# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_buni210204a
_database_code_depnum_ccdc_archive 'CCDC 2130703'
loop_
_audit_author_name
_audit_author_address
'Michaela Reil'
;Friedrich Alexander University Erlangen Nurnberg
Germany
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_audit_creation_date             2022-03-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N4 O6, 1(C4 H8 O)'
_chemical_formula_sum            'C14 H16 N4 O7'
_chemical_formula_weight         352.31
_chemical_melting_point          ?
_chemical_oxdiff_formula         C14H12N4O7
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.8518(3)
_cell_length_b                   15.4697(4)
_cell_length_c                   13.9712(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.252(2)
_cell_angle_gamma                90
_cell_volume                     3371.35(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.2610
_cell_measurement_theta_min      4.2740
_shelx_estimated_absorpt_T_max   0.910
_shelx_estimated_absorpt_T_min   0.669
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -2 0.1529
1 1 0 0.1531
-2 1 0 0.1440
0 10 -1 0.0601
3 9 -4 0.0521
6 5 -6 0.0562
5 -9 0 0.0847
2 -10 -3 0.0206
-2 -10 2 0.0313
-1 0 -1 0.1646
-1 -2 1 0.0495
-2 0 -1 0.1581
-6 -5 6 0.0623
-7 -2 7 0.0792
-2 1 -2 0.1636
7 -1 -8 0.0338
-1 1 1 0.0888

_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.099
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 0.0061 0.0100 0.2785
1.0000 1.0000 0.0000 -0.1354 -0.0353 -0.0094
-2.0000 1.0000 -0.0000 0.0151 0.1806 0.1271
0.1666 9.9633 -1.1726 -0.8333 0.2951 0.4675
3.0217 8.9485 -3.5761 -0.8405 -0.0661 0.5377
6.1403 5.4498 -6.2391 -0.6440 -0.5500 0.5319
5.1911 -8.6102 0.1046 0.4712 -0.6837 -0.5572
1.7039 -9.5623 -2.5654 0.7823 -0.5993 -0.1700
-1.9289 -9.6739 2.0429 0.8791 -0.1147 -0.4626
-1.0000 -0.0000 -1.0000 0.0708 0.0227 0.1440
-1.0000 -2.0000 1.0000 0.2000 0.0480 -0.1252
-2.0000 0.0000 -1.0000 0.1209 0.0946 0.1895
-5.9409 -5.4618 6.3678 0.6323 0.5415 -0.5540
-6.8170 -2.1470 7.4722 0.3710 0.7804 -0.5033
-2.0000 1.0000 -2.0000 0.0563 0.0819 0.3240
7.0532 -0.9191 -7.5459 -0.1201 -0.9133 0.3891
-1.0000 1.0000 1.0000 -0.0557 0.1579 -0.0169

