) 1 d . . P A 1
F45A F 0.3969(10) -0.1190(8) 0.2902(5) 0.067(3) Uani 0.4257(17) 1 d . . P A 1
F47A F 0.5182(13) -0.2476(11) 0.2982(5) 0.082(3) Uani 0.4257(17) 1 d . . P A 1
F46A F 0.6239(13) -0.0692(13) 0.3116(5) 0.103(4) Uani 0.4257(17) 1 d . . P A 1
C44A C 0.5139(17) -0.1488(16) 0.2747(7) 0.065(5) Uani 0.4257(17) 1 d . . P A 1
Br1B Br 0.58789(18) 0.87044(16) 0.70357(12) 0.0733(6) Uani 0.4257(17) 1 d D . P
A 2
O3WA O 0.4147(6) 0.1334(5) 0.2062(3) 0.0344(12) Uani 0.5743(17) 1 d . . P A 1
H3WA H 0.445691 0.068333 0.193192 0.052 Uiso 0.5743(17) 1 d G . P A 1
H3WB H 0.431381 0.153708 0.255160 0.052 Uiso 0.5743(17) 1 d G . P A 1
O42A O 0.3797(11) -0.2875(7) 0.1415(5) 0.045(2) Uani 0.4257(17) 1 d . . P A 1
O41A O 0.6480(13) -0.2311(14) 0.1668(7) 0.088(4) Uani 0.4257(17) 1 d . U P A 1
O51A O 0.2939(4) 0.3125(4) 0.4641(2) 0.0482(9) Uani 0.5743(17) 1 d . . P A 1
H1WA H 0.210962 0.256761 0.462457 0.072 Uiso 0.4257(17) 1 d GR . P A 2
H1WB H 0.365961 0.292166 0.495530 0.072 Uiso 0.4257(17) 1 d GR . P A 2
O2WB O 0.4318(4) 0.6939(5) 0.5179(2) 0.0604(12) Uani 0.4257(17) 1 d . . P A 2
H2WA H 0.404072 0.746260 0.483692 0.091 Uiso 0.4257(17) 1 d GR . P A 2
H2WB H 0.448013 0.757629 0.569492 0.091 Uiso 0.4257(17) 1 d GR . P A 2
O4WB O 0.4907(16) 1.0529(11) 0.8584(8) 0.052(3) Uani 0.5743(17) 1 d . . P A 2
H4WA H 0.466495 1.115201 0.849347 0.078 Uiso 0.5743(17) 1 d DG . P A 2
H4WB H 0.510688 1.014128 0.816207 0.078 Uiso 0.5743(17) 1 d DG . P A 2
O43A O 0.502(2) -0.0918(14) 0.1518(10) 0.048(4) Uani 0.4257(17) 1 d . . P A 1
O50A O 0.4318(4) 0.6939(5) 0.5179(2) 0.0604(12) Uani 0.5743(17) 1 d . . P A 1
O1WB O 0.2939(4) 0.3125(4) 0.4641(2) 0.0482(9) Uani 0.4257(17) 1 d . . P A 2
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'
F F 0.0727 0.0534 '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'
Nd Nd -3.1807 10.9079 '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'
S S 0.3331 0.5567 '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
-6 0 6 0.0183
6 0 -6 0.0183
-2 0 -10 0.0521
2 0 10 0.0521
1 -7 -2 0.0380
-1 7 2 0.0380
1 7 -1 0.0368
-4 0 10 0.0223
3 -7 6 0.0661
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
O18 Nd1 O38 143.63(13) . 1_554
O18 Nd1 O51A 74.63(13) . .
O18 Nd1 O2WB 137.80(12) . .
O18 Nd1 O50A 137.80(12) . .
O18 Nd1 O1WB 74.63(13) . .
O38 Nd1 O51A 72.17(13) 1_554 .
O38 Nd1 O2WB 74.08(13) 1_554 .
O38 Nd1 O50A 74.08(13) 1_554 .
O38 Nd1 O1WB 72.17(13) 1_554 .
O28 Nd1 O18 75.32(12) 1_565 .
O28 Nd1 O38 141.04(13) 1_565 1_554
O28 Nd1 O51A 141.85(12) 1_565 .
O28 Nd1 O2WB 70.59(13) 1_565 .
O28 Nd1 O50A 70.59(13) 1_565 .
O28 Nd1 O1WB 141.85(12) 1_565 .
O39 Nd1 O18 77.38(13) 2_667 .
