#------------------------------------------------------------------------------
#$Date: 2023-04-19 02:42:20 +0300 (Wed, 19 Apr 2023) $
#$Revision: 282710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/28/7712815.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712815
loop_
_publ_author_name
'Brechin, Euan K.'
'Agapaki, Eleftheria'
'Canaj, Angelos'
'Nichol, Gary Stephen'
_publ_section_title
;
 Tetra-, tetradeca- and octadecametallic clusters of Mn
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00732D
_journal_year                    2023
_chemical_formula_moiety
'C24 H44 Br4 Mn4 N8 O8, 2(C2 H3 N), [+ solvents]'
_chemical_formula_sum            'C28.5 H50.75 Br4 Mn4 N10.25 O8'
_chemical_formula_weight         1204.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-29 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                99.820(2)
_cell_angle_beta                 90.437(2)
_cell_angle_gamma                105.874(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1989(2)
_cell_length_b                   12.8405(3)
_cell_length_c                   18.4168(3)
_cell_measurement_reflns_used    29932
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      32.4360
_cell_measurement_theta_min      3.7190
_cell_volume                     2282.13(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  -6.00   1.00   10.00    --  -24.07 134.00 -49.00   77
  2  ω    -83.00  -6.00   1.00   10.00    --  -24.07 135.00 129.00   77
  3  ω      6.00  85.00   1.00   10.00    --   25.94-135.00  63.00   79
  4  ω      6.00  85.00   1.00   10.00    --   25.94-134.00-116.00   79
  5  ω    -91.00  -7.00   1.00   10.00    --  -24.07 -57.00  30.00   84
  6  ω    -95.00   5.00   1.00   10.00    --  -24.07 -19.00  30.00  100
  7  ω    -93.00  -5.00   1.00   10.00    --  -24.07 -38.00  60.00   88
  8  ω    -20.00  65.00   1.00   10.00    --   25.94 -99.00 120.00   85
  9  ω      7.00  95.00   1.00   10.00    --   25.94  38.00-150.00   88
 10  ω    -20.00  65.00   1.00   10.00    --   25.94 -99.00 -60.00   85
 11  ω     -3.00  97.00   1.00   10.00    --   25.94  19.00  30.00  100
 12  ω      9.00  93.00   1.00   10.00    --   25.94  57.00 -60.00   84
 13  ω     35.00  99.00   1.00   10.00    --   25.94-178.00 -30.00   64
 14  ω    -43.00  39.00   1.00   10.00    --  -24.07  38.00 120.00   82
 15  ω      9.00  93.00   1.00   10.00    --   25.94  57.00 150.00   84
 16  ω      9.00  93.00   1.00   10.00    --   25.94  57.00  30.00   84
 17  ω      9.00  93.00   1.00   10.00    --   25.94  57.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0050093000
_diffrn_orient_matrix_UB_12      -0.0546099000
_diffrn_orient_matrix_UB_13      0.0047162000
_diffrn_orient_matrix_UB_21      -0.0052008000
_diffrn_orient_matrix_UB_22      -0.0172472000
_diffrn_orient_matrix_UB_23      -0.0388650000
_diffrn_orient_matrix_UB_31      0.0720620000
_diffrn_orient_matrix_UB_32      0.0113234000
_diffrn_orient_matrix_UB_33      -0.0002234000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            87672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.847
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1195
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         15804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0332
_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)+(0.0195P)²+1.4328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12560
_reflns_number_total             15804
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00732d2.cif
_cod_data_source_block           eb21266
_cod_original_formula_sum        'C28.50 H50.75 Br4 Mn4 N10.25 O8'
_cod_database_code               7712815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 O10 N10 Mn4 Br4'
_chemical_oxdiff_usercomment     '@ 120 K EA205'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N11, C30}
3. Uiso/Uaniso restraints and constraints
Uanis(N11) = Uanis(C30)
4. Rigid body (RIGU) restrains
 N11, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N11(0.25) C30(0.25) H11D(0.25) H11E(0.25) H11F(0.25) C29(0.25)
6.a Everything fixed:
 H11D, H11E, H11F
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B), C22(H22A,H22B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C14(H14), C20(H20)
6.d Idealised Me refined as rotating group:
 C5(H5C,H5D,H5E), C6(H6C,H6D,H6E), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id EA205
_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 2.228
_oxdiff_exptl_absorpt_empirical_full_min 0.717
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.84266(2) 0.42611(2) 0.76928(2) 0.01976(5) Uani 1 1 d . . . . .