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9810
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.726
_diffrn_reflns_theta_min         4.025
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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    3.00    --  -41.48 -38.00 -90.00   99
  2  ω    -87.00  -6.00   1.00    3.00    --  -41.48 125.00  60.00   81
  3  ω     31.00 112.00   1.00    9.00    --  104.33-125.00 -90.00   81
  4  ω     31.00 130.00   1.00    9.00    --  104.33 -45.00 -60.00   99
  5  ω     97.00 178.00   1.00    9.00    --  104.33 125.00  90.00   81
  6  ω    103.00 178.00   1.00    9.00    --  104.33  77.00 -30.00   75
  7  ω    103.00 178.00   1.00    9.00    --  104.33  77.00  30.00   75
  8  ω     28.00 137.00   1.00    9.00    --  104.33 -77.00 -90.00  109
  9  ω     76.00 178.00   1.00    9.00    --  104.33  30.00-180.00  102
 10  ω   -116.00 -65.00   1.00    3.00    --  -41.48 -38.00   0.00   51
 11  ω     13.00 114.00   1.00    3.00    --   41.48  57.00 120.00  101
;
_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      -0.0501663000
_diffrn_orient_matrix_UB_12      -0.0852200000
_diffrn_orient_matrix_UB_13      -0.0205984000
_diffrn_orient_matrix_UB_21      -0.0719660000
_diffrn_orient_matrix_UB_22      0.0366210000
_diffrn_orient_matrix_UB_23      0.0493080000
_diffrn_orient_matrix_UB_31      -0.0454852000
_diffrn_orient_matrix_UB_32      0.0360955000
_diffrn_orient_matrix_UB_33      -0.0984805000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2949
_reflns_number_total             3302
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3302
_refine_ls_number_restraints     296
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+4.7913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1345
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C32-C31 = C32-C33
 1.44 with sigma of 0.02
 C31-O3 = C34-C33
 1.53 with sigma of 0.02
 O3-C34
 1.54 with sigma of 0.02
 O5-C51 = O5-C54
 1.44 with sigma of 0.02
 C51-C52 = C53-C54
 1.53 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 C32-O3 = C32-C34 = C31-C34 = O3-C33
 2.38 with sigma of 0.04
 O5-C52 = O5-C53 = C51-C53 = C52-C54
 2.38 with sigma of 0.04
 O3-C33 \\sim C31-C34
 with sigma of 0.04
 C32-O3 \\sim C32-C34
 with sigma of 0.04
 C31-O3 \\sim O3-C34 \\sim C34-C33
 with sigma of 0.02
 C32-C31 \\sim C32-C33
 with sigma of 0.02
 C51-C52 \\sim C52-C53 \\sim C53-C54
 with sigma of 0.02
 O5-C52 \\sim O5-C53
 with sigma of 0.04
 O5-C51 \\sim O5-C54
 with sigma of 0.02
 C52-C54 \\sim C51-C53
 with sigma of 0.04
3. Rigid bond restraints
 C44, O4, C41, C42, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C2, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, C2, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C32 \\sim C31 \\sim O3 \\sim C34 \\sim C33: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O5 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C44 \\sim O4 \\sim C41 \\sim C42 \\sim C43: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1 \\sim C2 \\sim O2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(O5) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.1
Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(C44) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Rigid body (RIGU) restrains
 C32, C31, O3, C34, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(C32)+Sof(H32a)+Sof(H32b)+Sof(C31)+Sof(H31a)+Sof(H31b)+Sof(O3)+Sof(C34)+
 Sof(H34a)+Sof(H34b)+Sof(C33)+Sof(H33a)+Sof(H33b)]+1*[Sof(O5)+Sof(C51)+
 Sof(H51a)+Sof(H51b)+Sof(C52)+Sof(H52a)+Sof(H52b)+Sof(C53)+Sof(H53a)+Sof(H53b)+
 Sof(C54)+Sof(H54a)+Sof(H54b)]+1*[Sof(C44)+Sof(H44a)+Sof(H44b)+Sof(O4)+Sof(C41)+
 Sof(H41a)+Sof(H41b)+Sof(C42)+Sof(H42a)+Sof(H42b)+Sof(C43)+Sof(H43a)+Sof(H43b)]=
 1 with esd of 0.001
 Sof(C32)=Sof(H32a)=Sof(H32b)=Sof(C31)=Sof(H31a)=Sof(H31b)=Sof(O3)=Sof(C34)=
 Sof(H34a)=Sof(H34b)=Sof(C33)=Sof(H33a)=Sof(H33b)=FVAR(1)
 Sof(O5)=Sof(C51)=Sof(H51a)=Sof(H51b)=Sof(C52)=Sof(H52a)=Sof(H52b)=Sof(C53)=
 Sof(H53a)=Sof(H53b)=Sof(C54)=Sof(H54a)=Sof(H54b)=FVAR(2)
 Sof(C44)=Sof(H44a)=Sof(H44b)=Sof(O4)=Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(C42)=
 Sof(H42a)=Sof(H42b)=Sof(C43)=Sof(H43a)=Sof(H43b)=FVAR(3)
 Sof(H1)=1-FVAR(4)
 Sof(H2)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C1(H1a)
7.b Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C31(H31a,H31b), C34(H34a,H34b), C33(H33a,H33b), C51(H51a,
 H51b), C52(H52a,H52b), C53(H53a,H53b), C54(H54a,H54b), C44(H44a,H44b),
 C41(H41a,H41b), C42(H42a,H42b), C43(H43a,H43b)
7.c Aromatic/amide H refined with riding coordinates:
 C22(H22)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O11 O 0.64525(9) 0.71184(9) 0.61144(9) 0.0318(3) Uani 1 1 d . . . . .
O21 O 0.36019(8) 0.53120(9) 0.00646(9) 0.0307(3) Uani 1 1 d . . . . .
O12 O 0.63929(9) 0.84659(9) 0.55112(9) 0.0321(3) Uani 1 1 d . . . . .
O22 O 0.28238(8) 0.49047(10) 0.11800(9) 0.0343(3) Uani 1 1 d . . . . .
O2 O 0.76914(9) 0.50712(11) 0.38141(11) 0.0432(4) Uani 1 1 d . U . . .
N12 N 0.65384(9) 0.63718(9) 0.32881(10) 0.0231(3) Uani 1 1 d . . . . .
N22 N 0.56227(9) 0.53238(10) 0.23987(10) 0.0265(3) Uani 1 1 d . . . . .
N11 N 0.65013(10) 0.71684(10) 0.28675(10) 0.0281(3) Uani 1 1 d . . . . .
O1 O 0.69004(13) 0.41453(11) 0.27996(15) 0.0597(5) Uani 1 1 d . U . . .
N21 N 0.52149(11) 0.50152(12) 0.31098(11) 0.0368(4) Uani 1 1 d . . . . .
C14 C 0.65055(10) 0.64218(12) 0.42452(12) 0.0241(4) Uani 1 1 d . . . . .
C24 C 0.51054(11) 0.53950(12) 0.15316(12) 0.0249(4) Uani 1 1 d . . . . .
C13 C 0.64595(11) 0.72829(12) 0.44622(12) 0.0258(4) Uani 1 1 d . . . . .
C1 C 0.65012(10) 0.56151(12) 0.26744(12) 0.0246(4) Uani 1 1 d . . . . .
H1A H 0.671101 0.578519 0.206716 0.029 Uiso 1 1 calc R U . . .
C16 C 0.64322(11) 0.76875(12) 0.54051(12) 0.0261(4) Uani 1 1 d . . . . .
C23 C 0.43083(11) 0.51198(12) 0.16670(13) 0.0275(4) Uani 1 1 d . . . . .
C26 C 0.35158(11) 0.51005(12) 0.09529(13) 0.0276(4) Uani 1 1 d . . . . .
C12 C 0.64632(12) 0.77213(13) 0.35817(13) 0.0304(4) Uani 1 1 d . . . . .
C2 C 0.70840(13) 0.48922(14) 0.31637(15) 0.0362(4) Uani 1 1 d . U . . .
C22 C 0.44173(12) 0.48923(15) 0.26598(14) 0.0364(5) Uani 1 1 d . . . . .
H22 H 0.397153 0.467711 0.296723 0.044 Uiso 1 1 calc R U . . .
C32 C 0.4105(18) 0.7467(8) 0.5113(11) 0.072(4) Uani 0.439(5) 1 d D U P A 1
H32A H 0.461427 0.771919 0.553438 0.086 Uiso 0.439(5) 1 calc R U P A 1
H32B H 0.358060 0.764988 0.535094 0.086 Uiso 0.439(5) 1 calc R U P A 1
C31 C 0.4165(6) 0.6542(5) 0.5058(6) 0.084(2) Uani 0.439(5) 1 d D U P A 1
H31A H 0.477243 0.636340 0.512465 0.101 Uiso 0.439(5) 1 calc R U P A 1
H31B H 0.391887 0.626962 0.558742 0.101 Uiso 0.439(5) 1 calc R U P A 1
O3 O 0.3712(4) 0.6286(4) 0.4161(5) 0.090(2) Uani 0.439(5) 1 d D U P A 1
C34 C 0.3820(7) 0.6937(5) 0.3471(5) 0.094(3) Uani 0.439(5) 1 d D U P A 1
H34A H 0.327962 0.704419 0.300951 0.112 Uiso 0.439(5) 1 calc R U P A 1
H34B H 0.427572 0.677840 0.310169 0.112 Uiso 0.439(5) 1 calc R U P A 1
C33 C 0.4071(10) 0.7696(7) 0.4106(8) 0.085(4) Uani 0.439(5) 1 d D U P A 1
H33A H 0.463910 0.790765 0.401018 0.102 Uiso 0.439(5) 1 calc R U P A 1
H33B H 0.364962 0.816716 0.392580 0.102 Uiso 0.439(5) 1 calc R U P A 1
O5 O 0.2798(6) 0.7125(6) 0.3339(7) 0.075(3) Uani 0.267(5) 1 d D U P B 2
C51 C 0.3402(8) 0.7135(10) 0.2676(9) 0.087(3) Uani 0.267(5) 1 d D U P B 2
H51A H 0.325320 0.758786 0.217386 0.104 Uiso 0.267(5) 1 calc R U P B 2
H51B H 0.342088 0.656781 0.235312 0.104 Uiso 0.267(5) 1 calc R U P B 2
C52 C 0.4213(8) 0.7325(12) 0.3303(10) 0.094(4) Uani 0.267(5) 1 d D U P B 2
H52A H 0.433288 0.795272 0.330265 0.113 Uiso 0.267(5) 1 calc R U P B 2
H52B H 0.468615 0.701527 0.307274 0.113 Uiso 0.267(5) 1 calc R U P B 2
C53 C 0.4137(8) 0.7025(14) 0.4320(10) 0.105(4) Uani 0.267(5) 1 d D U P B 2
H53A H 0.450585 0.737673 0.482015 0.126 Uiso 0.267(5) 1 calc R U P B 2
H53B H 0.430210 0.640951 0.441611 0.126 Uiso 0.267(5) 1 calc R U P B 2
C54 C 0.3188(8) 0.7155(12) 0.4369(10) 0.085(4) Uani 0.267(5) 1 d D U P B 2
H54A H 0.296853 0.668548 0.473958 0.103 Uiso 0.267(5) 1 calc R U P B 2
H54B H 0.308719 0.771875 0.466402 0.103 Uiso 0.267(5) 1 calc R U P B 2
H11 H 0.6455(18) 0.7407(19) 0.669(2) 0.060(8) Uiso 1 1 d . . . . .
H24 H 0.5308(13) 0.5606(14) 0.0973(16) 0.028(5) Uiso 1 1 d . . . . .
H14 H 0.6526(13) 0.5926(14) 0.4635(15) 0.026(5) Uiso 1 1 d . . . . .
H12 H 0.6441(15) 0.8371(17) 0.3478(17) 0.042(6) Uiso 1 1 d . . . . .
C44 C 0.3389(7) 0.7570(7) 0.3630(9) 0.073(3) Uani 0.294(6) 1 d . U P C 3
H44A H 0.299878 0.806780 0.364090 0.087 Uiso 0.294(6) 1 calc R U P C 3
H44B H 0.339963 0.746004 0.293411 0.087 Uiso 0.294(6) 1 calc R U P C 3
O4 O 0.2967(6) 0.6913(5) 0.3898(7) 0.089(3) Uani 0.294(6) 1 d . U P C 3
C41 C 0.3464(10) 0.6663(9) 0.4886(10) 0.086(4) Uani 0.294(6) 1 d . U P C 3
H41A H 0.310271 0.668109 0.539438 0.103 Uiso 0.294(6) 1 calc R U P C 3
H41B H 0.372797 0.608308 0.487633 0.103 Uiso 0.294(6) 1 calc R U P C 3
C42 C 0.413(2) 0.7373(14) 0.5017(18) 0.061(4) Uani 0.294(6) 1 d . U P C 3
H42A H 0.469706 0.711829 0.527892 0.073 Uiso 0.294(6) 1 calc R U P C 3
H42B H 0.399151 0.779178 0.550166 0.073 Uiso 0.294(6) 1 calc R U P C 3
C43 C 0.4192(8) 0.7898(9) 0.3991(11) 0.053(3) Uani 0.294(6) 1 d . U P C 3
H43A H 0.420955 0.853513 0.405725 0.064 Uiso 0.294(6) 1 calc R U P C 3
H43B H 0.464928 0.768561 0.365200 0.064 Uiso 0.294(6) 1 calc R U P C 3
H1 H 0.725(4) 0.374(4) 0.316(4) 0.10(2) Uiso 0.71(5) 1 d . . P D 2
H2 H 0.804(5) 0.454(5) 0.391(5) 0.03(2) Uiso 0.29(5) 1 d . . P D 1
H21 H 0.313(2) 0.5175(18) -0.036(2) 0.056(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
O11 C16 1.322(2) . ?
O11 H11 0.91(3) . ?
O21 C26 1.314(2) . ?
O21 H21 0.89(3) . ?
O12 C16 1.216(2) . ?
O22 C26 1.233(2) . ?
O2 C2 1.232(3) . ?
O2 H2 0.99(8) . ?
N12 N11 1.362(2) . ?
N12 C14 1.350(2) . ?
N12 C1 1.446(2) . ?
N22 N21 1.364(2) . ?
N22 C24 1.341(2) . ?
N22 C1 1.449(2) . ?
N11 C12 1.324(2) . ?
O1 C2 1.275(3) . ?
O1 H1 0.93(6) . ?
N21 C22 1.322(2) . ?
C14 C13 1.371(3) . ?
C14 H14 0.94(2) . ?
C24 C23 1.378(2) . ?
C24 H24 0.95(2) . ?
C13 C16 1.466(2) . ?
C13 C12 1.406(2) . ?
C1 H1A 1.0000 . ?
C1 C2 1.532(3) . ?
C23 C26 1.459(2) . ?
C23 C22 1.412(3) . ?
C12 H12 1.02(3) . ?
C22 H22 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.438(13) . ?
C32 C33 1.443(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 O3 1.386(9) . ?
O3 C34 1.425(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.483(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O5 C51 1.445(12) . ?
O5 C54 1.462(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.451(12) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.520(12) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.532(12) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 O4 1.309(13) . ?
C44 C43 1.379(16) . ?
O4 C41 1.512(14) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.51(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.67(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?

