#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:53:39 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/23/7232373.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_7232373
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 H31 N3 O8 Tb, 2(Br), C F3 O3 S'
_chemical_formula_sum            'C31 H49 Br2 F3 N3 O20 S Tb'
_chemical_formula_weight         1191.53
_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             2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-29 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                108.079(4)
_cell_angle_beta                 103.298(3)
_cell_angle_gamma                99.250(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5114(4)
_cell_length_b                   14.2612(6)
_cell_length_c                   18.8972(6)
_cell_measurement_reflns_used    7780
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.3710
_cell_measurement_theta_min      3.3660
_cell_volume                     2295.55(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  26.00   1.00    3.00    --  -41.90  69.00 -80.00   99
  2  ω      1.00  83.00   1.00    3.00    --   41.90 -99.00  30.00   82
  3  ω     44.00 140.00   1.00    6.00    --  112.00 -30.00  90.00   96
  4  ω     53.00 116.00   1.00    6.00    --  112.00-111.00  60.00   63
  5  ω     51.00 140.00   1.00    6.00    --  112.00 -30.00 -60.00   89
  6  ω     87.00 115.00   1.00    6.00    --  112.00-111.00-150.00   28
  7  ω     46.00 140.00   1.00    6.00    --  112.00 -30.00-150.00   94
  8  ω    100.00 155.00   1.00    6.00    --  112.00 111.00-120.00   55
  9  ω    101.00 132.00   1.00    6.00    --  112.00 111.00 -90.00   31
 10  ω    106.00 140.00   1.00    6.00    --  112.00 111.00  30.00   34
 11  ω     38.00 140.00   1.00    6.00    --  112.00 -77.00  90.00  102
 12  ω     36.00 135.00   1.00    6.00    --  112.00 -77.00-120.00   99
 13  ω   -115.00 -31.00   1.00    3.00    --  -41.90 -57.00 150.00   84
 14  ω   -115.00 -18.00   1.00    3.00    --  -41.90 -37.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616006000
_diffrn_orient_matrix_UB_12      -0.0357110000
_diffrn_orient_matrix_UB_13      0.0584456000
_diffrn_orient_matrix_UB_21      0.1549335000
_diffrn_orient_matrix_UB_22      -0.0116432000
_diffrn_orient_matrix_UB_23      0.0375438000
_diffrn_orient_matrix_UB_31      0.0419721000
_diffrn_orient_matrix_UB_32      0.1112195000
_diffrn_orient_matrix_UB_33      0.0569855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13793
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.995
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.819
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.048
_refine_diff_density_max         3.157
_refine_diff_density_min         -2.302
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8301
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0688
_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)+(0.0836P)²+32.1568P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7799
_reflns_number_total             8301
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_tb_otf_h2o_acet_red3
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2295.55(17)
_cod_database_code               7232373
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Tb1'
_chemical_oxdiff_usercomment     'clear colorless block'
_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.
;
_reflns_odcompleteness_completeness 99.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(N11) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(Br2A)=FVAR(1)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C15(H15), C16(H16), C13(H13), C35(H35), C32(H32), C26(H26),
 C23(H23), C33(H33), C22(H22), C12(H12), C36(H36)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.662
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
Tb1 Tb 0.23112(4) 1.01383(3) 0.49505(2) 0.01625(15) Uani 1 1 d . . . . .
Br1 Br 0.73788(14) 0.91405(11) -0.18594(7) 0.0592(3) Uani 1 1 d . . . . .
Br2A Br 0.78086(17) 1.41619(15) 0.79152(10) 0.0563(6) Uani 0.734(4) 1 d . . P A
2
S40 S -0.3024(2) 0.73611(17) 0.09799(12) 0.0292(4) Uani 1 1 d . . . B 1
O18 O 0.3715(5) 0.9593(4) 0.4122(3) 0.0213(11) Uani 1 1 d . . . . .
