#------------------------------------------------------------------------------
#$Date: 2022-05-04 01:50:10 +0300 (Wed, 04 May 2022) $
#$Revision: 274857 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710172.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_7710172
loop_
_publ_author_name
'Tzegai, Wintana'
'Reil, Michaela'
'Burzlaff, Nicolai'
_publ_section_title
;
 Bis(4-carboxylpyrazol-1-yl)acetic acid: a scorpionate ligand for
 complexes with improved water solubility.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6839
_journal_page_last               6845
_journal_paper_doi               10.1039/d2dt00848c
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C13 H7 N4 O9 Re, 0.5(H2 O)'
_chemical_formula_sum            'C13 H8 N4 O9.5 Re'
_chemical_formula_weight         558.43
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                107.251(3)
_cell_angle_beta                 94.748(3)
_cell_angle_gamma                110.515(3)
_cell_formula_units_Z            8
_cell_length_a                   14.3811(5)
_cell_length_b                   15.1010(5)
_cell_length_c                   17.2257(6)
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.2770
_cell_measurement_theta_min      3.3090
_cell_volume                     3272.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -17.00   1.00    5.00    --  -40.61 -38.00   0.00   92
  2  ω   -115.00 -19.00   1.00    5.00    --  -40.61 -38.00 -90.00   96
  3  ω      6.00  78.00   1.00    5.00    --   40.61 -99.00  60.00   72
  4  ω    -21.00  73.00   1.00    5.00    --   40.61 -77.00-180.00   94
  5  ω     30.00 128.00   1.00   20.00    --  104.57 -30.00-150.00   98
  6  ω     28.00  55.00   1.00   20.00    --  104.57-111.00  90.00   27
  7  ω     80.00 173.00   1.00   20.00    --  104.57  45.00-120.00   93
  8  ω     29.00 117.00   1.00   20.00    --  104.57 -77.00-180.00   88
  9  ω     71.00 109.00   1.00   20.00    --  104.57-111.00  90.00   38
 10  ω     23.00 106.00   1.00   20.00    --  104.57 -94.00 150.00   83
 11  ω     32.00 134.00   1.00   20.00    --  104.57 -61.00 -30.00  102
 12  ω    123.00 159.00   1.00   20.00    --  104.57  77.00-180.00   36
 13  ω     56.00 109.00   1.00   20.00    --  104.57-111.00 -30.00   53
 14  ω     27.00 130.00   1.00   20.00    --  104.57 -15.00  60.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1156875000
_diffrn_orient_matrix_UB_12      -0.0298128000
_diffrn_orient_matrix_UB_13      -0.0178049000
_diffrn_orient_matrix_UB_21      0.0142515000
_diffrn_orient_matrix_UB_22      0.1015528000
_diffrn_orient_matrix_UB_23      0.0651170000
_diffrn_orient_matrix_UB_31      0.0095729000
_diffrn_orient_matrix_UB_32      0.0480264000
_diffrn_orient_matrix_UB_33      -0.0679117000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21454
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.529
_diffrn_reflns_theta_min         2.747
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.146
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1008
_refine_ls_number_reflns         12476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0291P)²+1.6826P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10901
_reflns_number_total             12476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00848c2.cif
_cod_data_source_block           buni211203a
_cod_original_formula_sum        'C13 H8 N4 O9.50 Re'
_cod_database_code               7710172
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H8N4O9.5Re
_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 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C101(H101), C301(H301), C1(H1), C201(H201)
2.c Aromatic/amide H refined with riding coordinates:
 C324(H324), C224(H224), C114(H114), C222(H222), C314(H314), C14(H14),
 C212(H212), C12(H12), C322(H322), C122(H122), C24(H24), C214(H214), C112(H112),
  C22(H22), C124(H124), C312(H312)
2.d Idealised tetrahedral OH refined as rotating group:
 O321(H321), O111(H111), O11(H11), O121(H121), O311(H311), O221(H221), O21(H21)
;
_olex2_date_sample_data_collection 2021-12-03
_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 3.456
_oxdiff_exptl_absorpt_empirical_full_min 0.632
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
Re3 Re 0.28044(2) 0.21923(2) 0.22812(2) 0.01381(5) Uani 1 1 d . . . . .
Re1 Re 1.20666(2) 0.81506(2) 1.26647(2) 0.01598(6) Uani 1 1 d . . . . .
Re2 Re 1.20779(2) 1.13964(2) 0.69736(2) 0.01651(6) Uani 1 1 d . . . . .
Re4 Re 0.29585(2) 0.67415(2) -0.21618(2) 0.01877(6) Uani 1 1 d . . . . .
O201 O 0.1891(3) 0.3070(3) 0.2283(2) 0.0171(7) Uani 1 1 d . . . . .
O1 O 1.2944(3) 0.7206(3) 1.2501(2) 0.0188(7) Uani 1 1 d . . . . .
O321 O 0.1377(3) 0.5257(3) 0.0981(2) 0.0206(7) Uani 1 1 d . . . . .
H321 H 0.148090 0.499378 0.131407 0.031 Uiso 1 1 calc R U . . .
O302 O 0.0738(3) 0.7933(3) -0.1567(2) 0.0197(7) Uani 1 1 d . . . . .
O202 O 0.1609(3) 0.4310(3) 0.1999(2) 0.0185(7) Uani 1 1 d . . . . .
O101 O 1.3050(3) 1.0751(3) 0.7397(2) 0.0189(7) Uani 1 1 d . . . . .
O102 O 1.3371(3) 0.9822(3) 0.8080(2) 0.0177(7) Uani 1 1 d . . . . .
O301 O 0.2049(3) 0.7642(3) -0.1987(3) 0.0228(8) Uani 1 1 d . . . . .
O205 O 0.4135(3) 0.0997(3) 0.2299(3) 0.0279(8) Uani 1 1 d . . . . .
O222 O 0.4447(3) 0.2003(3) -0.0860(2) 0.0275(9) Uani 1 1 d . . . . .
O111 O 1.0505(3) 1.1772(3) 1.0562(2) 0.0234(8) Uani 1 1 d . . . . .
H111 H 1.014260 1.193842 1.086834 0.035 Uiso 1 1 calc R U . . .
O6 O 1.6841(3) 1.3664(3) 1.6289(3) 0.0271(8) Uani 1 1 d G . . . .
H6A H 1.730672 1.381011 1.601933 0.041 Uiso 1 1 d G U . . .
H6B H 1.712366 1.359895 1.671026 0.041 Uiso 1 1 d G U . . .
O4 O 1.0899(3) 0.9512(3) 1.2769(3) 0.0278(9) Uani 1 1 d . . . . .
O212 O 0.6682(3) 0.5443(3) 0.4835(3) 0.0300(9) Uani 1 1 d . . . . .