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
C16 O11 H11 108.9(18) . . ?
C26 O21 H21 110.6(19) . . ?
C2 O2 H2 105(4) . . ?
N11 N12 C1 118.85(13) . . ?
C14 N12 N11 111.68(14) . . ?
C14 N12 C1 128.99(15) . . ?
N21 N22 C1 118.22(14) . . ?
C24 N22 N21 113.18(14) . . ?
C24 N22 C1 128.22(15) . . ?
C12 N11 N12 105.28(14) . . ?
C2 O1 H1 109(3) . . ?
C22 N21 N22 103.95(15) . . ?
N12 C14 C13 106.71(15) . . ?
N12 C14 H14 121.7(13) . . ?
C13 C14 H14 131.6(13) . . ?
N22 C24 C23 106.19(15) . . ?
N22 C24 H24 121.8(12) . . ?
C23 C24 H24 132.0(12) . . ?
C14 C13 C16 128.66(16) . . ?
C14 C13 C12 105.47(15) . . ?
C12 C13 C16 125.86(17) . . ?
N12 C1 N22 110.20(13) . . ?
N12 C1 H1A 107.8 . . ?
N12 C1 C2 111.63(14) . . ?
N22 C1 H1A 107.8 . . ?
N22 C1 C2 111.48(15) . . ?
C2 C1 H1A 107.8 . . ?
O11 C16 C13 112.87(16) . . ?
O12 C16 O11 124.27(16) . . ?
O12 C16 C13 122.86(16) . . ?
C24 C23 C26 127.69(16) . . ?
C24 C23 C22 104.90(15) . . ?
C22 C23 C26 127.36(16) . . ?
O21 C26 C23 114.79(15) . . ?
O22 C26 O21 123.45(17) . . ?
O22 C26 C23 121.76(16) . . ?
N11 C12 C13 110.84(17) . . ?
N11 C12 H12 122.5(14) . . ?
C13 C12 H12 126.7(14) . . ?
O2 C2 O1 126.2(2) . . ?
O2 C2 C1 119.68(19) . . ?
O1 C2 C1 114.00(18) . . ?
N21 C22 C23 111.77(16) . . ?
N21 C22 H22 124.1 . . ?
C23 C22 H22 124.1 . . ?
H32A C32 H32B 109.4 . . ?
C31 C32 H32A 111.7 . . ?
C31 C32 H32B 111.7 . . ?
C31 C32 C33 100.5(11) . . ?
C33 C32 H32A 111.7 . . ?
C33 C32 H32B 111.7 . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
O3 C31 C32 107.7(9) . . ?
O3 C31 H31A 110.2 . . ?
O3 C31 H31B 110.2 . . ?
C31 O3 C34 107.8(6) . . ?
O3 C34 H34A 111.4 . . ?
O3 C34 H34B 111.4 . . ?
O3 C34 C33 101.9(6) . . ?
H34A C34 H34B 109.3 . . ?
C33 C34 H34A 111.4 . . ?
C33 C34 H34B 111.4 . . ?
C32 C33 C34 110.4(9) . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
C34 C33 H33A 109.6 . . ?
C34 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C51 O5 C54 114.7(10) . . ?
O5 C51 H51A 111.1 . . ?
O5 C51 H51B 111.1 . . ?
O5 C51 C52 103.4(9) . . ?
H51A C51 H51B 109.0 . . ?
C52 C51 H51A 111.1 . . ?
C52 C51 H51B 111.1 . . ?
C51 C52 H52A 110.3 . . ?
C51 C52 H52B 110.3 . . ?
C51 C52 C53 107.1(10) . . ?
H52A C52 H52B 108.6 . . ?
C53 C52 H52A 110.3 . . ?
C53 C52 H52B 110.3 . . ?
C52 C53 H53A 110.9 . . ?
C52 C53 H53B 110.9 . . ?
C52 C53 C54 104.1(9) . . ?
H53A C53 H53B 109.0 . . ?
C54 C53 H53A 110.9 . . ?
C54 C53 H53B 110.9 . . ?
O5 C54 C53 101.4(9) . . ?
O5 C54 H54A 111.5 . . ?
O5 C54 H54B 111.5 . . ?
C53 C54 H54A 111.5 . . ?
C53 C54 H54B 111.5 . . ?
H54A C54 H54B 109.3 . . ?
H44A C44 H44B 105.6 . . ?
O4 C44 H44A 104.3 . . ?
O4 C44 H44B 104.3 . . ?
O4 C44 C43 131.9(12) . . ?
C43 C44 H44A 104.3 . . ?
C43 C44 H44B 104.3 . . ?
C44 O4 C41 104.4(8) . . ?
O4 C41 H41A 111.9 . . ?
O4 C41 H41B 111.9 . . ?
H41A C41 H41B 109.6 . . ?
C42 C41 O4 99.4(12) . . ?
C42 C41 H41A 111.9 . . ?
C42 C41 H41B 111.9 . . ?
C41 C42 H42A 108.9 . . ?
C41 C42 H42B 108.9 . . ?
C41 C42 C43 113.4(16) . . ?
H42A C42 H42B 107.7 . . ?
C43 C42 H42A 108.9 . . ?
C43 C42 H42B 108.9 . . ?
C44 C43 C42 86.8(14) . . ?
C44 C43 H43A 114.2 . . ?
C44 C43 H43B 114.2 . . ?
C42 C43 H43A 114.2 . . ?
C42 C43 H43B 114.2 . . ?
H43A C43 H43B 111.4 . . ?

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
N12 N11 C12 C13 -1.1(2) . . . . ?
N12 C14 C13 C16 -178.36(16) . . . . ?
N12 C14 C13 C12 0.31(19) . . . . ?
N12 C1 C2 O2 -22.6(2) . . . . ?
N12 C1 C2 O1 160.92(17) . . . . ?
N22 N21 C22 C23 -0.1(2) . . . . ?
N22 C24 C23 C26 177.68(18) . . . . ?
N22 C24 C23 C22 0.0(2) . . . . ?
N22 C1 C2 O2 -146.29(18) . . . . ?
N22 C1 C2 O1 37.2(2) . . . . ?
N11 N12 C14 C13 -1.02(19) . . . . ?
N11 N12 C1 N22 -92.40(17) . . . . ?
N11 N12 C1 C2 143.15(15) . . . . ?
N21 N22 C24 C23 0.0(2) . . . . ?
N21 N22 C1 N12 -65.9(2) . . . . ?
N21 N22 C1 C2 58.6(2) . . . . ?
C14 N12 N11 C12 1.32(19) . . . . ?
C14 N12 C1 N22 78.9(2) . . . . ?
C14 N12 C1 C2 -45.6(2) . . . . ?
C14 C13 C16 O11 -0.3(3) . . . . ?
C14 C13 C16 O12 179.86(17) . . . . ?
C14 C13 C12 N11 0.5(2) . . . . ?
C24 N22 N21 C22 0.0(2) . . . . ?
C24 N22 C1 N12 106.5(2) . . . . ?
C24 N22 C1 C2 -128.97(19) . . . . ?
C24 C23 C26 O21 5.5(3) . . . . ?
C24 C23 C26 O22 -174.03(19) . . . . ?
C24 C23 C22 N21 0.1(2) . . . . ?
C1 N12 N11 C12 174.02(15) . . . . ?
C1 N12 C14 C13 -172.79(15) . . . . ?
C1 N22 N21 C22 173.59(17) . . . . ?
C1 N22 C24 C23 -172.76(17) . . . . ?
C16 C13 C12 N11 179.22(16) . . . . ?
C26 C23 C22 N21 -177.66(19) . . . . ?
C12 C13 C16 O11 -178.72(16) . . . . ?
C12 C13 C16 O12 1.5(3) . . . . ?
C22 C23 C26 O21 -177.26(19) . . . . ?
C22 C23 C26 O22 3.2(3) . . . . ?
C32 C31 O3 C34 35.1(14) . . . . ?
C31 C32 C33 C34 19(2) . . . . ?
C31 O3 C34 C33 -21.0(11) . . . . ?
O3 C34 C33 C32 0.4(17) . . . . ?
C33 C32 C31 O3 -32.4(19) . . . . ?
O5 C51 C52 C53 25.1(18) . . . . ?
C51 O5 C54 C53 -9.5(17) . . . . ?
C51 C52 C53 C54 -32(2) . . . . ?
C52 C53 C54 O5 23.9(18) . . . . ?
C54 O5 C51 C52 -9.6(17) . . . . ?
C44 O4 C41 C42 4.1(18) . . . . ?
O4 C44 C43 C42 -19.9(19) . . . . ?
O4 C41 C42 C43 -15(2) . . . . ?
C41 C42 C43 C44 18.7(19) . . . . ?
C43 C44 O4 C41 13(2) . . . . ?

_olex2_date_sample_data_collection 2021-02-04
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.787
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_buni210308a
_database_code_depnum_ccdc_archive 'CCDC 2130704'
loop_
_audit_author_name
_audit_author_address
'Michaela Reil'
;Friedrich Alexander University Erlangen Nurnberg
Germany
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_buni210308a         
;
PROBLEM: Short Inter D...A Contact  O3       ..O3       .       2.82 Ang.
RESPONSE: After careful consideration of the short D...A contact between O3...O3 (2.82 Ang.), this alert was discarded as in the packing of the  solvent-free structure the molecules are very close to each other, thus rendering distances very short.
;
# Added during the CSD deposition process: Wednesday 16 March 2022 02:03 PM
# end Validation Reply Form