O39 Nd1 O38 106.27(11) 2_667 1_554
O39 Nd1 O28 77.79(12) 2_667 1_565
O39 Nd1 O29 144.12(15) 2_667 2_556
O39 Nd1 O19 143.09(15) 2_667 2_566
O39 Nd1 O51A 73.16(13) 2_667 .
O39 Nd1 O2WB 71.79(15) 2_667 .
O39 Nd1 O50A 71.79(15) 2_667 .
O39 Nd1 O1WB 73.16(13) 2_667 .
O29 Nd1 O18 77.44(11) 2_556 .
O29 Nd1 O38 80.43(11) 2_556 1_554
O29 Nd1 O28 119.36(10) 2_556 1_565
O29 Nd1 O19 72.71(12) 2_556 2_566
O29 Nd1 O51A 75.80(11) 2_556 .
O29 Nd1 O2WB 141.73(12) 2_556 .
O29 Nd1 O50A 141.73(12) 2_556 .
O29 Nd1 O1WB 75.80(11) 2_556 .
O19 Nd1 O18 122.68(11) 2_566 .
O19 Nd1 O38 76.38(11) 2_566 1_554
O19 Nd1 O28 78.49(11) 2_566 1_565
O19 Nd1 O51A 138.42(11) 2_566 .
O19 Nd1 O2WB 73.85(13) 2_566 .
O19 Nd1 O50A 73.85(13) 2_566 .
O19 Nd1 O1WB 138.42(11) 2_566 .
O51A Nd1 O50A 120.93(15) . .
O1WB Nd1 O2WB 120.93(15) . .
C17 O18 Nd1 136.6(3) . .
C26 N21 C20 119.2(3) . .
C26 N21 C22 121.3(3) . .
C22 N21 C20 119.1(3) . .
C1 C6 C5 119.1(3) . .
C1 C6 C7 120.8(4) . .
C5 C6 C7 120.0(4) . .
C6 C1 C2 120.7(4) . .
C6 C1 C10 120.4(4) . .
C2 C1 C10 118.9(4) . .
C6 C5 C4 121.4(4) . .
C6 C5 C30 119.3(4) . .
C4 C5 C30 119.3(4) . .
C32 N31 C36 121.0(3) . .
C32 N31 C30 121.3(3) . .
C36 N31 C30 117.8(3) . .
C5 C4 C9 119.2(4) . .
C3 C4 C5 118.4(3) . .
C3 C4 C9 122.4(4) . .
C4 C3 C20 121.0(3) . .
C2 C3 C4 120.8(3) . .
C2 C3 C20 118.2(4) . .
C16 N11 C10 119.4(4) . .
C12 N11 C10 119.2(4) . .
C12 N11 C16 121.2(4) . .
N21 C26 H26 119.7 . .
N21 C26 C25 120.7(4) . .
C25 C26 H26 119.7 . .
C1 C2 C3 119.6(4) . .
C1 C2 C8 119.5(4) . .
C3 C2 C8 120.9(4) . .
C13 C14 C17 119.5(4) . .
C13 C14 C15 119.7(4) . .
C15 C14 C17 120.7(4) . .
C36 C35 H35 120.1 . .
C36 C35 C34 119.8(4) . .
C34 C35 H35 120.1 . .
C25 C24 C27 120.2(4) . .
C23 C24 C25 119.8(4) . .
C23 C24 C27 119.9(4) . .
N31 C32 H32 119.8 . .
N31 C32 C33 120.4(3) . .
C33 C32 H32 119.8 . .
N21 C20 C3 112.1(3) . .
N21 C20 H20A 109.2 . .
N21 C20 H20B 109.2 . .
C3 C20 H20A 109.2 . .
C3 C20 H20B 109.2 . .
H20A C20 H20B 107.9 . .
C32 C33 H33 120.1 . .
C32 C33 C34 119.8(4) . .
C34 C33 H33 120.1 . .
N21 C22 H22 119.7 . .
N21 C22 C23 120.6(4) . .
C23 C22 H22 119.7 . .
C26 C25 C24 118.6(4) . .
C26 C25 H25 120.7 . .
C24 C25 H25 120.7 . .
C24 C23 H23 120.6 . .
C22 C23 C24 118.8(4) . .
C22 C23 H23 120.6 . .
N31 C36 C35 120.4(4) . .
N31 C36 H36 119.8 . .
C35 C36 H36 119.8 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C14 C13 H13 120.2 . .