O11 O 1.3655(3) 0.9464(3) 0.9455(2) 0.0266(8) Uani 1 1 d . . . . .
H11 H 1.352444 0.963505 0.906417 0.040 Uiso 1 1 calc R U . . .
O204 O 0.1041(3) 0.0204(3) 0.1208(2) 0.0254(8) Uani 1 1 d . . . . .
O5 O 1.0022(3) 0.6399(3) 1.1760(3) 0.0307(9) Uani 1 1 d . . . . .
O121 O 0.8474(3) 0.6721(3) 0.5879(2) 0.0243(8) Uani 1 1 d . . . . .
H121 H 0.799596 0.625498 0.552820 0.036 Uiso 1 1 calc R U . . .
N221 N 0.3234(3) 0.2695(3) 0.1248(3) 0.0157(8) Uani 1 1 d . . . . .
O312 O -0.1625(3) 0.3869(3) -0.4681(3) 0.0315(9) Uani 1 1 d . . . . .
O22 O 1.6667(3) 1.1739(3) 1.4771(2) 0.0279(8) Uani 1 1 d . . . . .
O12 O 1.2278(3) 0.9719(3) 0.9780(2) 0.0270(8) Uani 1 1 d . . . . .
O311 O -0.0377(3) 0.3526(3) -0.5225(2) 0.0286(9) Uani 1 1 d . . . . .
H311 H -0.084452 0.311729 -0.561480 0.043 Uiso 1 1 calc R U . . .
O304 O 0.4211(3) 0.5494(3) -0.2116(3) 0.0311(9) Uani 1 1 d . . . . .
N22 N 1.4397(3) 0.9243(3) 1.2955(2) 0.0161(8) Uani 1 1 d . . . . .
N11 N 1.2637(3) 0.8417(3) 1.1585(3) 0.0162(8) Uani 1 1 d . . . . .
O112 O 1.0335(3) 1.2929(3) 1.0051(2) 0.0258(8) Uani 1 1 d . . . . .
O221 O 0.4840(3) 0.3608(3) -0.0751(3) 0.0284(9) Uani 1 1 d . . . . .
H221 H 0.506612 0.344135 -0.116724 0.043 Uiso 1 1 calc R U . . .
O21 O 1.5358(3) 1.1947(3) 1.5299(3) 0.0339(9) Uani 1 1 d . . . . .
H21 H 1.579075 1.250221 1.558573 0.051 Uiso 1 1 calc R U . . .
O211 O 0.6567(4) 0.6650(3) 0.4364(3) 0.0355(10) Uani 1 1 d . . . . .
N321 N 0.2348(3) 0.6335(3) -0.1155(3) 0.0185(8) Uani 1 1 d . . . . .
N203 N 0.3481(3) 0.3692(3) 0.1327(3) 0.0153(8) Uani 1 1 d . . . . .
O2 O 1.4232(3) 0.6845(3) 1.2089(3) 0.0267(9) Uani 1 1 d . . . . .
N12 N 1.3615(3) 0.8554(3) 1.1520(2) 0.0150(8) Uani 1 1 d . . . . .
N212 N 0.3972(3) 0.4508(3) 0.2798(3) 0.0153(8) Uani 1 1 d . . . . .
N21 N 1.3579(4) 0.9303(3) 1.3288(3) 0.0195(9) Uani 1 1 d . . . . .
O122 O 0.8531(3) 0.7449(3) 0.4904(2) 0.0296(9) Uani 1 1 d . . . . .
O3 O 1.1429(3) 0.7995(4) 1.4297(3) 0.0343(10) Uani 1 1 d . . . . .
O206 O 0.2469(4) 0.1635(3) 0.3831(2) 0.0306(9) Uani 1 1 d . . . . .
O103 O 1.2517(4) 1.0913(3) 0.5216(3) 0.0356(11) Uani 1 1 d . . . . .
O322 O 0.2799(4) 0.5122(4) 0.0648(3) 0.0377(11) Uani 1 1 d . . . . .
N111 N 1.1687(3) 1.1540(3) 0.8192(3) 0.0165(8) Uani 1 1 d . . . . .
O303 O 0.4917(3) 0.8422(3) -0.0997(3) 0.0360(10) Uani 1 1 d . . . . .
O105 O 1.3789(4) 1.3499(3) 0.7593(3) 0.0400(11) Uani 1 1 d . . . . .
O305 O 0.3807(4) 0.7191(4) -0.3644(3) 0.0366(10) Uani 1 1 d . . . . .
N112 N 1.1590(3) 1.0779(3) 0.8500(2) 0.0143(8) Uani 1 1 d . . . . .
O104 O 1.0595(4) 1.2306(4) 0.6569(3) 0.0408(12) Uani 1 1 d . . . . .
N211 N 0.3948(3) 0.3689(3) 0.3010(2) 0.0151(8) Uani 1 1 d . . . . .
N312 N 0.0629(3) 0.5612(3) -0.2536(3) 0.0194(9) Uani 1 1 d . . . . .
N122 N 1.0953(3) 0.9387(3) 0.7229(3) 0.0172(8) Uani 1 1 d . . . . .
N121 N 1.0995(3) 0.9860(3) 0.6654(2) 0.0173(8) Uani 1 1 d . . . . .
N311 N 0.1464(4) 0.5610(3) -0.2886(3) 0.0207(9) Uani 1 1 d . . . . .
N322 N 0.1361(3) 0.6186(3) -0.1093(3) 0.0190(9) Uani 1 1 d . . . . .
O7 O -0.1963(4) 0.1990(3) -0.6321(3) 0.0345(10) Uani 1 1 d G . . . .
H7A H -0.202703 0.243764 -0.650051 0.052 Uiso 1 1 d G U . . .
H7B H -0.245791 0.183380 -0.608050 0.052 Uiso 1 1 d G U . . .
C324 C 0.1114(4) 0.5852(4) -0.0467(3) 0.0180(10) Uani 1 1 d . . . . .
H324 H 0.049299 0.570756 -0.030505 0.022 Uiso 1 1 calc R U . . .
C224 C 0.3933(4) 0.3898(4) 0.0719(3) 0.0149(9) Uani 1 1 d . . . . .
H224 H 0.417719 0.452105 0.064957 0.018 Uiso 1 1 calc R U . . .
C202 C 0.2167(4) 0.3872(3) 0.2111(3) 0.0138(9) Uani 1 1 d . . . . .
C203 C 0.1708(4) 0.0945(4) 0.1605(3) 0.0224(11) Uani 1 1 d . . . . .
C114 C 1.1217(4) 1.0928(4) 0.9193(3) 0.0154(9) Uani 1 1 d . . . . .
H114 H 1.107722 1.050878 0.950715 0.018 Uiso 1 1 calc R U . . .