_audit_creation_date             2022-03-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H7 Mn N4 O9'
_chemical_formula_sum            'C13 H7 Mn N4 O9'
_chemical_formula_weight         418.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Mn Br Cl'
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'
Mn Mn -0.5299 2.8052 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.9306(5)
_cell_length_b                   5.6066(2)
_cell_length_c                   20.6630(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.404(4)
_cell_angle_gamma                90
_cell_volume                     1650.51(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2064
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      72.3240
_cell_measurement_theta_min      3.2100
_shelx_estimated_absorpt_T_max   0.810
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    7.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.278
_diffrn_reflns_theta_min         3.238
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  34.00   1.00    8.22    --  -40.61  38.00-180.00   99
  2  ω   -115.00 -16.00   1.00    8.22    --  -40.61 -38.00   0.00   99
  3  ω      6.00  82.00   1.00    8.22    --   40.61 -99.00 -60.00   76
  4  ω     22.00 106.00   1.00   32.91    --  104.57 -94.00 -60.00   84
  5  ω     79.00 178.00   1.00   32.91    --  104.57  45.00-150.00   99
  6  ω     32.00 130.00   1.00   32.91    --  104.57 -45.00-120.00   98
  7  ω    103.00 178.00   1.00   32.91    --  104.57  77.00 -30.00   75
  8  ω     28.00 109.00   1.00   32.91    --  104.57-111.00-120.00   81
  9  ω    104.00 178.00   1.00   32.91    --  104.57 111.00-120.00   74
 10  ω   -113.00 -12.00   1.00    8.22    --  -40.61 -57.00 120.00  101
;
_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      -0.1079782000
_diffrn_orient_matrix_UB_12      -0.0120367000
_diffrn_orient_matrix_UB_13      -0.0224052000
_diffrn_orient_matrix_UB_21      0.0045111000
_diffrn_orient_matrix_UB_22      -0.2737003000
_diffrn_orient_matrix_UB_23      -0.0048447000
_diffrn_orient_matrix_UB_31      0.0015837000
_diffrn_orient_matrix_UB_32      -0.0213253000
_diffrn_orient_matrix_UB_33      0.0746935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2540
_reflns_number_total             3171
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0382P)²+0.4141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0991
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C24(H24), C22(H22)
2.c Idealised tetrahedral OH refined as rotating group:
 O11(H11), O21(H21)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mn1 Mn 0.47317(3) 0.57119(9) 0.32798(2) 0.01929(13) Uani 1 1 d . . . . .
O1 O 0.55739(14) 0.8118(4) 0.29806(10) 0.0218(4) Uani 1 1 d . . . . .
O2 O 0.66813(14) 0.8802(4) 0.24745(11) 0.0246(5) Uani 1 1 d . . . . .
O5 O 0.30211(15) 0.8484(4) 0.26123(13) 0.0326(5) Uani 1 1 d . . . . .
O4 O 0.35804(17) 0.2159(4) 0.37244(12) 0.0338(5) Uani 1 1 d . . . . .
N12 N 0.65695(16) 0.3653(4) 0.33163(12) 0.0198(5) Uani 1 1 d . . . . .
N22 N 0.54795(16) 0.3730(4) 0.22141(12) 0.0196(5) Uani 1 1 d . . . . .
O3 O 0.49315(18) 0.7909(5) 0.46097(12) 0.0391(6) Uani 1 1 d . . . . .
N21 N 0.46770(16) 0.3978(4) 0.23949(12) 0.0209(5) Uani 1 1 d . . . . .
N11 N 0.59332(17) 0.3796(5) 0.36770(12) 0.0213(5) Uani 1 1 d . . . . .
O12 O 0.83533(19) -0.1434(6) 0.45700(14) 0.0547(9) Uani 1 1 d . . . . .
O11 O 0.7279(2) -0.1038(6) 0.51287(15) 0.0565(9) Uani 1 1 d . . . . .
H11 H 0.758412 -0.211532 0.536101 0.085 Uiso 1 1 calc R U . . .
O21 O 0.4391(2) -0.0559(7) 0.05122(15) 0.0581(9) Uani 1 1 d . . . . .
H21 H 0.405094 -0.131678 0.019323 0.087 Uiso 1 1 calc R U . . .
O22 O 0.3062(2) -0.0224(6) 0.08073(16) 0.0604(10) Uani 1 1 d . . . . .
C2 C 0.61943(19) 0.7486(5) 0.27070(15) 0.0196(6) Uani 1 1 d . . . . .
C1 C 0.63375(19) 0.4768(5) 0.26536(14) 0.0187(6) Uani 1 1 d . . . . .
H1 H 0.684943 0.448953 0.245661 0.022 Uiso 1 1 calc R U . . .
C14 C 0.7283(2) 0.2201(6) 0.36142(15) 0.0237(6) Uani 1 1 d . . . . .
H14 H 0.779064 0.183153 0.345961 0.028 Uiso 1 1 calc R U . . .
C12 C 0.6271(2) 0.2398(6) 0.42088(15) 0.0254(6) Uani 1 1 d . . . . .
H12 H 0.598625 0.214004 0.454588 0.031 Uiso 1 1 calc R U . . .
C24 C 0.5334(2) 0.2424(6) 0.16492(15) 0.0255(6) Uani 1 1 d . . . . .
H24 H 0.577841 0.201707 0.143497 0.031 Uiso 1 1 calc R U . . .
C22 C 0.4022(2) 0.2809(6) 0.19295(16) 0.0270(7) Uani 1 1 d . . . . .
H22 H 0.339868 0.267491 0.192312 0.032 Uiso 1 1 calc R U . . .
C13 C 0.7120(2) 0.1357(6) 0.41953(16) 0.0291(7) Uani 1 1 d . . . . .
C3 C 0.4863(2) 0.7162(6) 0.40900(17) 0.0254(7) Uani 1 1 d . . . . .
C4 C 0.4021(2) 0.3513(6) 0.35398(16) 0.0248(6) Uani 1 1 d . . . . .
C5 C 0.3692(2) 0.7435(6) 0.28715(16) 0.0250(7) Uani 1 1 d . . . . .
C23 C 0.4399(2) 0.1800(7) 0.14463(17) 0.0324(7) Uani 1 1 d . . . . .
C16 C 0.7647(2) -0.0479(8) 0.46509(18) 0.0390(9) Uani 1 1 d . . . . .
C26 C 0.3891(3) 0.0255(8) 0.08913(19) 0.0414(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mn1 O1 2.061(2) . ?
Mn1 N21 2.051(2) . ?
Mn1 N11 2.041(3) . ?
Mn1 C3 1.818(3) . ?
Mn1 C4 1.809(3) . ?
Mn1 C5 1.809(3) . ?
O1 C2 1.271(3) . ?
O2 C2 1.230(3) . ?
O5 C5 1.147(4) . ?
O4 C4 1.143(4) . ?
N12 N11 1.374(3) . ?
N12 C1 1.450(4) . ?
N12 C14 1.336(4) . ?
N22 N21 1.365(3) . ?
N22 C1 1.452(4) . ?
N22 C24 1.339(4) . ?
O3 C3 1.128(4) . ?
N21 C22 1.322(4) . ?
N11 C12 1.321(4) . ?
O12 C16 1.237(4) . ?
O11 H11 0.8200 . ?
O11 C16 1.305(4) . ?
O21 H21 0.8200 . ?
O21 C26 1.315(4) . ?
O22 C26 1.226(4) . ?
C2 C1 1.547(4) . ?
C1 H1 0.9800 . ?
C14 H14 0.9300 . ?
C14 C13 1.378(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.403(4) . ?
C24 H24 0.9300 . ?
C24 C23 1.377(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.403(4) . ?
C13 C16 1.457(5) . ?
C23 C26 1.456(5) . ?

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
N21 Mn1 O1 84.72(9) . . ?
N11 Mn1 O1 85.61(9) . . ?
N11 Mn1 N21 84.54(10) . . ?
C3 Mn1 O1 94.37(12) . . ?
C3 Mn1 N21 175.95(12) . . ?
C3 Mn1 N11 91.46(12) . . ?
C4 Mn1 O1 177.90(11) . . ?
C4 Mn1 N21 94.08(12) . . ?
C4 Mn1 N11 92.56(12) . . ?
C4 Mn1 C3 86.71(14) . . ?
C5 Mn1 O1 91.50(11) . . ?
C5 Mn1 N21 92.15(12) . . ?
C5 Mn1 N11 175.79(11) . . ?
C5 Mn1 C3 91.82(14) . . ?
C5 Mn1 C4 90.27(14) . . ?
C2 O1 Mn1 122.82(19) . . ?
N11 N12 C1 118.6(2) . . ?
C14 N12 N11 111.8(2) . . ?
C14 N12 C1 129.1(2) . . ?
N21 N22 C1 118.1(2) . . ?
C24 N22 N21 111.5(2) . . ?
C24 N22 C1 130.3(2) . . ?
N22 N21 Mn1 119.23(18) . . ?
C22 N21 Mn1 135.0(2) . . ?
C22 N21 N22 105.6(2) . . ?
N12 N11 Mn1 118.67(18) . . ?
C12 N11 Mn1 135.9(2) . . ?
C12 N11 N12 105.2(2) . . ?
C16 O11 H11 109.5 . . ?
C26 O21 H21 109.5 . . ?
O1 C2 C1 116.2(2) . . ?
O2 C2 O1 126.9(3) . . ?
O2 C2 C1 116.9(2) . . ?
N12 C1 N22 109.6(2) . . ?
N12 C1 C2 110.9(2) . . ?
N12 C1 H1 109.2 . . ?
N22 C1 C2 108.9(2) . . ?
N22 C1 H1 109.2 . . ?
C2 C1 H1 109.2 . . ?
N12 C14 H14 126.7 . . ?
N12 C14 C13 106.7(3) . . ?
C13 C14 H14 126.7 . . ?
N11 C12 H12 124.7 . . ?
N11 C12 C13 110.7(3) . . ?
C13 C12 H12 124.7 . . ?
N22 C24 H24 126.6 . . ?
N22 C24 C23 106.9(3) . . ?
C23 C24 H24 126.6 . . ?
N21 C22 H22 124.7 . . ?
N21 C22 C23 110.5(3) . . ?
C23 C22 H22 124.7 . . ?
C14 C13 C12 105.7(3) . . ?
C14 C13 C16 127.1(3) . . ?
C12 C13 C16 126.7(3) . . ?
O3 C3 Mn1 175.1(3) . . ?
O4 C4 Mn1 177.8(3) . . ?
O5 C5 Mn1 178.5(3) . . ?
C24 C23 C22 105.5(3) . . ?
C24 C23 C26 129.3(3) . . ?
C22 C23 C26 125.1(3) . . ?
O12 C16 O11 124.6(3) . . ?
O12 C16 C13 122.4(3) . . ?
O11 C16 C13 112.9(3) . . ?
O21 C26 C23 114.9(3) . . ?
O22 C26 O21 124.6(3) . . ?
O22 C26 C23 120.5(3) . . ?