O43 O -0.1921(8) 0.6896(6) 0.0760(5) 0.053(2) Uani 1 1 d . . . B 1
O42 O -0.4486(8) 0.6760(5) 0.0691(4) 0.0426(16) Uani 1 1 d . . . B 1
F47 F -0.1672(8) 0.9023(6) 0.0823(5) 0.077(2) Uani 1 1 d . . . B 1
C37 C 0.0304(8) 0.9462(6) -0.3817(4) 0.0210(15) Uani 1 1 d . . . . .
O41 O -0.2546(10) 0.8016(8) 0.1811(5) 0.071(3) Uani 1 1 d . . . B 1
F45 F -0.4045(8) 0.8857(5) 0.0711(5) 0.0677(19) Uani 1 1 d . . . B 1
C25 C 0.0744(8) 0.3300(6) -0.2798(4) 0.0214(15) Uani 1 1 d . . . . .
H25 H -0.031374 0.308007 -0.295502 0.026 Uiso 1 1 calc R . . . .
C17 C 0.4382(8) 0.9201(5) 0.3670(4) 0.0160(14) Uani 1 1 d . . . . .
C1 C 0.1954(9) 0.7279(6) -0.0164(4) 0.0251(17) Uani 1 1 d . . . . .
N21 N 0.2984(7) 0.4440(5) -0.1911(4) 0.0237(14) Uani 1 1 d . . . . .
C3 C 0.3140(9) 0.6194(5) -0.0969(4) 0.0213(15) Uani 1 1 d . . . . .
F46 F -0.3334(10) 0.7982(7) -0.0209(4) 0.083(3) Uani 1 1 d . . . B 1
C15 C 0.4232(9) 0.8367(6) 0.2255(4) 0.0234(16) Uani 1 1 d . . . . .
H15 H 0.526265 0.838561 0.241295 0.028 Uiso 1 1 calc R . . . .
C2 C 0.2336(9) 0.6352(6) -0.0422(4) 0.0262(17) Uani 1 1 d . . . . .
C34 C 0.1183(9) 0.9218(6) -0.3157(4) 0.0230(16) Uani 1 1 d . . . . .
N31 N 0.2829(8) 0.8847(5) -0.1933(4) 0.0267(15) Uani 1 1 d . . . . .
C20 C 0.3814(9) 0.5294(6) -0.1152(4) 0.0267(17) Uani 1 1 d . . . . .
H20A H 0.484585 0.553438 -0.115745 0.032 Uiso 1 1 calc R . . . .
H20B H 0.387486 0.502283 -0.072587 0.032 Uiso 1 1 calc R . . . .
C27 C 0.0790(8) 0.1818(5) -0.3957(4) 0.0199(15) Uani 1 1 d . . . . .
C16 C 0.3440(9) 0.7961(7) 0.1483(4) 0.0278(17) Uani 1 1 d . . . . .
H16 H 0.392065 0.769044 0.110589 0.033 Uiso 1 1 calc R . . . .
C13 C 0.2037(9) 0.8720(7) 0.2557(4) 0.0255(17) Uani 1 1 d . . . . .
H13 H 0.153132 0.897756 0.292495 0.031 Uiso 1 1 calc R . . . .
C35 C 0.2716(9) 0.9358(8) -0.3003(5) 0.036(2) Uani 1 1 d . . . . .
H35 H 0.320419 0.958363 -0.332806 0.043 Uiso 1 1 calc R . . . .
C24 C 0.1551(8) 0.2777(6) -0.3229(4) 0.0200(15) Uani 1 1 d . . . . .
C4 C 0.3489(8) 0.6947(6) -0.1283(4) 0.0224(16) Uani 1 1 d . . . . .
C5 C 0.3150(9) 0.7885(6) -0.0996(4) 0.0252(17) Uani 1 1 d . . . . .
C32 C 0.1368(10) 0.8671(8) -0.2080(5) 0.036(2) Uani 1 1 d . . . . .
H32 H 0.090423 0.841709 -0.175823 0.044 Uiso 1 1 calc R . . . .
C26 C 0.1486(9) 0.4138(6) -0.2142(4) 0.0236(16) Uani 1 1 d . . . . .
H26 H 0.093780 0.450931 -0.184695 0.028 Uiso 1 1 calc R . . . .