C23 C 1.5017(4) 1.0562(4) 1.4091(3) 0.0208(10) Uani 1 1 d . . . . .
C5 C 1.0797(4) 0.7056(4) 1.2085(3) 0.0222(11) Uani 1 1 d . . . . .
C303 C 0.4185(4) 0.7817(4) -0.1428(4) 0.0253(12) Uani 1 1 d . . . . .
C222 C 0.3515(4) 0.2289(4) 0.0569(3) 0.0156(9) Uani 1 1 d . . . . .
H222 H 0.342437 0.161554 0.035503 0.019 Uiso 1 1 calc R U . . .
C323 C 0.1953(4) 0.5766(4) -0.0113(3) 0.0209(10) Uani 1 1 d . . . . .
C102 C 1.2804(4) 1.0169(3) 0.7819(3) 0.0141(9) Uani 1 1 d . . . . .
C116 C 1.0611(4) 1.2248(4) 1.0020(3) 0.0164(9) Uani 1 1 d . . . . .
C113 C 1.1077(4) 1.1819(4) 0.9355(3) 0.0166(9) Uani 1 1 d . . . . .
C223 C 0.3972(4) 0.3018(4) 0.0211(3) 0.0171(10) Uani 1 1 d . . . . .
C314 C -0.0232(4) 0.5033(4) -0.3110(3) 0.0195(10) Uani 1 1 d . . . . .
H314 H -0.088633 0.493200 -0.302448 0.023 Uiso 1 1 calc R U . . .
C304 C 0.3721(4) 0.5929(4) -0.2187(3) 0.0233(11) Uani 1 1 d . . . . .
C13 C 1.3040(4) 0.9006(4) 1.0550(3) 0.0176(10) Uani 1 1 d . . . . .
C101 C 1.1724(4) 0.9891(3) 0.8005(3) 0.0143(9) Uani 1 1 d . . . . .
H101 H 1.162792 0.942782 0.831493 0.017 Uiso 1 1 calc R U . . .
C302 C 0.1215(4) 0.7397(4) -0.1746(3) 0.0168(9) Uani 1 1 d . . . . .
C14 C 1.3875(4) 0.8901(3) 1.0903(3) 0.0183(10) Uani 1 1 d . . . . .
H14 H 1.449868 0.904418 1.074411 0.022 Uiso 1 1 calc R U . . .
C2 C 1.3776(4) 0.7397(4) 1.2251(3) 0.0184(10) Uani 1 1 d . . . . .
C226 C 0.4434(4) 0.2818(4) -0.0518(3) 0.0170(10) Uani 1 1 d . . . . .
C205 C 0.2536(4) 0.1843(4) 0.3254(3) 0.0217(11) Uani 1 1 d . . . . .
C16 C 1.2947(4) 0.9427(4) 0.9894(3) 0.0192(10) Uani 1 1 d . . . . .
C301 C 0.0743(4) 0.6316(4) -0.1725(3) 0.0174(10) Uani 1 1 d . . . . .
H301 H 0.006894 0.619960 -0.159527 0.021 Uiso 1 1 calc R U . . .
C1 C 1.4247(4) 0.8451(4) 1.2168(3) 0.0172(10) Uani 1 1 d . . . . .
H1 H 1.491087 0.854014 1.202272 0.021 Uiso 1 1 calc R U . . .
C313 C 0.0016(5) 0.4619(4) -0.3839(3) 0.0235(11) Uani 1 1 d . . . . .
C212 C 0.4709(4) 0.4050(4) 0.3649(3) 0.0176(9) Uani 1 1 d . . . . .
H212 H 0.487543 0.366727 0.392821 0.021 Uiso 1 1 calc R U . . .
C105 C 1.3145(5) 1.2716(4) 0.7349(4) 0.0266(12) Uani 1 1 d . . . . .
C12 C 1.2288(4) 0.8690(4) 1.0993(3) 0.0181(10) Uani 1 1 d . . . . .
H12 H 1.163636 0.867356 1.088806 0.022 Uiso 1 1 calc R U . . .
C322 C 0.2700(4) 0.6070(4) -0.0565(3) 0.0237(11) Uani 1 1 d . . . . .
H322 H 0.335071 0.608409 -0.046243 0.028 Uiso 1 1 calc R U . . .
C122 C 1.0270(4) 0.9207(4) 0.6007(3) 0.0206(10) Uani 1 1 d . . . . .
H122 H 1.012534 0.932016 0.551756 0.025 Uiso 1 1 calc R U . . .
C26 C 1.5760(4) 1.1467(4) 1.4750(3) 0.0234(11) Uani 1 1 d . . . . .
C24 C 1.5264(4) 0.9979(4) 1.3432(3) 0.0190(10) Uani 1 1 d . . . . .
H24 H 1.591332 1.007896 1.333517 0.023 Uiso 1 1 calc R U . . .
C201 C 0.3291(4) 0.4348(3) 0.2049(3) 0.0141(9) Uani 1 1 d . . . . .
H201 H 0.342006 0.500050 0.198220 0.017 Uiso 1 1 calc R U . . .
C204 C 0.3648(4) 0.1461(4) 0.2265(3) 0.0221(11) Uani 1 1 d . . . . .
C216 C 0.6228(4) 0.5735(4) 0.4400(3) 0.0221(11) Uani 1 1 d . . . . .
C103 C 1.2370(5) 1.1117(4) 0.5876(4) 0.0272(12) Uani 1 1 d . . . . .
C4 C 1.1352(4) 0.9012(4) 1.2743(3) 0.0223(11) Uani 1 1 d . . . . .
C213 C 0.5234(4) 0.5095(4) 0.3850(3) 0.0192(10) Uani 1 1 d . . . . .
C214 C 0.4734(4) 0.5348(4) 0.3289(3) 0.0184(10) Uani 1 1 d . . . . .
H214 H 0.489956 0.598823 0.325925 0.022 Uiso 1 1 calc R U . . .
C112 C 1.1376(4) 1.2164(4) 0.8706(3) 0.0207(10) Uani 1 1 d . . . . .
H112 H 1.135638 1.275048 0.864724 0.025 Uiso 1 1 calc R U . . .
C3 C 1.1680(4) 0.8027(4) 1.3691(4) 0.0269(12) Uani 1 1 d . . . . .
C22 C 1.3951(4) 1.0107(4) 1.3972(3) 0.0183(10) Uani 1 1 d . . . . .
H22 H 1.356631 1.033935 1.432499 0.022 Uiso 1 1 calc R U . . .
C126 C 0.8873(4) 0.7458(4) 0.5577(3) 0.0246(11) Uani 1 1 d . . . . .
C316 C -0.0744(5) 0.3966(4) -0.4620(3) 0.0255(11) Uani 1 1 d . . . . .