C12 C13 C14 119.5(4) . .
C12 C13 H13 120.2 . .
C5 C30 H30A 108.9 . .
C5 C30 H30B 108.9 . .
N31 C30 C5 113.3(3) . .
N31 C30 H30A 108.9 . .
N31 C30 H30B 108.9 . .
H30A C30 H30B 107.7 . .
C1 C10 H10A 109.2 . .
C1 C10 H10B 109.2 . .
N11 C10 C1 112.2(3) . .
N11 C10 H10A 109.2 . .
N11 C10 H10B 109.2 . .
H10A C10 H10B 107.9 . .
N11 C16 H16 119.7 . .
N11 C16 C15 120.6(4) . .
C15 C16 H16 119.7 . .
O18 C17 C14 115.7(4) . .
O18 C17 O19 128.7(4) . .
O19 C17 C14 115.6(4) . .
C4 C9 H9A 109.5 . .
C4 C9 H9B 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C35 C34 C37 121.7(4) . .
C33 C34 C35 118.6(4) . .
C33 C34 C37 119.6(4) . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N11 C12 C13 120.1(4) . .
N11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C14 C15 H15 120.6 . .
C16 C15 C14 118.9(4) . .
C16 C15 H15 120.6 . .
C37 O38 Nd1 129.9(3) . 1_556
C27 O28 Nd1 113.5(3) . 1_545
O28 C27 C24 117.0(4) . .
O28 C27 O29 124.5(4) . .
O29 C27 C24 118.4(4) . .
C37 O39 Nd1 171.6(4) . 2_667
O38 C37 C34 116.6(4) . .
O39 C37 C34 117.4(4) . .
O39 C37 O38 126.0(4) . .
C27 O29 Nd1 177.4(3) . 2_556
C17 O19 Nd1 133.9(3) . 2_566
O49A S48A C52A 104.4(5) . .
O49A S48A O51A 114.2(3) . .
O49A S48A O50A 112.6(3) . 2_666
O51A S48A C52A 98.2(5) . .
O50A S48A C52A 98.8(5) 2_666 .
O50A S48A O51A 123.7(3) 2_666 .
F54A C52A S48A 112.1(8) . .
F54A C52A F53A 107.4(10) . .
F54A C52A F55A 109.4(12) . .
F53A C52A S48A 109.3(10) . .
F53A C52A F55A 108.9(11) . .
F55A C52A S48A 109.7(8) . .
O42A S40A C44A 103.4(6) . .
O41A S40A C44A 104.1(8) . .
O41A S40A O42A 118.0(8) . .
O41A S40A O43A 114.8(10) . .
O43A S40A C44A 101.1(10) . .
O43A S40A O42A 112.7(9) . .
F45A C44A S40A 113.5(10) . .
F45A C44A F47A 105.0(11) . .
F45A C44A F46A 110.3(17) . .
F47A C44A S40A 105.2(12) . .
F46A C44A S40A 113.3(10) . .
F46A C44A F47A 109.0(13) . .
H3WA O3WA H3WB 104.5 . .
S48A O51A Nd1 136.6(3) . .
Nd1 O2WB H2WA 115.2 . .
Nd1 O2WB H2WB 114.4 . .
H2WA O2WB H2WB 97.3 . .
H4WA O4WB H4WB 104.5 . .
S48A O50A Nd1 133.8(3) 2_666 .
Nd1 O1WB H1WA 109.1 . .
Nd1 O1WB H1WB 119.5 . .
H1WA O1WB H1WB 101.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nd1 O18 2.447(3) .
Nd1 O38 2.453(3) 1_554
Nd1 O28 2.437(3) 1_565
Nd1 O39 2.374(3) 2_667
Nd1 O29 2.385(3) 2_556
Nd1 O19 2.402(3) 2_566
Nd1 O51A 2.503(4) .
Nd1 O2WB 2.528(4) .
Nd1 O50A 2.528(4) .
Nd1 O1WB 2.503(4) .
O18 C17 1.241(6) .
N21 C26 1.334(5) .
N21 C20 1.493(5) .
N21 C22 1.336(5) .
C6 C1 1.393(6) .
C6 C5 1.398(6) .
C6 C7 1.512(5) .
C1 C2 1.398(5) .
C1 C10 1.507(5) .
C5 C4 1.406(6) .
C5 C30 1.517(5) .
N31 C32 1.344(5) .
N31 C36 1.352(5) .
N31 C30 1.508(5) .
C4 C3 1.402(6) .