C14 C 0.3535(8) 0.8751(5) 0.2807(4) 0.0169(14) Uani 1 1 d . . . . .
C44 C -0.2999(11) 0.8415(10) 0.0641(10) 0.073(5) Uani 1 1 d . . . B 1
C23 C 0.3097(9) 0.3120(6) -0.2985(5) 0.0266(17) Uani 1 1 d . . . . .
H23 H 0.366712 0.278175 -0.328420 0.032 Uiso 1 1 calc R . . . .
C33 C 0.0507(9) 0.8850(8) -0.2692(5) 0.035(2) Uani 1 1 d . . . . .
H33 H -0.054503 0.872179 -0.279409 0.042 Uiso 1 1 calc R . . . .
C7 C 0.1934(12) 0.5542(7) -0.0091(6) 0.041(2) Uani 1 1 d . . . . .
H7A H 0.121054 0.571209 0.019180 0.062 Uiso 1 1 calc GR . . . .
H7B H 0.283508 0.550838 0.026702 0.062 Uiso 1 1 calc GR . . . .
H7C H 0.149624 0.487991 -0.051703 0.062 Uiso 1 1 calc GR . . . .
C22 C 0.3793(9) 0.3941(7) -0.2317(5) 0.0293(18) Uani 1 1 d . . . . .
H22 H 0.485200 0.416052 -0.213865 0.035 Uiso 1 1 calc R . . . .
C12 C 0.1281(9) 0.8313(7) 0.1770(4) 0.0288(18) Uani 1 1 d . . . . .
H12 H 0.025478 0.829799 0.159621 0.035 Uiso 1 1 calc R . . . .
C36 C 0.3522(10) 0.9175(7) -0.2387(5) 0.034(2) Uani 1 1 d . . . . .
H36 H 0.457331 0.927877 -0.227973 0.041 Uiso 1 1 calc R . . . .
C6 C 0.2390(10) 0.8071(7) -0.0430(4) 0.0299(18) Uani 1 1 d . . . . .
C8 C 0.4249(10) 0.6744(7) -0.1915(5) 0.0331(19) Uani 1 1 d . . . . .
H8A H 0.532729 0.688408 -0.167719 0.050 Uiso 1 1 calc GR . . . .
H8B H 0.404938 0.718749 -0.221191 0.050 Uiso 1 1 calc GR . . . .
H8C H 0.386283 0.602997 -0.226520 0.050 Uiso 1 1 calc GR . . . .
C30 C 0.3813(10) 0.8732(7) -0.1229(5) 0.034(2) Uani 1 1 d . . . . .
H30A H 0.475497 0.861656 -0.133616 0.041 Uiso 1 1 calc R . . . .
H30B H 0.406977 0.938222 -0.078142 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2034(14) 0.9075(8) -0.0118(6) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.094880 0.897754 -0.025250 0.074 Uiso 1 1 calc GR . . . .
H9B H 0.245358 0.954149 -0.034602 0.074 Uiso 1 1 calc GR . . . .
H9C H 0.246643 0.936408 0.045090 0.074 Uiso 1 1 calc GR . . . .
O28 O 0.1588(6) 0.1577(4) -0.4399(3) 0.0213(11) Uani 1 1 d . . . . .
O29 O -0.0516(5) 0.1391(4) -0.4046(3) 0.0201(11) Uani 1 1 d . . . . .
O39 O 0.0987(6) 0.9713(4) -0.4253(3) 0.0222(11) Uani 1 1 d . . . . .
O38 O -0.1063(6) 0.9412(4) -0.3894(3) 0.0214(11) Uani 1 1 d . . . . .
O19 O 0.5724(5) 0.9154(4) 0.3858(3) 0.0229(11) Uani 1 1 d . . . . .
Br2B Br 0.6528(6) 1.3510(4) 0.6375(3) 0.0632(16) Uani 0.266(4) 1 d . . P A 1
O1W O 0.3142(7) 0.8733(5) 0.5201(4) 0.0350(14) Uani 1 1 d . . . . .
H1WA H 0.239014 0.827549 0.517735 0.053 Uiso 1 1 d GR . . . .