C326 C 0.2090(5) 0.5354(4) 0.0539(3) 0.0229(11) Uani 1 1 d . . . . .
C124 C 1.0201(4) 0.8471(4) 0.6942(3) 0.0179(10) Uani 1 1 d . . . . .
H124 H 1.001926 0.801804 0.722409 0.022 Uiso 1 1 calc R U . . .
C123 C 0.9746(4) 0.8321(4) 0.6157(3) 0.0210(10) Uani 1 1 d . . . . .
C305 C 0.3485(4) 0.7042(4) -0.3099(4) 0.0267(12) Uani 1 1 d . . . . .
C312 C 0.1080(4) 0.4991(4) -0.3666(3) 0.0210(10) Uani 1 1 d . . . . .
H312 H 0.146499 0.482364 -0.404888 0.025 Uiso 1 1 calc R U . . .
C104 C 1.1151(5) 1.1956(5) 0.6695(4) 0.0266(12) Uani 1 1 d . . . . .
H211 H 0.719(6) 0.688(5) 0.453(5) 0.029(19) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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 -1 -2 0.0297
-2 9 -2 0.0066
1 -2 -1 0.0222
0 1 -2 0.0278
0 -1 2 0.0300
1 -2 0 0.0181
-2 0 1 0.0338
1 1 0 0.0291
0 2 -1 0.0156
-3 10 -4 0.0156
-2 -8 4 0.0156
-3 -2 -8 0.0321
2 -1 0 0.0260
1 0 -2 0.0326
-9 7 0 0.0228
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
O201 Re3 N221 80.82(14) . . ?
O201 Re3 N211 80.80(14) . . ?
N211 Re3 N221 82.04(15) . . ?
C203 Re3 O201 93.17(18) . . ?
C203 Re3 N221 95.55(18) . . ?
C203 Re3 N211 173.78(18) . . ?
C203 Re3 C205 89.4(2) . . ?
C205 Re3 O201 100.00(18) . . ?
C205 Re3 N221 174.9(2) . . ?
C205 Re3 N211 93.14(19) . . ?
C204 Re3 O201 177.58(18) . . ?
C204 Re3 N221 97.16(19) . . ?
C204 Re3 N211 97.64(19) . . ?
C204 Re3 C203 88.3(2) . . ?
C204 Re3 C205 81.9(2) . . ?
N11 Re1 O1 81.80(14) . . ?
N11 Re1 N21 80.61(16) . . ?
N21 Re1 O1 80.17(15) . . ?
C5 Re1 O1 94.69(18) . . ?
C5 Re1 N11 97.98(19) . . ?
C5 Re1 N21 174.80(18) . . ?
C5 Re1 C3 87.7(2) . . ?
C4 Re1 O1 175.47(17) . . ?
C4 Re1 N11 93.73(18) . . ?
C4 Re1 N21 98.4(2) . . ?
C4 Re1 C5 86.6(2) . . ?
C4 Re1 C3 86.3(2) . . ?
C3 Re1 O1 98.06(19) . . ?
C3 Re1 N11 174.3(2) . . ?
C3 Re1 N21 93.8(2) . . ?
O101 Re2 N111 82.83(14) . . ?
O101 Re2 N121 80.30(15) . . ?
N121 Re2 N111 82.68(15) . . ?
C105 Re2 O101 92.6(2) . . ?
C105 Re2 N111 94.3(2) . . ?
C105 Re2 N121 172.6(2) . . ?
C105 Re2 C103 91.1(2) . . ?
C103 Re2 O101 94.04(18) . . ?
C103 Re2 N111 173.86(19) . . ?
C103 Re2 N121 91.6(2) . . ?
C104 Re2 O101 173.99(18) . . ?
C104 Re2 N111 91.30(19) . . ?
C104 Re2 N121 97.7(2) . . ?
C104 Re2 C105 89.1(3) . . ?
C104 Re2 C103 91.7(2) . . ?
O301 Re4 N311 78.80(15) . . ?
N321 Re4 O301 83.44(15) . . ?
N321 Re4 N311 82.08(16) . . ?
C303 Re4 O301 95.11(19) . . ?
C303 Re4 N321 93.3(2) . . ?
C303 Re4 N311 172.69(19) . . ?
C303 Re4 C305 88.7(2) . . ?
C304 Re4 O301 172.84(18) . . ?
C304 Re4 N321 89.53(19) . . ?
C304 Re4 N311 101.6(2) . . ?
C304 Re4 C303 83.9(2) . . ?
C304 Re4 C305 89.0(2) . . ?
C305 Re4 O301 98.05(19) . . ?
C305 Re4 N321 177.4(2) . . ?
C305 Re4 N311 96.1(2) . . ?
C202 O201 Re3 124.0(3) . . ?
C2 O1 Re1 125.2(3) . . ?
C326 O321 H321 109.5 . . ?
C102 O101 Re2 124.1(3) . . ?
C302 O301 Re4 123.7(3) . . ?
C116 O111 H111 109.5 . . ?
H6A O6 H6B 104.4 . . ?
C16 O11 H11 109.5 . . ?
C126 O121 H121 109.5 . . ?
N203 N221 Re3 119.9(3) . . ?
C222 N221 Re3 132.7(3) . . ?
C222 N221 N203 105.9(4) . . ?
C316 O311 H311 109.5 . . ?
N21 N22 C1 120.1(4) . . ?
C24 N22 N21 111.4(4) . . ?
C24 N22 C1 128.5(4) . . ?
N12 N11 Re1 121.2(3) . . ?
C12 N11 Re1 132.0(4) . . ?
C12 N11 N12 105.3(4) . . ?
C226 O221 H221 109.5 . . ?
C26 O21 H21 109.5 . . ?
C216 O211 H211 105(5) . . ?
N322 N321 Re4 121.3(3) . . ?
C322 N321 Re4 132.9(4) . . ?
C322 N321 N322 105.3(4) . . ?
N221 N203 C201 118.5(4) . . ?
C224 N203 N221 110.7(4) . . ?
C224 N203 C201 130.7(4) . . ?
N11 N12 C1 117.9(4) . . ?
C14 N12 N11 111.8(4) . . ?
C14 N12 C1 129.7(5) . . ?
N211 N212 C201 119.4(4) . . ?
C214 N212 N211 111.3(4) . . ?
C214 N212 C201 128.9(4) . . ?
N22 N21 Re1 119.3(3) . . ?
C22 N21 Re1 135.0(4) . . ?
C22 N21 N22 105.8(4) . . ?
N112 N111 Re2 119.1(3) . . ?
C112 N111 Re2 134.2(3) . . ?
C112 N111 N112 106.1(4) . . ?
N111 N112 C101 119.4(4) . . ?
C114 N112 N111 110.8(4) . . ?
C114 N112 C101 129.0(4) . . ?