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
Mn1 O1 C2 O2 174.9(2) . . . . ?
Mn1 O1 C2 C1 -4.2(4) . . . . ?
Mn1 N21 C22 C23 -175.2(2) . . . . ?
Mn1 N11 C12 C13 174.4(2) . . . . ?
O1 C2 C1 N12 -57.0(3) . . . . ?
O1 C2 C1 N22 63.6(3) . . . . ?
O2 C2 C1 N12 123.9(3) . . . . ?
O2 C2 C1 N22 -115.5(3) . . . . ?
N12 N11 C12 C13 0.1(4) . . . . ?
N12 C14 C13 C12 0.4(4) . . . . ?
N12 C14 C13 C16 172.8(4) . . . . ?
N22 N21 C22 C23 0.0(4) . . . . ?
N22 C24 C23 C22 -0.4(4) . . . . ?
N22 C24 C23 C26 -175.3(4) . . . . ?
N21 N22 C1 N12 62.0(3) . . . . ?
N21 N22 C1 C2 -59.5(3) . . . . ?
N21 N22 C24 C23 0.4(4) . . . . ?
N21 C22 C23 C24 0.2(4) . . . . ?
N21 C22 C23 C26 175.4(4) . . . . ?
N11 N12 C1 N22 -59.4(3) . . . . ?
N11 N12 C1 C2 60.9(3) . . . . ?
N11 N12 C14 C13 -0.3(4) . . . . ?
N11 C12 C13 C14 -0.3(4) . . . . ?
N11 C12 C13 C16 -172.8(4) . . . . ?
C1 N12 N11 Mn1 -3.1(3) . . . . ?
C1 N12 N11 C12 172.4(3) . . . . ?
C1 N12 C14 C13 -171.5(3) . . . . ?
C1 N22 N21 Mn1 -1.5(3) . . . . ?
C1 N22 N21 C22 -177.7(3) . . . . ?
C1 N22 C24 C23 177.4(3) . . . . ?
C14 N12 N11 Mn1 -175.3(2) . . . . ?
C14 N12 N11 C12 0.2(3) . . . . ?
C14 N12 C1 N22 111.3(3) . . . . ?
C14 N12 C1 C2 -128.5(3) . . . . ?
C14 C13 C16 O12 3.2(7) . . . . ?
C14 C13 C16 O11 -174.6(4) . . . . ?
C12 C13 C16 O12 174.2(4) . . . . ?
C12 C13 C16 O11 -3.7(6) . . . . ?
C24 N22 N21 Mn1 175.9(2) . . . . ?
C24 N22 N21 C22 -0.3(3) . . . . ?
C24 N22 C1 N12 -114.8(3) . . . . ?
C24 N22 C1 C2 123.7(3) . . . . ?
C24 C23 C26 O21 -3.7(7) . . . . ?
C24 C23 C26 O22 175.5(4) . . . . ?
C22 C23 C26 O21 -177.7(4) . . . . ?
C22 C23 C26 O22 1.5(7) . . . . ?

_olex2_date_sample_data_collection 2021-03-08
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.844
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_buni211203a
_database_code_depnum_ccdc_archive 'CCDC 2130706'
loop_
_audit_author_name
_audit_author_address
'Michaela Reil'
;Friedrich Alexander University Erlangen Nurnberg
Germany
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_buni211203a         
;
PROBLEM: Short Inter D-H..H-D       H7A      ..H311     .       1.92 Ang.
RESPONSE: After careful consideration, the short D-H..H-D interaction between H7A..H311 is deemed acceptable and inevitable due to the packing mode. 
;
_vrf_PLAT430_buni211203a         
;
PROBLEM: Short Inter D...A Contact  O105     ..O304     .       2.73 Ang.
RESPONSE: After careful consideration, the short inter D...A contact between O105 and O304 is deemed acceptable and inevitable due to the packing mode. 
;
# Added during the CSD deposition process: Wednesday 16 March 2022 02:03 PM
# end Validation Reply Form

_audit_creation_date             2022-03-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H7 N4 O9 Re, 0.5(H2 O)'
_chemical_formula_sum            'C13 H8 N4 O9.50 Re'
_chemical_formula_weight         558.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         C13H8N4O9.5Re
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.3811(5)
_cell_length_b                   15.1010(5)
_cell_length_c                   17.2257(6)
_cell_angle_alpha                107.251(3)
_cell_angle_beta                 94.748(3)
_cell_angle_gamma                110.515(3)
_cell_volume                     3272.3(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.2770
_cell_measurement_theta_min      3.3090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
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

_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.026
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

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10901
_reflns_number_total             12476
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.036
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_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_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) . . . . ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_buni210826a
_database_code_depnum_ccdc_archive 'CCDC 2130707'
loop_
_audit_author_name
_audit_author_address
'Michaela Reil'
;Friedrich Alexander University Erlangen Nurnberg
Germany
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_audit_creation_date             2022-03-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H7 Cl N4 O8 Ru, C H4 O'
_chemical_formula_sum            'C13 H11 Cl N4 O9 Ru'
_chemical_formula_weight         503.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         C13H11ClN4O9Ru
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'
Cl Cl 0.3639 0.7018 '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'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   33.2013(8)
_cell_length_b                   11.7943(3)
_cell_length_c                   10.7307(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.218(2)
_cell_angle_gamma                90
_cell_volume                     4177.27(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5011
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      72.2580
_cell_measurement_theta_min      3.9790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.726
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 2 0.1764
2 -1 -2 0.1527
2 0 -1 0.1664
0 0 1 0.1930
21 2 0 0.0777
-21 -2 0 0.0210
1 1 -2 0.1613
-1 -1 2 0.1860
0 1 -1 0.1391
1 -2 2 0.1562
2 1 0 0.0720
-1 1 -1 0.1196
1 -1 1 0.1575
-2 2 -1 0.0881
1 -2 1 0.1148
1 1 0 0.0663
-1 2 0 0.0498
-1 2 1 0.1009
-19 3 0 0.0156
-1 0 0 0.0092
0 -1 0 0.0258
1 0 0 0.0715

_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.081
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
-1.0001 1.0000 2.0000 0.1412 0.2323 -0.1606
2.0001 -1.0000 -2.0000 -0.1628 -0.2486 0.1225
2.0000 0.0000 -1.0000 -0.1377 -0.0855 0.0193
-0.0000 -0.0000 1.0000 0.0946 0.0528 -0.0954
20.6324 2.0653 -0.0122 -0.5895 -0.1106 -0.8002
-20.6424 -2.1182 0.1935 0.6105 0.1144 0.7837
1.0000 1.0000 -2.0000 -0.2802 -0.0116 0.1448
-1.0000 -1.0000 2.0000 0.2802 0.0116 -0.1448
-0.0000 1.0000 -1.0000 -0.1641 0.0576 0.0875
1.0000 -2.0000 2.0000 0.3066 -0.1315 -0.2130
2.0000 1.0000 0.0000 -0.1126 0.0776 -0.0840
-1.0000 1.0000 -1.0000 -0.1425 0.0739 0.1255
1.0000 -1.0000 1.0000 0.1425 -0.0739 -0.1255
-2.0000 2.0000 -1.0000 -0.1905 0.2007 0.1557
1.0000 -2.0000 1.0000 0.2121 -0.1843 -0.1176
1.0000 1.0000 0.0000 -0.0911 0.0940 -0.0459
-1.0001 2.0000 0.0000 -0.1175 0.2371 0.0223
-1.0001 2.0000 1.0000 -0.0229 0.2898 -0.0731
-19.1318 3.3969 -0.1296 0.1640 0.6812 0.7135
-1.0000 -0.0000 0.0000 0.0216 0.0164 0.0380
0.0000 -1.0000 -0.0000 0.0695 -0.1103 0.0079
1.0000 0.0000 -0.0000 -0.0216 -0.0164 -0.0380