H1WB H 0.377904 0.894249 0.566266 0.053 Uiso 1 1 d GR . . . .
O2W O 0.3959(7) 1.1636(4) 0.4913(3) 0.0292(12) Uani 1 1 d . . . . .
H2WA H 0.451605 1.202684 0.538321 0.044 Uiso 1 1 d GR . . . .
H2WB H 0.343652 1.199378 0.471466 0.044 Uiso 1 1 d GR . . . .
N11 N 0.1981(7) 0.7939(5) 0.1251(3) 0.0219(13) Uani 1 1 d . U . . .
C10 C 0.1058(9) 0.7465(7) 0.0411(4) 0.0294(18) Uani 1 1 d . U . . .
H10A H 0.041740 0.791427 0.029614 0.035 Uiso 1 1 calc R . . . .
H10B H 0.039426 0.680661 0.033014 0.035 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'
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'
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'
Tb Tb -9.1472 9.1891 '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
0 -8 10 0.0239
0 8 -10 0.0239
0 -4 -8 0.0353
0 4 8 0.0353
-6 1 5 0.0682
6 -1 -5 0.0413
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 Tb1 O28 142.36(19) . 1_566
O18 Tb1 O29 81.88(17) . 2_565
O18 Tb1 O39 145.4(2) . 1_556
O18 Tb1 O38 82.04(18) . 2_575
O18 Tb1 O19 98.18(17) . 2_676
O18 Tb1 O1W 72.5(2) . .
O18 Tb1 O2W 70.75(19) . .
O28 Tb1 O29 121.73(17) 1_566 2_565
O28 Tb1 O38 77.76(18) 1_566 2_575
O28 Tb1 O19 79.03(18) 1_566 2_676
O28 Tb1 O1W 138.92(19) 1_566 .
O28 Tb1 O2W 72.74(19) 1_566 .
O29 Tb1 O38 74.49(18) 2_565 2_575
O29 Tb1 O1W 72.9(2) 2_565 .
O29 Tb1 O2W 138.15(18) 2_565 .
O39 Tb1 O28 71.95(19) 1_556 1_566
O39 Tb1 O29 78.78(18) 1_556 2_565
O39 Tb1 O38 119.27(18) 1_556 2_575
O39 Tb1 O19 81.97(17) 1_556 2_676
O39 Tb1 O1W 74.5(2) 1_556 .
O39 Tb1 O2W 139.47(19) 1_556 .
O38 Tb1 O1W 140.8(2) 2_575 .
O38 Tb1 O2W 70.93(19) 2_575 .
O19 Tb1 O29 144.52(19) 2_676 2_565
O19 Tb1 O38 140.90(19) 2_676 2_575
O19 Tb1 O1W 73.4(2) 2_676 .
O19 Tb1 O2W 72.35(19) 2_676 .
O1W Tb1 O2W 124.4(2) . .
O43 S40 O41 112.7(6) . .
O43 S40 C44 106.9(6) . .
O42 S40 O43 117.1(5) . .
O42 S40 O41 115.5(5) . .
O42 S40 C44 107.3(5) . .
O41 S40 C44 94.2(7) . .
C17 O18 Tb1 173.3(5) . .
O39 C37 C34 117.6(7) . .
O39 C37 O38 124.4(7) . .
O38 C37 C34 118.1(7) . .
C24 C25 H25 120.4 . .
C26 C25 H25 120.4 . .
C26 C25 C24 119.2(7) . .
O18 C17 C14 117.5(6) . .
O18 C17 O19 125.8(6) . .
O19 C17 C14 116.7(6) . .
C2 C1 C6 121.1(7) . .
C2 C1 C10 120.8(7) . .
C6 C1 C10 118.0(8) . .
C26 N21 C20 120.9(7) . .
C22 N21 C20 117.5(7) . .
C22 N21 C26 121.4(7) . .
C2 C3 C20 121.1(7) . .
C2 C3 C4 120.1(7) . .
C4 C3 C20 118.4(7) . .
C16 C15 H15 120.0 . .
C16 C15 C14 119.9(7) . .
C14 C15 H15 120.0 . .