N212 N211 Re3 119.5(3) . . ?
C212 N211 Re3 134.9(3) . . ?
C212 N211 N212 105.5(4) . . ?
N311 N312 C301 121.3(4) . . ?
C314 N312 N311 110.2(4) . . ?
C314 N312 C301 127.3(4) . . ?
N121 N122 C101 119.1(4) . . ?
C124 N122 N121 110.8(4) . . ?
C124 N122 C101 130.0(4) . . ?
N122 N121 Re2 119.3(3) . . ?
C122 N121 Re2 135.2(3) . . ?
C122 N121 N122 105.5(4) . . ?
N312 N311 Re4 117.3(3) . . ?
C312 N311 Re4 136.4(4) . . ?
C312 N311 N312 105.1(4) . . ?
N321 N322 C301 117.7(4) . . ?
C324 N322 N321 111.4(4) . . ?
C324 N322 C301 130.6(5) . . ?
H7A O7 H7B 104.4 . . ?
N322 C324 H324 126.5 . . ?
N322 C324 C323 106.9(5) . . ?
C323 C324 H324 126.5 . . ?
N203 C224 H224 126.2 . . ?
N203 C224 C223 107.5(4) . . ?
C223 C224 H224 126.2 . . ?
O201 C202 C201 117.4(4) . . ?
O202 C202 O201 125.0(5) . . ?
O202 C202 C201 117.6(4) . . ?
O204 C203 Re3 178.8(5) . . ?
N112 C114 H114 126.3 . . ?
N112 C114 C113 107.3(4) . . ?
C113 C114 H114 126.3 . . ?
C24 C23 C26 124.1(5) . . ?
C24 C23 C22 105.5(5) . . ?
C22 C23 C26 130.4(5) . . ?
O5 C5 Re1 177.8(5) . . ?
O303 C303 Re4 177.5(5) . . ?
N221 C222 H222 124.7 . . ?
N221 C222 C223 110.6(4) . . ?
C223 C222 H222 124.7 . . ?
C324 C323 C322 105.8(5) . . ?
C324 C323 C326 130.6(5) . . ?
C322 C323 C326 123.3(5) . . ?
O101 C102 C101 117.0(4) . . ?
O102 C102 O101 124.0(5) . . ?
O102 C102 C101 119.0(4) . . ?
O111 C116 C113 111.0(4) . . ?
O112 C116 O111 124.7(4) . . ?
O112 C116 C113 124.3(4) . . ?
C114 C113 C116 126.6(4) . . ?
C114 C113 C112 105.3(4) . . ?
C112 C113 C116 127.8(4) . . ?
C224 C223 C222 105.2(4) . . ?
C224 C223 C226 131.0(4) . . ?
C222 C223 C226 123.7(4) . . ?
N312 C314 H314 125.9 . . ?
N312 C314 C313 108.3(5) . . ?
C313 C314 H314 125.9 . . ?
O304 C304 Re4 172.9(5) . . ?
C14 C13 C16 128.8(5) . . ?
C14 C13 C12 105.5(4) . . ?
C12 C13 C16 125.6(5) . . ?
N112 C101 N122 109.1(4) . . ?
N112 C101 C102 111.1(4) . . ?
N112 C101 H101 108.6 . . ?
N122 C101 C102 110.6(4) . . ?
N122 C101 H101 108.6 . . ?
C102 C101 H101 108.6 . . ?
O302 C302 O301 125.0(5) . . ?
O302 C302 C301 117.9(4) . . ?
O301 C302 C301 117.1(4) . . ?
N12 C14 C13 106.8(5) . . ?
N12 C14 H14 126.6 . . ?
C13 C14 H14 126.6 . . ?
O1 C2 C1 115.5(4) . . ?
O2 C2 O1 126.3(5) . . ?
O2 C2 C1 118.2(5) . . ?
O222 C226 O221 123.7(5) . . ?
O222 C226 C223 121.8(4) . . ?
O221 C226 C223 114.5(4) . . ?
O206 C205 Re3 173.4(5) . . ?
O11 C16 C13 113.8(5) . . ?
O12 C16 O11 123.7(5) . . ?
O12 C16 C13 122.5(5) . . ?
N312 C301 N322 111.3(4) . . ?
N312 C301 C302 108.6(4) . . ?
N312 C301 H301 108.6 . . ?
N322 C301 C302 111.1(4) . . ?
N322 C301 H301 108.6 . . ?
C302 C301 H301 108.6 . . ?
N22 C1 N12 109.2(4) . . ?
N22 C1 C2 110.4(4) . . ?
N22 C1 H1 108.4 . . ?
N12 C1 C2 112.0(4) . . ?
N12 C1 H1 108.4 . . ?
C2 C1 H1 108.4 . . ?
C314 C313 C316 123.4(5) . . ?
C314 C313 C312 105.2(5) . . ?
C312 C313 C316 131.4(5) . . ?
N211 C212 H212 124.8 . . ?
N211 C212 C213 110.4(4) . . ?
C213 C212 H212 124.8 . . ?
O105 C105 Re2 178.1(5) . . ?
N11 C12 C13 110.6(5) . . ?
N11 C12 H12 124.7 . . ?
C13 C12 H12 124.7 . . ?
N321 C322 C323 110.6(5) . . ?
N321 C322 H322 124.7 . . ?
C323 C322 H322 124.7 . . ?
N121 C122 H122 124.6 . . ?
N121 C122 C123 110.8(4) . . ?
C123 C122 H122 124.6 . . ?
O22 C26 O21 124.0(5) . . ?
O22 C26 C23 121.7(5) . . ?
O21 C26 C23 114.3(5) . . ?
N22 C24 C23 107.1(5) . . ?
N22 C24 H24 126.4 . . ?
C23 C24 H24 126.4 . . ?
N203 C201 C202 109.6(4) . . ?
N203 C201 H201 108.8 . . ?
N212 C201 N203 109.8(4) . . ?
N212 C201 C202 110.9(4) . . ?
N212 C201 H201 108.8 . . ?
C202 C201 H201 108.8 . . ?
O205 C204 Re3 175.3(5) . . ?
O212 C216 O211 124.9(5) . . ?
O212 C216 C213 123.3(5) . . ?
O211 C216 C213 111.8(5) . . ?
O103 C103 Re2 177.4(6) . . ?
O4 C4 Re1 177.9(5) . . ?
C212 C213 C216 127.3(5) . . ?
C214 C213 C212 105.4(5) . . ?
C214 C213 C216 125.9(5) . . ?
N212 C214 C213 107.3(4) . . ?
N212 C214 H214 126.3 . . ?
C213 C214 H214 126.3 . . ?
N111 C112 C113 110.4(4) . . ?
N111 C112 H112 124.8 . . ?