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8112
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.544
_diffrn_reflns_theta_min         3.980
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -111.00 -14.00   1.00    1.97    --  -41.69 -57.00-120.00   97
  2  ω    -86.00  -6.00   1.00    1.97    --  -41.69 125.00 -60.00   80
  3  ω     41.00 106.00   1.00    7.86    --  104.37 -94.00  60.00   65
  4  ω    116.00 178.00   1.00    7.86    --  104.37  77.00  90.00   62
  5  ω    105.00 154.00   1.00    7.86    --  104.37  77.00   0.00   49
  6  ω     31.00 112.00   1.00    7.86    --  104.37-125.00-120.00   81
  7  ω     75.00 137.00   1.00    7.86    --  104.37 -77.00  60.00   62
  8  ω     64.00 118.00   1.00    7.86    --  104.37 -45.00 -90.00   54
  9  ω     79.00 165.00   1.00    7.86    --  104.37  45.00 150.00   86
;
_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      -0.0215555000
_diffrn_orient_matrix_UB_12      -0.0695173000
_diffrn_orient_matrix_UB_13      0.0945796000
_diffrn_orient_matrix_UB_21      -0.0163723000
_diffrn_orient_matrix_UB_22      0.1103431000
_diffrn_orient_matrix_UB_23      0.0527703000
_diffrn_orient_matrix_UB_31      -0.0380491000
_diffrn_orient_matrix_UB_32      -0.0078969000
_diffrn_orient_matrix_UB_33      -0.0953634000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3810
_reflns_number_total             4030
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.041
_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)+(0.0611P)²+19.7346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1128
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12_$1-H11_$2
 1.721 with sigma of 0.02
 H11_$2-O12_$2
 2.351 with sigma of 0.02
 O21-H21 = O11-H11
 0.8 with sigma of 0.02
 O11-H11 \\sim O21-H21
 with sigma of 0.02
3. Rigid bond restraints
 C3, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim O3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C4 \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
5. Others
 Fixed Uiso: H11(0.087)
6.a Ternary CH refined with riding coordinates:
 C1(H1)
6.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C14(H14), C12(H12)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
6.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ru1 Ru 0.63621(2) 0.80296(2) 0.49434(2) 0.02523(12) Uani 1 1 d . . . . .
Cl02 Cl 0.61310(3) 0.94583(9) 0.34866(10) 0.0434(2) Uani 1 1 d . . . . .
O1 O 0.65671(8) 0.6645(2) 0.6083(2) 0.0272(5) Uani 1 1 d . . . . .
O2 O 0.67486(8) 0.4832(2) 0.6178(2) 0.0294(5) Uani 1 1 d . . . . .
O21 O 0.78799(9) 0.7031(2) 0.1554(3) 0.0338(6) Uani 1 1 d D . . . .
O22 O 0.77214(8) 0.8875(2) 0.1647(2) 0.0308(6) Uani 1 1 d . . . . .
N22 N 0.69457(8) 0.6568(3) 0.3754(3) 0.0225(6) Uani 1 1 d . . . . .
N21 N 0.68583(9) 0.7681(3) 0.3948(3) 0.0238(6) Uani 1 1 d . . . . .
O4 O 0.68429(9) 0.9841(3) 0.6409(3) 0.0446(7) Uani 1 1 d . U . . .
N11 N 0.60668(9) 0.6790(3) 0.3741(3) 0.0278(6) Uani 1 1 d . . . . .
N12 N 0.62759(8) 0.5821(3) 0.3543(3) 0.0237(6) Uani 1 1 d . . . . .
O11 O 0.54593(10) 0.4398(3) 0.0841(3) 0.0518(9) Uani 1 1 d D . . . .
O5 O 0.83898(13) 0.7832(3) 0.0101(4) 0.0578(10) Uani 1 1 d . . . . .
H5 H 0.829411 0.831029 -0.040111 0.087 Uiso 1 1 calc R U . . .
O12 O 0.51023(10) 0.6005(4) 0.1013(3) 0.0607(11) Uani 1 1 d . . . . .
C23 C 0.73733(10) 0.7557(3) 0.2778(3) 0.0247(7) Uani 1 1 d . . . . .
C24 C 0.72527(10) 0.6470(3) 0.3040(3) 0.0226(7) Uani 1 1 d . . . . .
H24 H 0.736277 0.579823 0.277378 0.027 Uiso 1 1 calc R U . . .
C22 C 0.71174(11) 0.8279(3) 0.3371(3) 0.0255(7) Uani 1 1 d . . . . .
H22 H 0.712906 0.906673 0.335865 0.031 Uiso 1 1 calc R U . . .
C26 C 0.76753(11) 0.7898(3) 0.1947(3) 0.0264(7) Uani 1 1 d . . . . .
C1 C 0.66861(10) 0.5683(3) 0.4159(3) 0.0222(7) Uani 1 1 d . . . . .
H1 H 0.679101 0.494453 0.392866 0.027 Uiso 1 1 calc R U . . .
C2 C 0.66706(10) 0.5718(3) 0.5599(3) 0.0237(7) Uani 1 1 d . . . . .
C14 C 0.60670(10) 0.5146(3) 0.2707(3) 0.0285(7) Uani 1 1 d . . . . .
H14 H 0.614528 0.443999 0.243322 0.034 Uiso 1 1 calc R U . . .
C4 C 0.66657(12) 0.9162(4) 0.5926(4) 0.0331(8) Uani 1 1 d . U . . .
C12 C 0.57219(11) 0.6731(4) 0.3006(3) 0.0327(8) Uani 1 1 d . . . . .
H12 H 0.551918 0.727884 0.294567 0.039 Uiso 1 1 calc R U . . .
C13 C 0.57094(11) 0.5717(4) 0.2334(4) 0.0345(9) Uani 1 1 d . . . . .
O3 O 0.56492(14) 0.8394(5) 0.6410(5) 0.0882(16) Uani 1 1 d . U . . .
C3 C 0.58878(14) 0.8251(4) 0.5850(4) 0.0397(9) Uani 1 1 d . U . . .
C16 C 0.53915(12) 0.5376(4) 0.1353(4) 0.0422(10) Uani 1 1 d . . . . .
C5 C 0.8706(2) 0.7269(5) -0.0390(7) 0.0677(16) Uani 1 1 d . . . . .
H5A H 0.862926 0.710708 -0.126083 0.102 Uiso 1 1 calc R U . . .
H5B H 0.876196 0.657184 0.005707 0.102 Uiso 1 1 calc R U . . .
H5C H 0.894304 0.773845 -0.030642 0.102 Uiso 1 1 calc R U . . .
H21 H 0.8020(14) 0.731(4) 0.105(4) 0.048(15) Uiso 1 1 d D . . . .
H11 H 0.5268(11) 0.419(3) 0.031(4) 0.087 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ru1 Cl02 2.3690(11) . ?
Ru1 O1 2.108(3) . ?
Ru1 N21 2.099(3) . ?
Ru1 N11 2.118(3) . ?
Ru1 C4 1.919(4) . ?
Ru1 C3 1.956(5) . ?
O1 C2 1.274(4) . ?
O2 C2 1.229(4) . ?
O21 C26 1.321(5) . ?
O21 H21 0.818(16) . ?
O22 C26 1.210(4) . ?
N22 N21 1.365(4) . ?
N22 C24 1.345(4) . ?
N22 C1 1.450(4) . ?
N21 C22 1.318(5) . ?
O4 C4 1.091(5) . ?
N11 N12 1.366(4) . ?
N11 C12 1.321(5) . ?
N12 C1 1.457(4) . ?
N12 C14 1.336(5) . ?
O11 C16 1.308(6) . ?
O11 H11 0.842(14) . ?
O5 H5 0.8200 . ?
O5 C5 1.392(7) . ?
O12 C16 1.236(6) . ?
C23 C24 1.381(5) . ?
C23 C22 1.403(5) . ?
C23 C26 1.468(5) . ?
C24 H24 0.9300 . ?
C22 H22 0.9300 . ?
C1 H1 0.9800 . ?
C1 C2 1.552(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.385(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(6) . ?
C13 C16 1.463(5) . ?
O3 C3 1.058(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 Cl02 174.16(7) . . ?
O1 Ru1 N11 85.28(11) . . ?
N21 Ru1 Cl02 91.12(8) . . ?
N21 Ru1 O1 85.50(11) . . ?
N21 Ru1 N11 83.78(12) . . ?
N11 Ru1 Cl02 89.63(9) . . ?
C4 Ru1 Cl02 88.91(12) . . ?
C4 Ru1 O1 95.92(14) . . ?
C4 Ru1 N21 91.25(14) . . ?
C4 Ru1 N11 174.79(14) . . ?
C4 Ru1 C3 92.11(18) . . ?
C3 Ru1 Cl02 90.71(14) . . ?
C3 Ru1 O1 92.39(15) . . ?
C3 Ru1 N21 176.20(16) . . ?
C3 Ru1 N11 92.91(16) . . ?
C2 O1 Ru1 120.9(2) . . ?
C26 O21 H21 105(4) . . ?
N21 N22 C1 120.2(3) . . ?
C24 N22 N21 110.9(3) . . ?
C24 N22 C1 128.4(3) . . ?
N22 N21 Ru1 117.2(2) . . ?
C22 N21 Ru1 136.2(3) . . ?
C22 N21 N22 106.4(3) . . ?
N12 N11 Ru1 117.6(2) . . ?
C12 N11 Ru1 135.6(3) . . ?
C12 N11 N12 106.6(3) . . ?
N11 N12 C1 119.2(3) . . ?
C14 N12 N11 111.6(3) . . ?
C14 N12 C1 129.0(3) . . ?
C16 O11 H11 113.0(16) . . ?
C5 O5 H5 109.5 . . ?
C24 C23 C22 105.5(3) . . ?
C24 C23 C26 127.6(3) . . ?
C22 C23 C26 126.6(3) . . ?
N22 C24 C23 106.9(3) . . ?
N22 C24 H24 126.6 . . ?
C23 C24 H24 126.6 . . ?
N21 C22 C23 110.2(3) . . ?
N21 C22 H22 124.9 . . ?
C23 C22 H22 124.9 . . ?
O21 C26 C23 113.0(3) . . ?
O22 C26 O21 124.6(3) . . ?
O22 C26 C23 122.5(3) . . ?
N22 C1 N12 109.9(3) . . ?
N22 C1 H1 109.0 . . ?
N22 C1 C2 111.4(3) . . ?
N12 C1 H1 109.0 . . ?
N12 C1 C2 108.6(3) . . ?
C2 C1 H1 109.0 . . ?
O1 C2 C1 117.9(3) . . ?
O2 C2 O1 125.1(3) . . ?
O2 C2 C1 117.0(3) . . ?
N12 C14 H14 127.1 . . ?
N12 C14 C13 105.7(3) . . ?
C13 C14 H14 127.1 . . ?
O4 C4 Ru1 175.1(4) . . ?
N11 C12 H12 125.4 . . ?
N11 C12 C13 109.2(4) . . ?
C13 C12 H12 125.4 . . ?
C14 C13 C12 106.9(3) . . ?
C14 C13 C16 127.1(4) . . ?
C12 C13 C16 125.8(4) . . ?
O3 C3 Ru1 174.9(5) . . ?
O11 C16 C13 113.6(4) . . ?
O12 C16 O11 124.6(4) . . ?
O12 C16 C13 121.6(4) . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