C4 C9 1.513(6) .
C3 C2 1.399(5) .
C3 C20 1.522(5) .
N11 C10 1.499(5) .
N11 C16 1.353(6) .
N11 C12 1.342(6) .
C26 H26 0.9500 .
C26 C25 1.380(6) .
C2 C8 1.503(6) .
C14 C13 1.384(7) .
C14 C17 1.533(6) .
C14 C15 1.385(6) .
C35 H35 0.9500 .
C35 C36 1.369(6) .
C35 C34 1.390(6) .
C24 C25 1.382(6) .
C24 C23 1.381(6) .
C24 C27 1.510(5) .
C32 H32 0.9500 .
C32 C33 1.375(5) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C33 H33 0.9500 .
C33 C34 1.386(5) .
C22 H22 0.9500 .
C22 C23 1.377(6) .
C25 H25 0.9500 .
C23 H23 0.9500 .
C36 H36 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C13 H13 0.9500 .
C13 C12 1.382(6) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C16 H16 0.9500 .
C16 C15 1.380(6) .
C17 O19 1.253(5) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C34 C37 1.518(5) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C12 H12 0.9500 .
C15 H15 0.9500 .
O38 C37 1.250(5) .
O28 C27 1.254(5) .
C27 O29 1.258(5) .
O39 C37 1.243(5) .
S48A O49A 1.420(6) .
S48A C52A 1.799(12) .
S48A O51A 1.465(4) .
S48A O50A 1.454(4) 2_666
F54A C52A 1.296(15) .
F53A C52A 1.351(16) .
F55A C52A 1.364(15) .
S40A C44A 1.873(14) .
S40A O42A 1.453(10) .
S40A O41A 1.403(10) .
S40A O43A 1.428(14) .
F45A C44A 1.26(2) .
F47A C44A 1.38(2) .
F46A C44A 1.265(17) .
O3WA H3WA 0.8708 .
O3WA H3WB 0.8705 .
O2WB H2WA 1.0477 .
O2WB H2WB 1.0407 .
O4WB H4WA 0.8706 .
O4WB H4WB 0.8702 .
O1WB H1WA 0.9347 .
O1WB H1WB 0.9414 .
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_4
Nd1 O18 C17 C14 -156.1(3) . .
Nd1 O18 C17 O19 21.8(8) . .
Nd1 O38 C37 C34 167.7(3) 1_556 .
Nd1 O38 C37 O39 -11.1(9) 1_556 .
Nd1 O28 C27 C24 175.1(3) 1_545 .
Nd1 O28 C27 O29 -2.0(6) 1_545 .
O18 C17 O19 Nd1 -59.7(7) . 2_566
N21 C26 C25 C24 1.4(7) . .
N21 C22 C23 C24 -0.1(7) . .
C6 C1 C2 C3 1.8(6) . .
C6 C1 C2 C8 -177.1(4) . .
C6 C1 C10 N11 104.4(4) . .
C6 C5 C4 C3 1.3(5) . .
C6 C5 C4 C9 -179.7(4) . .
C6 C5 C30 N31 86.4(4) . .
C1 C6 C5 C4 0.3(6) . .
C1 C6 C5 C30 178.8(3) . .
C5 C6 C1 C2 -1.9(6) . .
C5 C6 C1 C10 178.1(3) . .
C5 C4 C3 C2 -1.4(5) . .
C5 C4 C3 C20 178.6(3) . .
N31 C32 C33 C34 -0.5(6) . .
C4 C5 C30 N31 -95.1(4) . .
C4 C3 C2 C1 -0.1(6) . .
C4 C3 C2 C8 178.8(4) . .
C4 C3 C20 N21 -102.8(4) . .
N11 C16 C15 C14 -0.7(7) . .
C26 N21 C20 C3 -126.2(4) . .
C26 N21 C22 C23 -2.9(6) . .
C2 C1 C10 N11 -75.6(5) . .
C2 C3 C20 N21 77.2(4) . .
C14 C13 C12 N11 -1.5(7) . .
C14 C17 O19 Nd1 118.2(4) . 2_566
C35 C34 C37 O38 -178.9(5) . .
C35 C34 C37 O39 0.0(8) . .
C32 N31 C36 C35 2.1(6) . .
C32 N31 C30 C5 -15.6(5) . .
C32 C33 C34 C35 1.6(6) . .
C32 C33 C34 C37 -175.6(4) . .
C20 N21 C26 C25 -170.4(4) . .