C113 C112 H112 124.8 . . ?
O3 C3 Re1 176.1(5) . . ?
N21 C22 C23 110.2(4) . . ?
N21 C22 H22 124.9 . . ?
C23 C22 H22 124.9 . . ?
O121 C126 C123 113.4(5) . . ?
O122 C126 O121 124.3(5) . . ?
O122 C126 C123 122.2(5) . . ?
O312 C316 O311 124.3(5) . . ?
O312 C316 C313 121.3(5) . . ?
O311 C316 C313 114.4(5) . . ?
O321 C326 C323 114.5(5) . . ?
O322 C326 O321 123.8(5) . . ?
O322 C326 C323 121.7(5) . . ?
N122 C124 H124 126.3 . . ?
N122 C124 C123 107.5(4) . . ?
C123 C124 H124 126.3 . . ?
C122 C123 C126 124.7(5) . . ?
C124 C123 C122 105.4(5) . . ?
C124 C123 C126 129.8(5) . . ?
O305 C305 Re4 177.4(5) . . ?
N311 C312 C313 111.1(5) . . ?
N311 C312 H312 124.4 . . ?
C313 C312 H312 124.4 . . ?
O104 C104 Re2 176.6(5) . . ?
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
Re3 O201 2.168(3) . ?
Re3 N221 2.186(4) . ?
Re3 N211 2.182(4) . ?
Re3 C203 1.924(6) . ?
Re3 C205 1.929(5) . ?
Re3 C204 1.902(6) . ?
Re1 O1 2.189(3) . ?
Re1 N11 2.181(4) . ?
Re1 N21 2.183(5) . ?
Re1 C5 1.915(6) . ?
Re1 C4 1.903(6) . ?
Re1 C3 1.937(6) . ?
Re2 O101 2.154(3) . ?
Re2 N111 2.187(4) . ?
Re2 N121 2.163(4) . ?
Re2 C105 1.916(6) . ?
Re2 C103 1.927(6) . ?
Re2 C104 1.909(6) . ?
Re4 O301 2.172(4) . ?
Re4 N321 2.158(4) . ?
Re4 N311 2.194(5) . ?
Re4 C303 1.937(6) . ?
Re4 C304 1.905(6) . ?
Re4 C305 1.945(6) . ?
O201 C202 1.267(6) . ?
O1 C2 1.273(6) . ?
O321 H321 0.8200 . ?
O321 C326 1.320(7) . ?
O302 C302 1.225(6) . ?
O202 C202 1.243(6) . ?
O101 C102 1.276(6) . ?
O102 C102 1.233(6) . ?
O301 C302 1.269(6) . ?
O205 C204 1.160(7) . ?
O222 C226 1.204(6) . ?
O111 H111 0.8200 . ?
O111 C116 1.326(6) . ?
O6 H6A 0.8497 . ?
O6 H6B 0.8506 . ?
O4 C4 1.151(7) . ?
O212 C216 1.225(7) . ?
O11 H11 0.8200 . ?
O11 C16 1.313(7) . ?
O204 C203 1.152(7) . ?
O5 C5 1.154(7) . ?
O121 H121 0.8200 . ?
O121 C126 1.335(7) . ?
N221 N203 1.381(5) . ?
N221 C222 1.317(6) . ?
O312 C316 1.216(7) . ?
O22 C26 1.217(7) . ?
O12 C16 1.214(7) . ?
O311 H311 0.8200 . ?
O311 C316 1.316(7) . ?
O304 C304 1.141(7) . ?
N22 N21 1.369(6) . ?
N22 C1 1.458(6) . ?
N22 C24 1.335(7) . ?
N11 N12 1.367(6) . ?
N11 C12 1.332(6) . ?
O112 C116 1.213(6) . ?
O221 H221 0.8200 . ?
O221 C226 1.326(6) . ?
O21 H21 0.8200 . ?
O21 C26 1.315(7) . ?
O211 C216 1.316(7) . ?
O211 H211 0.82(8) . ?
N321 N322 1.376(6) . ?
N321 C322 1.322(7) . ?
N203 C224 1.335(6) . ?
N203 C201 1.455(6) . ?
O2 C2 1.215(6) . ?
N12 C14 1.342(6) . ?
N12 C1 1.460(6) . ?
N212 N211 1.380(5) . ?
N212 C201 1.457(6) . ?
N212 C214 1.326(7) . ?
N21 C22 1.320(7) . ?
O122 C126 1.217(7) . ?
O3 C3 1.142(7) . ?
O206 C205 1.130(7) . ?
O103 C103 1.144(7) . ?
O322 C326 1.206(7) . ?
N111 N112 1.373(5) . ?
N111 C112 1.319(7) . ?
O303 C303 1.134(8) . ?
O105 C105 1.142(8) . ?
O305 C305 1.128(7) . ?
N112 C114 1.340(6) . ?
N112 C101 1.447(6) . ?
O104 C104 1.142(7) . ?
N211 C212 1.316(7) . ?
N312 N311 1.388(6) . ?
N312 C314 1.342(7) . ?
N312 C301 1.438(7) . ?
N122 N121 1.377(6) . ?
N122 C101 1.468(6) . ?
N122 C124 1.336(7) . ?
N121 C122 1.317(7) . ?
N311 C312 1.324(7) . ?
N322 C324 1.342(7) . ?
N322 C301 1.451(6) . ?
O7 H7A 0.8512 . ?
O7 H7B 0.8508 . ?
C324 H324 0.9300 . ?
C324 C323 1.372(7) . ?
C224 H224 0.9300 . ?
C224 C223 1.381(7) . ?
C202 C201 1.549(7) . ?
C114 H114 0.9300 . ?
C114 C113 1.379(7) . ?
C23 C26 1.468(8) . ?
C23 C24 1.373(7) . ?
C23 C22 1.410(8) . ?
C222 H222 0.9300 . ?
C222 C223 1.408(7) . ?
C323 C322 1.405(8) . ?
C323 C326 1.466(7) . ?
C102 C101 1.547(7) . ?
C116 C113 1.474(7) . ?
C113 C112 1.406(7) . ?
C223 C226 1.471(7) . ?
C314 H314 0.9300 . ?
C314 C313 1.364(7) . ?
C13 C14 1.382(7) . ?
C13 C16 1.468(7) . ?
C13 C12 1.404(7) . ?
C101 H101 0.9800 . ?
C302 C301 1.545(7) . ?
C14 H14 0.9300 . ?
C2 C1 1.552(7) . ?
C301 H301 0.9800 . ?
C1 H1 0.9800 . ?
C313 C316 1.480(8) . ?
C313 C312 1.403(8) . ?
C212 H212 0.9300 . ?
C212 C213 1.406(7) . ?
C12 H12 0.9300 . ?
C322 H322 0.9300 . ?