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
Ru1 O1 C2 O2 -171.2(3) . . . . ?
Ru1 O1 C2 C1 6.6(4) . . . . ?
Ru1 N21 C22 C23 -175.6(2) . . . . ?
Ru1 N11 N12 C1 0.1(4) . . . . ?
Ru1 N11 N12 C14 -175.9(2) . . . . ?
Ru1 N11 C12 C13 174.0(3) . . . . ?
N22 N21 C22 C23 0.9(4) . . . . ?
N22 C1 C2 O1 55.1(4) . . . . ?
N22 C1 C2 O2 -126.9(3) . . . . ?
N21 N22 C24 C23 1.0(4) . . . . ?
N21 N22 C1 N12 59.4(4) . . . . ?
N21 N22 C1 C2 -60.9(4) . . . . ?
N11 N12 C1 N22 -61.3(4) . . . . ?
N11 N12 C1 C2 60.7(4) . . . . ?
N11 N12 C14 C13 1.0(4) . . . . ?
N11 C12 C13 C14 0.5(5) . . . . ?
N11 C12 C13 C16 -175.1(4) . . . . ?
N12 N11 C12 C13 0.1(4) . . . . ?
N12 C1 C2 O1 -66.1(4) . . . . ?
N12 C1 C2 O2 111.9(3) . . . . ?
N12 C14 C13 C12 -0.9(4) . . . . ?
N12 C14 C13 C16 174.7(4) . . . . ?
C24 N22 N21 Ru1 176.1(2) . . . . ?
C24 N22 N21 C22 -1.2(4) . . . . ?
C24 N22 C1 N12 -111.4(4) . . . . ?
C24 N22 C1 C2 128.2(3) . . . . ?
C24 C23 C22 N21 -0.3(4) . . . . ?
C24 C23 C26 O21 -8.8(5) . . . . ?
C24 C23 C26 O22 169.8(3) . . . . ?
C22 C23 C24 N22 -0.4(4) . . . . ?
C22 C23 C26 O21 178.2(3) . . . . ?
C22 C23 C26 O22 -3.1(6) . . . . ?
C26 C23 C24 N22 -174.5(3) . . . . ?
C26 C23 C22 N21 173.9(3) . . . . ?
C1 N22 N21 Ru1 3.8(4) . . . . ?
C1 N22 N21 C22 -173.5(3) . . . . ?
C1 N22 C24 C23 172.5(3) . . . . ?
C1 N12 C14 C13 -174.4(3) . . . . ?
C14 N12 C1 N22 113.8(4) . . . . ?
C14 N12 C1 C2 -124.1(4) . . . . ?
C14 C13 C16 O11 3.0(7) . . . . ?
C14 C13 C16 O12 -172.9(5) . . . . ?
C12 N11 N12 C1 175.2(3) . . . . ?
C12 N11 N12 C14 -0.7(4) . . . . ?
C12 C13 C16 O11 177.9(4) . . . . ?
C12 C13 C16 O12 1.9(8) . . . . ?

_olex2_date_sample_data_collection 2021-08-26
_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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.754
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_buni211221a
_database_code_depnum_ccdc_archive 'CCDC 2130708'
loop_
_audit_author_name
_audit_author_address
'Michaela Reil'
;Friedrich Alexander University Erlangen Nurnberg
Germany
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_audit_creation_date             2022-03-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H7 Cl N4 O8 Ru, H2 O'
_chemical_formula_sum            'C12 H9 Cl N4 O9 Ru'
_chemical_formula_weight         489.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H7ClN4O9Ru
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'
Cl Cl 0.3639 0.7018 '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'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5010(2)
_cell_length_b                   14.0811(2)
_cell_length_c                   9.18410(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.0360(10)
_cell_angle_gamma                90
_cell_volume                     1614.39(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      72.4800
_cell_measurement_theta_min      5.7430
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.973
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 1 0.0751
0 -1 0 0.0552
1 -1 0 0.0521
-2 1 2 0.0991
-8 -2 0 0.0379
-5 7 1 0.0236
3 8 1 0.0454
5 7 -1 0.0512
1 1 -2 0.1125
2 -1 -2 0.1016
0 -1 -2 0.1088
1 -1 -1 0.0931
2 2 1 0.0755
-2 1 0 0.0321
2 -1 0 0.0577
-2 -1 -2 0.0839
-1 -2 0 0.0626
2 -2 1 0.0690
0 -2 1 0.1106
-6 5 -1 0.0184
1 0 0 0.0590
0 1 2 0.1089

_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.076
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
1.9999 -0.9991 0.9997 -0.1204 -0.1483 -0.2624
0.0001 -0.9997 0.0001 -0.1090 0.0090 -0.0008
1.0001 -0.9993 0.0001 -0.1078 0.0137 -0.1240
-2.0004 0.9986 1.9994 0.0789 -0.3517 0.2170
-7.8111 -2.2134 -0.4429 -0.2446 0.0574 0.9679
-5.1512 7.0379 0.5616 0.7537 -0.1812 0.6317
2.8250 8.4193 0.9256 0.9089 -0.2172 -0.3560
5.0227 7.1471 -0.6289 0.7942 0.0637 -0.6043
1.0002 1.0005 -1.9996 0.1379 0.3290 -0.0923
2.0004 -0.9986 -1.9994 -0.0789 0.3517 -0.2170
0.0005 -0.9994 -1.9992 -0.0814 0.3423 0.0295
1.0003 -0.9992 -0.9996 -0.0940 0.1803 -0.1089
1.9995 2.0002 0.9993 0.2067 -0.1753 -0.2601
-2.0001 0.9989 0.0000 0.1066 -0.0183 0.2473
2.0001 -0.9989 -0.0000 -0.1066 0.0183 -0.2473
-1.9994 -1.0003 -1.9991 -0.0839 0.3330 0.2760
-0.9997 -1.9999 0.0003 -0.2193 0.0134 0.1217
2.0000 -1.9988 0.9998 -0.2294 -0.1393 -0.2632
0.0001 -1.9997 0.9999 -0.2319 -0.1486 -0.0166
-6.4092 5.3938 -0.7470 0.5910 0.0460 0.8054
1.0000 0.0004 -0.0001 0.0012 0.0047 -0.1233
-0.0005 0.9994 1.9992 0.0814 -0.3423 -0.0295