C1 C2 C3 119.5(7) . .
C1 C2 C7 120.0(8) . .
C3 C2 C7 120.5(8) . .
C35 C34 C37 120.1(7) . .
C33 C34 C37 121.7(7) . .
C33 C34 C35 118.1(7) . .
C32 N31 C36 121.5(7) . .
C32 N31 C30 121.9(7) . .
C36 N31 C30 116.6(7) . .
N21 C20 C3 115.2(6) . .
N21 C20 H20A 108.5 . .
N21 C20 H20B 108.5 . .
C3 C20 H20A 108.5 . .
C3 C20 H20B 108.5 . .
H20A C20 H20B 107.5 . .
O28 C27 C24 114.4(6) . .
O29 C27 C24 117.2(6) . .
O29 C27 O28 128.5(7) . .
C15 C16 H16 119.7 . .
N11 C16 C15 120.7(7) . .
N11 C16 H16 119.7 . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.2 . .
C12 C13 C14 119.6(7) . .
C34 C35 H35 119.9 . .
C36 C35 C34 120.3(8) . .
C36 C35 H35 119.9 . .
C25 C24 C27 121.7(7) . .
C25 C24 C23 119.0(7) . .
C23 C24 C27 119.3(7) . .
C3 C4 C8 120.0(7) . .
C5 C4 C3 119.6(7) . .
C5 C4 C8 120.5(7) . .
C4 C5 C6 121.1(7) . .
C4 C5 C30 117.4(8) . .
C6 C5 C30 120.9(8) . .
N31 C32 H32 119.6 . .
N31 C32 C33 120.8(8) . .
C33 C32 H32 119.6 . .
C25 C26 H26 119.7 . .
N21 C26 C25 120.5(7) . .
N21 C26 H26 119.7 . .
C15 C14 C17 121.2(6) . .
C15 C14 C13 118.6(7) . .
C13 C14 C17 120.2(6) . .
F47 C44 S40 115.0(7) . .
F47 C44 F46 99.9(11) . .
F45 C44 S40 115.7(9) . .
F45 C44 F47 115.3(11) . .
F45 C44 F46 101.4(10) . .
F46 C44 S40 106.7(9) . .
C24 C23 H23 120.0 . .
C22 C23 C24 119.9(7) . .
C22 C23 H23 120.0 . .
C34 C33 H33 120.3 . .
C32 C33 C34 119.5(8) . .
C32 C33 H33 120.3 . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
C2 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N21 C22 C23 119.9(7) . .
N21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
C13 C12 H12 119.8 . .
N11 C12 C13 120.4(7) . .
N11 C12 H12 119.8 . .
N31 C36 C35 119.8(8) . .
N31 C36 H36 120.1 . .
C35 C36 H36 120.1 . .
C1 C6 C9 120.3(8) . .
C5 C6 C1 118.4(8) . .
C5 C6 C9 121.3(8) . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N31 C30 H30A 108.4 . .
N31 C30 H30B 108.4 . .
C5 C30 N31 115.4(7) . .
C5 C30 H30A 108.4 . .
C5 C30 H30B 108.4 . .
H30A C30 H30B 107.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C27 O28 Tb1 139.0(5) . 1_544
C27 O29 Tb1 136.1(5) . 2_565
C37 O39 Tb1 177.8(5) . 1_554
C37 O38 Tb1 114.5(5) . 2_575
C17 O19 Tb1 133.2(4) . 2_676
Tb1 O1W H1WA 110.3 . .
Tb1 O1W H1WB 110.3 . .
H1WA O1W H1WB 108.5 . .
Tb1 O2W H2WA 110.3 . .
Tb1 O2W H2WB 110.8 . .
H2WA O2W H2WB 108.2 . .
C16 N11 C10 122.3(7) . .
C12 N11 C16 120.8(6) . .
C12 N11 C10 116.9(6) . .
C1 C10 H10A 108.6 . .
C1 C10 H10B 108.6 . .
N11 C10 C1 114.5(7) . .
N11 C10 H10A 108.6 . .
N11 C10 H10B 108.6 . .