Br2 Br 0.35952(2) 0.31919(2) 0.51925(2) 0.01796(5) Uani 1 1 d . . . . .
Br3 Br 0.26703(2) 0.71834(2) 0.75017(2) 0.01812(5) Uani 1 1 d . . . . .
Br4 Br 0.29249(2) 0.34775(2) 0.94167(2) 0.01715(5) Uani 1 1 d . . . . .
Mn1 Mn 0.63367(3) 0.49813(2) 0.80636(2) 0.01079(6) Uani 1 1 d . . . . .
Mn2 Mn 0.43655(3) 0.33485(2) 0.65740(2) 0.01128(6) Uani 1 1 d . . . . .
Mn3 Mn 0.43106(3) 0.60089(2) 0.71203(2) 0.01082(6) Uani 1 1 d . . . . .
Mn4 Mn 0.28894(3) 0.40552(2) 0.81346(2) 0.01025(6) Uani 1 1 d . . . . .
O1 O 0.45102(13) 0.56129(11) 0.82323(7) 0.0106(3) Uani 1 1 d . . . . .
O2 O 0.46652(13) 0.34607(11) 0.77864(7) 0.0119(3) Uani 1 1 d . . . . .
O3 O 0.57836(13) 0.50007(11) 0.69027(7) 0.0121(3) Uani 1 1 d . . . . .
O4 O 0.29570(13) 0.43312(11) 0.69703(7) 0.0112(3) Uani 1 1 d . . . . .
O5 O 0.62454(17) 0.45065(14) 0.91774(8) 0.0177(3) Uani 1 1 d . . . . .
H5A H 0.547(3) 0.419(2) 0.9263(14) 0.023(7) Uiso 1 1 d . . . . .
H5B H 0.652(3) 0.496(3) 0.9535(19) 0.059(11) Uiso 1 1 d . . . . .
O6 O 0.62506(17) 0.28467(15) 0.63150(9) 0.0203(3) Uani 1 1 d . . . . .
H6A H 0.622(3) 0.223(3) 0.6196(16) 0.036(9) Uiso 1 1 d . . . . .
H6B H 0.688(3) 0.310(3) 0.6631(17) 0.041(9) Uiso 1 1 d . . . . .
O7 O 0.39006(18) 0.58275(16) 0.58896(9) 0.0226(3) Uani 1 1 d . . . . .
H7A H 0.448(3) 0.611(3) 0.5653(18) 0.049(10) Uiso 1 1 d . . . . .
H7B H 0.375(4) 0.517(3) 0.5665(19) 0.063(12) Uiso 1 1 d . . . . .
O8 O 0.15603(16) 0.51766(14) 0.84383(8) 0.0157(3) Uani 1 1 d . . . . .
H8A H 0.183(3) 0.575(3) 0.8240(16) 0.042(9) Uiso 1 1 d . . . . .
H8B H 0.078(3) 0.495(3) 0.8343(16) 0.043(9) Uiso 1 1 d . . . . .
N1 N 0.71440(16) 0.67228(14) 0.86179(9) 0.0127(3) Uani 1 1 d . . . . .
N2 N 0.61225(16) 0.71684(14) 0.88701(9) 0.0114(3) Uani 1 1 d . . . . .
N3 N 0.33889(17) 0.16555(14) 0.68001(9) 0.0133(3) Uani 1 1 d . . . . .
N4 N 0.37434(17) 0.15627(14) 0.74966(9) 0.0136(3) Uani 1 1 d . . . . .
N5 N 0.63093(17) 0.71856(14) 0.69976(9) 0.0142(3) Uani 1 1 d . . . . .