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5952
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.586
_diffrn_reflns_theta_min         3.541
_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 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -112.00 -40.00   1.00    1.00    --  -41.69 -38.00 -90.00   72
  2  ω    -21.00  74.00   1.00    1.00    --   41.69 -77.00 150.00   95
  3  ω     23.00 102.00   1.00    4.00    --  104.37 -94.00 -60.00   79
  4  ω    108.00 150.00   1.00    4.00    --  104.37 125.00-150.00   42
  5  ω     61.00 106.00   1.00    4.00    --  104.37 -94.00  30.00   45
  6  ω     56.00 174.00   1.00    4.00    --  104.37  15.00 -30.00  118
  7  ω     87.00 112.00   1.00    4.00    --  104.37-125.00 -90.00   25
  8  ω     35.00  60.00   1.00    4.00    --  104.37-125.00 -90.00   25
  9  ω     32.00 127.00   1.00    4.00    --  104.37 -45.00 -60.00   95
;
_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      0.0011899000
_diffrn_orient_matrix_UB_12      0.1090717000
_diffrn_orient_matrix_UB_13      -0.0138049000
_diffrn_orient_matrix_UB_21      0.0046594000
_diffrn_orient_matrix_UB_22      -0.0090316000
_diffrn_orient_matrix_UB_23      -0.1667137000
_diffrn_orient_matrix_UB_31      -0.1232677000
_diffrn_orient_matrix_UB_32      0.0007414000
_diffrn_orient_matrix_UB_33      -0.0151481000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2970
_reflns_number_total             3100
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.058
_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)+(0.0458P)²+1.4266P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0768
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O11-H11 = O21-H21
 0.8 with sigma of 0.02
 O21-H21 \\sim O11-H11
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O4 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C3 \\sim O3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
C4 \\sim O4: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
4. Rigid body (RIGU) restrains
 H13a, O13, H13b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, O4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C24(H24), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ru1 Ru 0.25021(2) 0.38818(2) 0.63588(2) 0.01301(9) Uani 1 1 d . . . . .
Cl1 Cl 0.25289(5) 0.22099(5) 0.61918(7) 0.02552(16) Uani 1 1 d . . . . .
O11 O 0.58949(15) 0.41660(14) 0.1057(2) 0.0202(4) Uani 1 1 d D . . . .
O1 O 0.24584(13) 0.53810(14) 0.63063(18) 0.0164(4) Uani 1 1 d . . . . .
O2 O 0.21860(15) 0.66744(14) 0.4966(2) 0.0219(4) Uani 1 1 d . . . . .
O22 O -0.10328(16) 0.37757(15) 0.0608(2) 0.0232(4) Uani 1 1 d . . . . .
O13 O 0.70964(16) 0.35605(14) -0.0946(2) 0.0195(4) Uani 1 1 d . . . . .
O21 O -0.10852(15) 0.25455(15) 0.2168(2) 0.0229(4) Uani 1 1 d D . . . .
N12 N 0.34039(16) 0.46823(15) 0.3665(2) 0.0147(4) Uani 1 1 d . . . . .
O12 O 0.61204(16) 0.28123(14) 0.2318(2) 0.0248(4) Uani 1 1 d . . . . .
O4 O 0.42745(18) 0.36779(16) 0.8691(3) 0.0297(5) Uani 1 1 d . U . . .
N21 N 0.13443(18) 0.39510(15) 0.4574(3) 0.0162(5) Uani 1 1 d . . . . .
N11 N 0.36152(18) 0.40080(15) 0.4710(3) 0.0153(4) Uani 1 1 d . . . . .
N22 N 0.15004(16) 0.46072(15) 0.3513(2) 0.0145(4) Uani 1 1 d . . . . .
O3 O 0.0853(2) 0.38328(15) 0.8627(3) 0.0319(5) Uani 1 1 d . U . . .
C12 C 0.4487(2) 0.35592(19) 0.4326(3) 0.0168(5) Uani 1 1 d . . . . .
H12 H 0.481520 0.306153 0.484401 0.020 Uiso 1 1 calc R U . . .
C3 C 0.1430(3) 0.38382(17) 0.7800(3) 0.0207(6) Uani 1 1 d . U . . .
C23 C 0.0123(2) 0.37702(19) 0.2716(3) 0.0166(5) Uani 1 1 d . . . . .
C16 C 0.5698(2) 0.35774(19) 0.2127(3) 0.0173(5) Uani 1 1 d . . . . .
C13 C 0.4846(2) 0.39407(17) 0.3028(3) 0.0173(5) Uani 1 1 d . . . . .
C22 C 0.05072(19) 0.34342(18) 0.4093(3) 0.0169(5) Uani 1 1 d . . . . .
H22 H 0.021892 0.292740 0.458946 0.020 Uiso 1 1 calc R U . . .
C24 C 0.07850(19) 0.45103(18) 0.2378(3) 0.0155(5) Uani 1 1 d . . . . .
H24 H 0.074523 0.487228 0.152960 0.019 Uiso 1 1 calc R U . . .
C14 C 0.41243(19) 0.46497(18) 0.2636(3) 0.0158(5) Uani 1 1 d . . . . .
H14 H 0.413593 0.503302 0.181257 0.019 Uiso 1 1 calc R U . . .
C1 C 0.24212(18) 0.52359(19) 0.3672(3) 0.0147(5) Uani 1 1 d . . . . .
H1 H 0.240258 0.567473 0.284296 0.018 Uiso 1 1 calc R U . . .
C26 C -0.07315(19) 0.33743(19) 0.1737(3) 0.0165(5) Uani 1 1 d . . . . .
C2 C 0.23538(19) 0.58229(18) 0.5101(3) 0.0156(5) Uani 1 1 d . . . . .
C4 C 0.3617(2) 0.37870(17) 0.7856(3) 0.0182(5) Uani 1 1 d . U . . .
H21 H -0.151(3) 0.236(3) 0.156(4) 0.052(13) Uiso 1 1 d D . . . .
H11 H 0.628(3) 0.392(2) 0.052(3) 0.024(10) Uiso 1 1 d D . . . .
H13A H 0.683(3) 0.307(3) -0.128(4) 0.022(9) Uiso 1 1 d . . . . .
H13B H 0.769(3) 0.346(3) -0.055(4) 0.019(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ru1 Cl1 2.3596(8) . ?
Ru1 O1 2.1123(19) . ?
Ru1 N21 2.131(2) . ?
Ru1 N11 2.118(2) . ?
Ru1 C3 1.934(3) . ?
Ru1 C4 1.910(3) . ?
O11 C16 1.319(3) . ?
O11 H11 0.795(14) . ?
O1 C2 1.271(3) . ?
O2 C2 1.222(3) . ?
O22 C26 1.223(3) . ?
O13 H13A 0.81(4) . ?
O13 H13B 0.82(4) . ?
O21 C26 1.316(3) . ?
O21 H21 0.792(14) . ?
N12 N11 1.365(3) . ?
N12 C14 1.340(3) . ?
N12 C1 1.455(3) . ?
O12 C16 1.209(3) . ?
O4 C4 1.105(4) . ?
N21 N22 1.364(3) . ?
N21 C22 1.331(3) . ?
N11 C12 1.324(4) . ?
N22 C24 1.344(3) . ?
N22 C1 1.453(3) . ?
O3 C3 1.075(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.403(4) . ?
C23 C22 1.410(4) . ?
C23 C24 1.377(4) . ?
C23 C26 1.469(4) . ?
C16 C13 1.474(4) . ?
C13 C14 1.380(4) . ?
C22 H22 0.9300 . ?
C24 H24 0.9300 . ?
C14 H14 0.9300 . ?
C1 H1 0.9800 . ?
C1 C2 1.557(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 Cl1 174.96(5) . . ?
O1 Ru1 N21 85.47(7) . . ?
O1 Ru1 N11 85.24(8) . . ?
N21 Ru1 Cl1 90.40(6) . . ?
N11 Ru1 Cl1 91.44(6) . . ?
N11 Ru1 N21 83.76(9) . . ?
C3 Ru1 Cl1 91.47(7) . . ?
C3 Ru1 O1 91.68(9) . . ?
C3 Ru1 N21 93.49(11) . . ?
C3 Ru1 N11 176.01(9) . . ?
C4 Ru1 Cl1 87.98(8) . . ?
C4 Ru1 O1 95.93(9) . . ?
C4 Ru1 N21 175.63(10) . . ?
C4 Ru1 N11 92.22(10) . . ?
C4 Ru1 C3 90.62(12) . . ?
C16 O11 H11 110(3) . . ?
C2 O1 Ru1 120.70(16) . . ?
H13A O13 H13B 111(4) . . ?
C26 O21 H21 108(4) . . ?
N11 N12 C1 120.1(2) . . ?
C14 N12 N11 111.1(2) . . ?
C14 N12 C1 128.3(2) . . ?
N22 N21 Ru1 117.60(16) . . ?
C22 N21 Ru1 136.12(18) . . ?
C22 N21 N22 105.8(2) . . ?
N12 N11 Ru1 116.79(16) . . ?
C12 N11 Ru1 137.03(18) . . ?
C12 N11 N12 106.0(2) . . ?
N21 N22 C1 118.9(2) . . ?
C24 N22 N21 111.8(2) . . ?
C24 N22 C1 129.1(2) . . ?
N11 C12 H12 124.8 . . ?
N11 C12 C13 110.4(2) . . ?
C13 C12 H12 124.8 . . ?
O3 C3 Ru1 177.8(3) . . ?
C22 C23 C26 128.6(2) . . ?
C24 C23 C22 106.0(2) . . ?
C24 C23 C26 125.1(2) . . ?
O11 C16 C13 111.7(2) . . ?
O12 C16 O11 124.8(3) . . ?
O12 C16 C13 123.5(2) . . ?
C12 C13 C16 128.1(2) . . ?
C14 C13 C12 105.3(2) . . ?
C14 C13 C16 125.9(3) . . ?
N21 C22 C23 109.8(2) . . ?
N21 C22 H22 125.1 . . ?
C23 C22 H22 125.1 . . ?
N22 C24 C23 106.6(2) . . ?
N22 C24 H24 126.7 . . ?
C23 C24 H24 126.7 . . ?
N12 C14 C13 107.2(2) . . ?
N12 C14 H14 126.4 . . ?
C13 C14 H14 126.4 . . ?
N12 C1 H1 108.7 . . ?
N12 C1 C2 111.80(19) . . ?
N22 C1 N12 109.7(2) . . ?
N22 C1 H1 108.7 . . ?
N22 C1 C2 109.28(19) . . ?
C2 C1 H1 108.7 . . ?
O22 C26 O21 124.9(2) . . ?
O22 C26 C23 121.7(2) . . ?
O21 C26 C23 113.4(2) . . ?
O1 C2 C1 117.8(2) . . ?
O2 C2 O1 125.3(2) . . ?
O2 C2 C1 116.9(2) . . ?
O4 C4 Ru1 175.7(2) . . ?

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
Ru1 O1 C2 O2 170.29(19) . . . . ?
Ru1 O1 C2 C1 -8.4(3) . . . . ?
Ru1 N21 N22 C24 173.21(16) . . . . ?
Ru1 N21 N22 C1 -1.7(3) . . . . ?
Ru1 N21 C22 C23 -172.13(19) . . . . ?
Ru1 N11 C12 C13 175.5(2) . . . . ?
O11 C16 C13 C12 -173.7(3) . . . . ?
O11 C16 C13 C14 17.0(4) . . . . ?
N12 N11 C12 C13 0.0(3) . . . . ?
N12 C1 C2 O1 -54.2(3) . . . . ?
N12 C1 C2 O2 126.9(2) . . . . ?
O12 C16 C13 C12 9.5(4) . . . . ?
O12 C16 C13 C14 -159.7(3) . . . . ?
N21 N22 C24 C23 0.9(3) . . . . ?
N21 N22 C1 N12 63.3(3) . . . . ?
N21 N22 C1 C2 -59.6(3) . . . . ?
N11 N12 C14 C13 -1.0(3) . . . . ?
N11 N12 C1 N22 -60.6(3) . . . . ?
N11 N12 C1 C2 60.8(3) . . . . ?
N11 C12 C13 C16 -171.5(2) . . . . ?
N11 C12 C13 C14 -0.6(3) . . . . ?
N22 N21 C22 C23 -0.4(3) . . . . ?
N22 C1 C2 O1 67.4(3) . . . . ?
N22 C1 C2 O2 -111.4(2) . . . . ?
C12 C13 C14 N12 0.9(3) . . . . ?
C16 C13 C14 N12 172.2(2) . . . . ?
C22 N21 N22 C24 -0.3(3) . . . . ?
C22 N21 N22 C1 -175.2(2) . . . . ?
C22 C23 C24 N22 -1.1(3) . . . . ?
C22 C23 C26 O22 175.1(3) . . . . ?
C22 C23 C26 O21 -7.8(4) . . . . ?
C24 N22 C1 N12 -110.6(3) . . . . ?
C24 N22 C1 C2 126.5(3) . . . . ?
C24 C23 C22 N21 1.0(3) . . . . ?
C24 C23 C26 O22 -11.8(4) . . . . ?
C24 C23 C26 O21 165.3(2) . . . . ?
C14 N12 N11 Ru1 -175.90(16) . . . . ?
C14 N12 N11 C12 0.7(3) . . . . ?
C14 N12 C1 N22 110.4(3) . . . . ?
C14 N12 C1 C2 -128.2(3) . . . . ?
C1 N12 N11 Ru1 -3.5(3) . . . . ?
C1 N12 N11 C12 173.1(2) . . . . ?
C1 N12 C14 C13 -172.7(2) . . . . ?
C1 N22 C24 C23 175.1(2) . . . . ?
C26 C23 C22 N21 175.1(2) . . . . ?
C26 C23 C24 N22 -175.5(2) . . . . ?

_olex2_date_sample_data_collection 2021-12-21
_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 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.756