H10A C10 H10B 107.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O18 2.319(5) .
Tb1 O28 2.339(5) 1_566
Tb1 O29 2.396(5) 2_565
Tb1 O39 2.327(5) 1_556
Tb1 O38 2.399(5) 2_575
Tb1 O19 2.373(5) 2_676
Tb1 O1W 2.407(6) .
Tb1 O2W 2.468(6) .
S40 O43 1.402(7) .
S40 O42 1.395(7) .
S40 O41 1.473(8) .
S40 C44 1.806(10) .
O18 C17 1.229(9) .
F47 C44 1.315(12) .
C37 C34 1.503(10) .
C37 O39 1.257(9) .
C37 O38 1.263(9) .
F45 C44 1.271(14) .
C25 H25 0.9500 .
C25 C24 1.379(10) .
C25 C26 1.368(10) .
C17 C14 1.517(9) .
C17 O19 1.262(9) .
C1 C2 1.399(12) .
C1 C6 1.413(12) .
C1 C10 1.515(11) .
N21 C20 1.500(9) .
N21 C26 1.344(10) .
N21 C22 1.341(11) .
C3 C2 1.406(11) .
C3 C20 1.506(11) .
C3 C4 1.410(11) .
F46 C44 1.465(19) .
C15 H15 0.9500 .
C15 C16 1.364(10) .
C15 C14 1.381(10) .
C2 C7 1.512(11) .
C34 C35 1.387(11) .
C34 C33 1.377(11) .
N31 C32 1.319(12) .
N31 C36 1.343(11) .
N31 C30 1.511(10) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C27 C24 1.530(9) .
C27 O28 1.261(9) .
C27 O29 1.240(9) .
C16 H16 0.9500 .
C16 N11 1.347(10) .
C13 H13 0.9500 .
C13 C14 1.383(10) .
C13 C12 1.380(10) .
C35 H35 0.9500 .
C35 C36 1.361(12) .
C24 C23 1.389(11) .
C4 C5 1.399(12) .
C4 C8 1.510(11) .
C5 C6 1.406(12) .
C5 C30 1.505(11) .
C32 H32 0.9500 .
C32 C33 1.375(12) .
C26 H26 0.9500 .
C23 H23 0.9500 .
C23 C22 1.361(12) .
C33 H33 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C22 H22 0.9500 .
C12 H12 0.9500 .
C12 N11 1.334(10) .
C36 H36 0.9500 .
C6 C9 1.496(13) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
O1W H1WA 0.8692 .
O1W H1WB 0.8685 .
O2W H2WA 0.8732 .
O2W H2WB 0.8737 .
N11 C10 1.499(9) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O18 C17 C14 C15 175.0(7) .
O18 C17 C14 C13 -5.0(11) .
O18 C17 O19 Tb1 -6.9(12) 2_676
O43 S40 C44 F47 -49.4(14) .
O43 S40 C44 F45 172.3(11) .
O43 S40 C44 F46 60.3(8) .
O42 S40 C44 F47 -175.8(11) .
O42 S40 C44 F45 45.8(14) .
O42 S40 C44 F46 -66.1(8) .
C37 C34 C35 C36 177.5(9) .
C37 C34 C33 C32 -177.9(8) .
O41 S40 C44 F47 65.9(13) .
O41 S40 C44 F45 -72.5(12) .
O41 S40 C44 F46 175.6(7) .
C25 C24 C23 C22 2.0(13) .
C3 C4 C5 C6 -3.7(11) .
C3 C4 C5 C30 167.9(7) .
C15 C16 N11 C12 -0.1(13) .
C15 C16 N11 C10 -177.7(8) .
C2 C1 C6 C5 3.4(11) .
C2 C1 C6 C9 -177.0(8) .
C2 C1 C10 N11 91.3(9) .
C2 C3 C20 N21 103.6(8) .
C2 C3 C4 C5 5.7(11) .
C2 C3 C4 C8 -175.4(7) .
C34 C37 O38 Tb1 178.5(5) 2_575
C34 C35 C36 N31 0.7(15) .
N31 C32 C33 C34 0.0(16) .