N6 N 0.72190(16) 0.66606(14) 0.66869(9) 0.0141(3) Uani 1 1 d . . . . .
N7 N 0.10505(16) 0.28041(14) 0.75330(9) 0.0128(3) Uani 1 1 d . . . . .
N8 N 0.08426(16) 0.30164(14) 0.68466(8) 0.0122(3) Uani 1 1 d . . . . .
C1 C 0.8293(2) 0.75528(17) 0.87581(11) 0.0151(4) Uani 1 1 d . . . . .
C2 C 0.8000(2) 0.85130(18) 0.91064(11) 0.0180(4) Uani 1 1 d . . . . .
H2 H 0.863444 0.921405 0.926410 0.022 Uiso 1 1 calc R U . . .
C3 C 0.6606(2) 0.82396(17) 0.91756(10) 0.0145(4) Uani 1 1 d . . . . .
C4 C 0.47344(19) 0.64315(16) 0.88578(10) 0.0121(4) Uani 1 1 d . . . . .
H4A H 0.462487 0.609421 0.930655 0.015 Uiso 1 1 calc R U . . .
H4B H 0.405842 0.685594 0.885144 0.015 Uiso 1 1 calc R U . . .
C5 C 0.9641(2) 0.7398(2) 0.85405(13) 0.0241(5) Uani 1 1 d . . . . .
H5C H 0.953380 0.661877 0.834309 0.036 Uiso 1 1 calc R U . . .
H5D H 1.028594 0.763494 0.897351 0.036 Uiso 1 1 calc R U . . .
H5E H 0.999077 0.783814 0.816207 0.036 Uiso 1 1 calc R U . . .
C6 C 0.5701(2) 0.89130(19) 0.95015(13) 0.0228(5) Uani 1 1 d . . . . .
H6C H 0.534182 0.866566 0.995379 0.034 Uiso 1 1 calc R U . . .
H6D H 0.494190 0.882619 0.914641 0.034 Uiso 1 1 calc R U . . .
H6E H 0.622681 0.968955 0.961839 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2483(2) 0.06916(17) 0.65242(11) 0.0152(4) Uani 1 1 d . . . . .
C8 C 0.2284(2) -0.00110(18) 0.70415(12) 0.0190(4) Uani 1 1 d . . . . .
H8 H 0.170078 -0.074085 0.698002 0.023 Uiso 1 1 calc R U . . .
C9 C 0.3108(2) 0.05727(17) 0.76615(11) 0.0166(4) Uani 1 1 d . . . . .
C10 C 0.4811(2) 0.24687(16) 0.79343(11) 0.0140(4) Uani 1 1 d . . . . .
H10A H 0.472096 0.244713 0.846673 0.017 Uiso 1 1 calc R U . . .
H10B H 0.572436 0.239495 0.780233 0.017 Uiso 1 1 calc R U . . .
C11 C 0.3316(3) 0.02758(19) 0.83931(12) 0.0246(5) Uani 1 1 d . . . . .
H11A H 0.295476 0.073452 0.877566 0.037 Uiso 1 1 calc R U . . .
H11B H 0.429382 0.039879 0.850345 0.037 Uiso 1 1 calc R U . . .
H11C H 0.283681 -0.050120 0.838114 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1844(2) 0.04711(19) 0.57599(11) 0.0213(4) Uani 1 1 d . . . . .
H12A H 0.242099 0.016714 0.540988 0.032 Uiso 1 1 calc R U . . .
H12B H 0.175147 0.115962 0.563327 0.032 Uiso 1 1 calc R U . . .
H12C H 0.093938 -0.005811 0.573572 0.032 Uiso 1 1 calc R U . . .
C13 C 0.6987(2) 0.82605(17) 0.71283(11) 0.0162(4) Uani 1 1 d . . . . .
C14 C 0.8314(2) 0.84058(19) 0.68806(12) 0.0211(4) Uani 1 1 d . . . . .
H14 H 0.899773 0.908425 0.690249 0.025 Uiso 1 1 calc R U . . .
C15 C 0.8427(2) 0.73735(19) 0.66003(11) 0.0173(4) Uani 1 1 d . . . . .