C20 N21 C22 C23 169.8(4) . .
C20 C3 C2 C1 179.9(3) . .
C20 C3 C2 C8 -1.2(6) . .
C33 C34 C37 O38 -1.7(7) . .
C33 C34 C37 O39 177.2(5) . .
C22 N21 C26 C25 2.3(6) . .
C22 N21 C20 C3 61.0(5) . .
C25 C24 C23 C22 3.8(6) . .
C25 C24 C27 O28 -175.3(4) . .
C25 C24 C27 O29 2.0(6) . .
C23 C24 C25 C26 -4.4(6) . .
C23 C24 C27 O28 1.2(6) . .
C23 C24 C27 O29 178.4(4) . .
C36 N31 C32 C33 -1.4(6) . .
C36 N31 C30 C5 166.1(3) . .
C36 C35 C34 C33 -1.0(7) . .
C36 C35 C34 C37 176.2(4) . .
C7 C6 C1 C2 177.1(4) . .
C7 C6 C1 C10 -2.9(6) . .
C7 C6 C5 C4 -178.7(4) . .
C7 C6 C5 C30 -0.2(6) . .
C13 C14 C17 O18 162.4(4) . .
C13 C14 C17 O19 -15.8(6) . .
C13 C14 C15 C16 -2.1(7) . .
C30 C5 C4 C3 -177.2(3) . .
C30 C5 C4 C9 1.8(5) . .
C30 N31 C32 C33 -179.7(4) . .
C30 N31 C36 C35 -179.6(4) . .
C10 C1 C2 C3 -178.2(3) . .
C10 C1 C2 C8 2.9(6) . .
C10 N11 C16 C15 -172.7(4) . .
C10 N11 C12 C13 173.8(4) . .
C16 N11 C10 C1 -42.8(5) . .
C16 N11 C12 C13 -1.4(6) . .
C17 C14 C13 C12 -172.5(4) . .
C17 C14 C15 C16 173.5(4) . .
C9 C4 C3 C2 179.6(4) . .
C9 C4 C3 C20 -0.4(6) . .
C34 C35 C36 N31 -0.9(7) . .
C12 N11 C10 C1 141.9(4) . .
C12 N11 C16 C15 2.5(6) . .
C15 C14 C13 C12 3.2(7) . .
C15 C14 C17 O18 -13.2(6) . .
C15 C14 C17 O19 168.6(4) . .
C27 C24 C25 C26 172.1(4) . .
C27 C24 C23 C22 -172.7(4) . .
O49A S48A C52A F54A 179.2(9) . .
O49A S48A C52A F53A 60.2(9) . .
O49A S48A C52A F55A -59.1(11) . .
O49A S48A O51A Nd1 -94.9(4) . .
C52A S48A O51A Nd1 155.2(5) . .
O42A S40A C44A F45A -53.5(13) . .
O42A S40A C44A F47A 60.8(11) . .
O42A S40A C44A F46A 179.7(14) . .
O41A S40A C44A F45A -177.3(13) . .
O41A S40A C44A F47A -63.0(12) . .
O41A S40A C44A F46A 55.9(17) . .
O51A S48A C52A F54A -63.1(10) . .
O51A S48A C52A F53A 177.9(8) . .
O51A S48A C52A F55A 58.6(10) . .
O43A S40A C44A F45A 63.3(14) . .
O43A S40A C44A F47A 177.6(12) . .
O43A S40A C44A F46A -63.5(18) . .
O50A S48A C52A F54A 63.0(10) 2_666 .
O50A S48A C52A F53A -56.0(9) 2_666 .
O50A S48A C52A F55A -175.3(9) 2_666 .
O50A S48A O51A Nd1 48.8(5) 2_666 .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0000 -0.0000 6.0000 -1.0389 0.0273 0.1299
6.0000 0.0000 -6.0000 1.0389 -0.0273 -0.1299
-2.0000 -0.0000 -10.0000 -0.0650 0.8560 -0.4926
2.0000 0.0000 10.0000 0.0650 -0.8560 0.4926
1.0000 -7.0000 -2.0000 0.0209 -0.1149 -0.9781
-1.0000 7.0000 2.0000 -0.0209 0.1149 0.9781
1.0000 7.0000 -1.0000 0.3488 0.1763 0.8902
-4.0000 -0.0000 10.0000 -0.8332 -0.4053 0.3545
3.0000 -7.0000 6.0000 0.1328 -0.8297 -0.5749