C122 H122 0.9300 . ?
C122 C123 1.399(8) . ?
C24 H24 0.9300 . ?
C201 H201 0.9800 . ?
C216 C213 1.463(8) . ?
C213 C214 1.377(7) . ?
C214 H214 0.9300 . ?
C112 H112 0.9300 . ?
C22 H22 0.9300 . ?
C126 C123 1.465(8) . ?
C124 H124 0.9300 . ?
C124 C123 1.369(7) . ?
C312 H312 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re3 O201 C202 O202 169.7(3) . . . . ?
Re3 O201 C202 C201 -11.1(6) . . . . ?
Re3 N221 N203 C224 166.1(3) . . . . ?
Re3 N221 N203 C201 -9.8(6) . . . . ?
Re3 N221 C222 C223 -164.1(4) . . . . ?
Re3 N211 C212 C213 177.7(4) . . . . ?
Re1 O1 C2 O2 -173.4(4) . . . . ?
Re1 O1 C2 C1 7.9(6) . . . . ?
Re1 N11 N12 C14 -167.7(3) . . . . ?
Re1 N11 N12 C1 4.0(5) . . . . ?
Re1 N11 C12 C13 165.4(3) . . . . ?
Re1 N21 C22 C23 177.6(4) . . . . ?
Re2 O101 C102 O102 -177.9(3) . . . . ?
Re2 O101 C102 C101 2.1(6) . . . . ?
Re2 N111 N112 C114 -171.6(3) . . . . ?
Re2 N111 N112 C101 -1.5(6) . . . . ?
Re2 N111 C112 C113 170.5(4) . . . . ?
Re2 N121 C122 C123 -176.0(4) . . . . ?
Re4 O301 C302 O302 172.7(4) . . . . ?
Re4 O301 C302 C301 -10.9(6) . . . . ?
Re4 N321 N322 C324 174.4(3) . . . . ?
Re4 N321 N322 C301 -0.4(6) . . . . ?
Re4 N321 C322 C323 -173.1(4) . . . . ?
Re4 N311 C312 C313 -164.2(4) . . . . ?
O201 C202 C201 N203 67.9(5) . . . . ?
O201 C202 C201 N212 -53.5(5) . . . . ?
O1 C2 C1 N22 56.2(6) . . . . ?
O1 C2 C1 N12 -65.7(6) . . . . ?
O302 C302 C301 N312 121.4(5) . . . . ?
O302 C302 C301 N322 -115.9(5) . . . . ?
O202 C202 C201 N203 -112.9(5) . . . . ?
O202 C202 C201 N212 125.8(4) . . . . ?
O101 C102 C101 N112 -62.2(5) . . . . ?
O101 C102 C101 N122 59.1(5) . . . . ?
O102 C102 C101 N112 117.8(5) . . . . ?
O102 C102 C101 N122 -120.9(5) . . . . ?
O301 C302 C301 N312 -55.2(6) . . . . ?
O301 C302 C301 N322 67.4(6) . . . . ?
O111 C116 C113 C114 12.1(8) . . . . ?
O111 C116 C113 C112 -175.0(5) . . . . ?
O212 C216 C213 C212 -8.8(9) . . . . ?
O212 C216 C213 C214 -173.3(5) . . . . ?
O121 C126 C123 C122 -177.0(5) . . . . ?
O121 C126 C123 C124 0.4(8) . . . . ?
N221 N203 C224 C223 1.2(6) . . . . ?
N221 N203 C201 N212 68.2(5) . . . . ?
N221 N203 C201 C202 -53.8(5) . . . . ?
N221 C222 C223 C224 -1.0(6) . . . . ?
N221 C222 C223 C226 175.3(5) . . . . ?
N22 N21 C22 C23 -0.9(6) . . . . ?
N11 N12 C14 C13 0.5(5) . . . . ?
N11 N12 C1 N22 -64.6(5) . . . . ?
N11 N12 C1 C2 57.9(5) . . . . ?
O112 C116 C113 C114 -166.0(5) . . . . ?
O112 C116 C113 C112 6.9(9) . . . . ?
O211 C216 C213 C212 171.1(5) . . . . ?
O211 C216 C213 C214 6.6(8) . . . . ?
N321 N322 C324 C323 -0.8(6) . . . . ?
N321 N322 C301 N312 61.6(6) . . . . ?
N321 N322 C301 C302 -59.5(6) . . . . ?
N203 N221 C222 C223 1.7(6) . . . . ?
N203 C224 C223 C222 -0.2(6) . . . . ?
N203 C224 C223 C226 -176.1(5) . . . . ?
O2 C2 C1 N22 -122.5(5) . . . . ?
O2 C2 C1 N12 115.6(5) . . . . ?
N12 N11 C12 C13 -0.2(5) . . . . ?
N212 N211 C212 C213 -0.6(6) . . . . ?
N21 N22 C1 N12 60.5(5) . . . . ?
N21 N22 C1 C2 -63.0(6) . . . . ?
N21 N22 C24 C23 -1.4(5) . . . . ?
O122 C126 C123 C122 0.0(9) . . . . ?
O122 C126 C123 C124 177.3(6) . . . . ?
N111 N112 C114 C113 -0.9(6) . . . . ?
N111 N112 C101 N122 -61.5(6) . . . . ?
N111 N112 C101 C102 60.7(6) . . . . ?
N112 N111 C112 C113 0.2(6) . . . . ?
N112 C114 C113 C116 175.2(5) . . . . ?
N112 C114 C113 C112 1.0(6) . . . . ?
N211 N212 C201 N203 -59.2(5) . . . . ?
N211 N212 C201 C202 62.1(5) . . . . ?
N211 N212 C214 C213 -0.5(6) . . . . ?
N211 C212 C213 C216 -166.6(5) . . . . ?
N211 C212 C213 C214 0.3(6) . . . . ?
N312 N311 C312 C313 2.1(5) . . . . ?
N312 C314 C313 C316 -177.6(5) . . . . ?
N312 C314 C313 C312 -0.2(6) . . . . ?
N122 N121 C122 C123 0.9(6) . . . . ?
N122 C124 C123 C122 -0.6(6) . . . . ?
N122 C124 C123 C126 -178.4(5) . . . . ?
N121 N122 C101 N112 67.5(5) . . . . ?
N121 N122 C101 C102 -55.0(5) . . . . ?
N121 N122 C124 C123 1.2(6) . . . . ?
N121 C122 C123 C126 177.7(5) . . . . ?
N121 C122 C123 C124 -0.2(6) . . . . ?
N311 N312 C314 C313 1.6(5) . . . . ?
N311 N312 C301 N322 -61.0(5) . . . . ?
N311 N312 C301 C302 61.5(6) . . . . ?
N322 N321 C322 C323 -0.9(6) . . . . ?