C20 N21 C26 C25 -173.9(7) .
C20 N21 C22 C23 175.9(8) .
C20 C3 C2 C1 168.7(7) .
C20 C3 C2 C7 -9.0(11) .
C20 C3 C4 C5 -166.5(7) .
C20 C3 C4 C8 12.4(10) .
C27 C24 C23 C22 -176.7(8) .
C16 C15 C14 C17 179.5(7) .
C16 C15 C14 C13 -0.5(12) .
C16 N11 C10 C1 -15.9(11) .
C13 C12 N11 C16 -0.6(13) .
C13 C12 N11 C10 177.1(8) .
C35 C34 C33 C32 2.3(14) .
C24 C25 C26 N21 -1.1(12) .
C24 C27 O28 Tb1 131.2(6) 1_544
C24 C27 O29 Tb1 -174.9(5) 2_565
C24 C23 C22 N21 -2.5(13) .
C4 C3 C2 C1 -3.2(11) .
C4 C3 C2 C7 179.0(7) .
C4 C3 C20 N21 -84.3(9) .
C4 C5 C6 C1 -0.9(11) .
C4 C5 C6 C9 179.6(8) .
C4 C5 C30 N31 94.6(9) .
C32 N31 C36 C35 1.8(15) .
C32 N31 C30 C5 35.1(12) .
C26 C25 C24 C27 178.5(7) .
C26 C25 C24 C23 -0.2(12) .
C26 N21 C20 C3 -41.9(11) .
C26 N21 C22 C23 1.1(13) .
C14 C17 O19 Tb1 171.7(5) 2_676
C14 C15 C16 N11 0.7(13) .
C14 C13 C12 N11 0.8(13) .
C33 C34 C35 C36 -2.7(14) .
C22 N21 C20 C3 143.4(8) .
C22 N21 C26 C25 0.7(12) .
C12 C13 C14 C17 179.8(7) .
C12 C13 C14 C15 -0.2(12) .
C12 N11 C10 C1 166.4(8) .
C36 N31 C32 C33 -2.1(15) .
C36 N31 C30 C5 -147.3(9) .
C6 C1 C2 C3 -1.4(11) .
C6 C1 C2 C7 176.4(8) .
C6 C1 C10 N11 -88.8(9) .
C6 C5 C30 N31 -93.8(9) .
C8 C4 C5 C6 177.4(7) .
C8 C4 C5 C30 -11.0(11) .
C30 N31 C32 C33 175.3(9) .
C30 N31 C36 C35 -175.8(9) .
C30 C5 C6 C1 -172.2(7) .
C30 C5 C6 C9 8.3(12) .
O28 C27 C24 C25 162.4(7) .
O28 C27 C24 C23 -18.9(10) .
O28 C27 O29 Tb1 6.4(13) 2_565
O29 C27 C24 C25 -16.5(11) .
O29 C27 C24 C23 162.2(7) .
O29 C27 O28 Tb1 -50.0(12) 1_544
O39 C37 C34 C35 5.6(12) .
O39 C37 C34 C33 -174.2(8) .
O39 C37 O38 Tb1 -0.7(9) 2_575
O38 C37 C34 C35 -173.7(8) .
O38 C37 C34 C33 6.5(12) .
O19 C17 C14 C15 -3.7(10) .
O19 C17 C14 C13 176.3(7) .
C10 C1 C2 C3 178.6(7) .
C10 C1 C2 C7 -3.7(12) .
C10 C1 C6 C5 -176.5(7) .
C10 C1 C6 C9 3.1(12) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0105 -8.0023 9.9911 0.8691 0.4699 -0.3202
-0.0105 8.0023 -9.9911 -0.8691 -0.4699 0.3202
-0.0054 -3.9954 -8.0022 -0.3247 -0.2547 -0.9006
0.0054 3.9954 8.0022 0.3247 0.2547 0.9006
-5.9986 0.9967 5.0081 0.6266 -0.7530 0.1445
5.9986 -0.9967 -5.0081 -0.6266 0.7530 -0.1445
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 -0.816 0.500 0.500 602.7 182.8 '18x water'