N322 C324 C323 C322 0.2(6) . . . . ?
N322 C324 C323 C326 -173.8(5) . . . . ?
C324 N322 C301 N312 -112.0(6) . . . . ?
C324 N322 C301 C302 126.9(5) . . . . ?
C324 C323 C322 N321 0.4(6) . . . . ?
C324 C323 C326 O321 -16.9(8) . . . . ?
C324 C323 C326 O322 162.6(6) . . . . ?
C224 N203 C201 N212 -106.8(6) . . . . ?
C224 N203 C201 C202 131.2(5) . . . . ?
C224 C223 C226 O222 175.4(6) . . . . ?
C224 C223 C226 O221 -3.7(8) . . . . ?
C114 N112 C101 N122 106.5(5) . . . . ?
C114 N112 C101 C102 -131.2(5) . . . . ?
C114 C113 C112 N111 -0.8(6) . . . . ?
C222 N221 N203 C224 -1.8(6) . . . . ?
C222 N221 N203 C201 -177.7(4) . . . . ?
C222 C223 C226 O222 0.2(8) . . . . ?
C222 C223 C226 O221 -179.0(5) . . . . ?
C116 C113 C112 N111 -174.8(5) . . . . ?
C314 N312 N311 Re4 167.2(3) . . . . ?
C314 N312 N311 C312 -2.3(5) . . . . ?
C314 N312 C301 N322 132.8(5) . . . . ?
C314 N312 C301 C302 -104.6(5) . . . . ?
C314 C313 C316 O312 9.9(8) . . . . ?
C314 C313 C316 O311 -171.0(5) . . . . ?
C314 C313 C312 N311 -1.2(6) . . . . ?
C101 N112 C114 C113 -169.8(5) . . . . ?
C101 N122 N121 Re2 -7.4(6) . . . . ?
C101 N122 N121 C122 175.2(4) . . . . ?
C101 N122 C124 C123 -174.8(5) . . . . ?
C14 N12 C1 N22 105.4(5) . . . . ?
C14 N12 C1 C2 -132.1(5) . . . . ?
C14 C13 C16 O11 18.9(7) . . . . ?
C14 C13 C16 O12 -160.5(5) . . . . ?
C14 C13 C12 N11 0.5(6) . . . . ?
C16 C13 C14 N12 175.1(5) . . . . ?
C16 C13 C12 N11 -175.4(5) . . . . ?
C301 N312 N311 Re4 -1.1(5) . . . . ?
C301 N312 N311 C312 -170.6(4) . . . . ?
C301 N312 C314 C313 169.0(4) . . . . ?
C301 N322 C324 C323 173.1(5) . . . . ?
C1 N22 N21 Re1 3.7(5) . . . . ?
C1 N22 N21 C22 -177.6(4) . . . . ?
C1 N22 C24 C23 177.5(4) . . . . ?
C1 N12 C14 C13 -170.0(5) . . . . ?
C212 C213 C214 N212 0.1(6) . . . . ?
C12 N11 N12 C14 -0.2(5) . . . . ?
C12 N11 N12 C1 171.5(4) . . . . ?
C12 C13 C14 N12 -0.6(5) . . . . ?
C12 C13 C16 O11 -166.2(5) . . . . ?
C12 C13 C16 O12 14.3(8) . . . . ?
C322 N321 N322 C324 1.1(6) . . . . ?
C322 N321 N322 C301 -173.7(4) . . . . ?
C322 C323 C326 O321 170.0(5) . . . . ?
C322 C323 C326 O322 -10.5(9) . . . . ?
C26 C23 C24 N22 -178.5(5) . . . . ?
C26 C23 C22 N21 179.3(5) . . . . ?
C24 N22 N21 Re1 -177.3(3) . . . . ?
C24 N22 N21 C22 1.4(5) . . . . ?
C24 N22 C1 N12 -118.3(5) . . . . ?
C24 N22 C1 C2 118.2(5) . . . . ?
C24 C23 C26 O22 -3.2(9) . . . . ?
C24 C23 C26 O21 176.4(5) . . . . ?
C24 C23 C22 N21 0.1(6) . . . . ?
C201 N203 C224 C223 176.5(5) . . . . ?
C201 N212 N211 Re3 -5.3(6) . . . . ?
C201 N212 N211 C212 173.3(4) . . . . ?
C201 N212 C214 C213 -172.2(5) . . . . ?
C216 C213 C214 N212 167.3(5) . . . . ?
C214 N212 N211 Re3 -177.9(3) . . . . ?
C214 N212 N211 C212 0.7(5) . . . . ?
C214 N212 C201 N203 112.0(5) . . . . ?
C214 N212 C201 C202 -126.8(5) . . . . ?
C112 N111 N112 C114 0.4(6) . . . . ?
C112 N111 N112 C101 170.5(5) . . . . ?
C22 C23 C26 O22 177.7(5) . . . . ?
C22 C23 C26 O21 -2.7(9) . . . . ?
C22 C23 C24 N22 0.8(6) . . . . ?
C316 C313 C312 N311 175.9(5) . . . . ?
C326 C323 C322 N321 175.0(5) . . . . ?
C124 N122 N121 Re2 176.1(3) . . . . ?
C124 N122 N121 C122 -1.3(6) . . . . ?
C124 N122 C101 N112 -116.8(5) . . . . ?
C124 N122 C101 C102 120.7(5) . . . . ?
C312 C313 C316 O312 -166.7(6) . . . . ?
C312 C313 C316 O311 12.3(8) . . . . ?
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
1.0000 -1.0000 -2.0000 -0.0503 -0.2175 0.0974
-1.6114 9.4937 -1.7922 -0.0647 0.8244 0.5622
1.0000 -2.0000 -1.0000 -0.0383 -0.2540 -0.0186
-0.0000 1.0000 -2.0000 0.0058 -0.0287 0.1838
0.0000 -1.0000 2.0000 -0.0058 0.0287 -0.1838
1.0000 -2.0000 0.0000 -0.0561 -0.1889 -0.0865
-2.0000 -0.0000 1.0000 0.2136 0.0366 -0.0871
1.0000 1.0000 -0.0000 -0.1455 0.1158 0.0576
0.0000 2.0000 -1.0000 -0.0418 0.1380 0.1640
-3.3120 9.7758 -4.0595 0.1640 0.6812 0.7135
-2.0371 -8.2074 4.2264 0.4051 -0.5873 -0.7007
-2.7485 -2.0007 -7.8259 0.5170 -0.7519 0.4091
2.0000 -1.0000 -0.0000 -0.2016 -0.0731 -0.0289
1.0000 -0.0000 -2.0000 -0.0801 -0.1160 0.1454
-8.5984 6.7131 -0.1644 0.7975 0.5485 0.2513