C16 C 0.6773(2) 0.54591(17) 0.64455(11) 0.0153(4) Uani 1 1 d . . . . .
H16A H 0.639300 0.527716 0.592854 0.018 Uiso 1 1 calc R U . . .
H16B H 0.756139 0.515388 0.646910 0.018 Uiso 1 1 calc R U . . .
C17 C 0.9564(2) 0.6992(2) 0.62429(13) 0.0259(5) Uani 1 1 d . . . . .
H17A H 1.032534 0.763065 0.619657 0.039 Uiso 1 1 calc R U . . .
H17B H 0.924085 0.655727 0.575181 0.039 Uiso 1 1 calc R U . . .
H17C H 0.987073 0.653598 0.654589 0.039 Uiso 1 1 calc R U . . .
C18 C 0.6339(2) 0.91034(18) 0.75030(12) 0.0205(4) Uani 1 1 d . . . . .
H18A H 0.539572 0.874250 0.760166 0.031 Uiso 1 1 calc R U . . .
H18B H 0.634198 0.964121 0.718359 0.031 Uiso 1 1 calc R U . . .
H18C H 0.685311 0.947977 0.796976 0.031 Uiso 1 1 calc R U . . .
C19 C 0.0098(2) 0.18636(17) 0.75731(11) 0.0145(4) Uani 1 1 d . . . . .
C20 C -0.0726(2) 0.14967(18) 0.69146(11) 0.0178(4) Uani 1 1 d . . . . .
H20 H -0.147523 0.085421 0.680132 0.021 Uiso 1 1 calc R U . . .
C21 C -0.0230(2) 0.22540(17) 0.64657(11) 0.0150(4) Uani 1 1 d . . . . .
C22 C 0.16301(18) 0.40679(17) 0.66610(10) 0.0126(4) Uani 1 1 d . . . . .
H22A H 0.164723 0.400835 0.611832 0.015 Uiso 1 1 calc R U . . .
H22B H 0.119879 0.465386 0.685629 0.015 Uiso 1 1 calc R U . . .
C23 C -0.0680(2) 0.2307(2) 0.57053(11) 0.0227(5) Uani 1 1 d . . . . .
H23A H -0.097153 0.297508 0.571434 0.034 Uiso 1 1 calc R U . . .
H23B H -0.144397 0.165918 0.551963 0.034 Uiso 1 1 calc R U . . .
H23C H 0.008048 0.232063 0.538128 0.034 Uiso 1 1 calc R U . . .
C24 C 0.0008(2) 0.13346(19) 0.82387(12) 0.0207(4) Uani 1 1 d . . . . .
H24A H 0.018884 0.061633 0.810723 0.031 Uiso 1 1 calc R U . . .
H24B H -0.090797 0.123535 0.842364 0.031 Uiso 1 1 calc R U . . .
H24C H 0.068610 0.180448 0.862257 0.031 Uiso 1 1 calc R U . . .
N9 N 0.3057(3) 0.8206(3) 1.07186(19) 0.0631(8) Uani 1 1 d . . . . .
N10 N 0.5806(2) 1.05229(19) 0.59182(12) 0.0309(5) Uani 1 1 d . . . . .
N11 N 0.1369(12) 0.5437(13) 0.5170(8) 0.172(6) Uani 0.25 1 d . . P . .
C30 C 0.1369(12) 0.5437(13) 0.5170(8) 0.172(6) Uani 0.25 1 d . . P . .
H11D H 0.145290 0.535140 0.569260 0.257 Uiso 0.25 1 d . U P . .
H11E H 0.157100 0.616880 0.511510 0.257 Uiso 0.25 1 d . U P . .
H11F H 0.178930 0.497600 0.485750 0.257 Uiso 0.25 1 d . U P . .
C25 C 0.2206(3) 0.7405(3) 1.05368(17) 0.0414(7) Uani 1 1 d . . . . .
C26 C 0.1126(3) 0.6380(2) 1.03289(15) 0.0365(6) Uani 1 1 d . . . . .
H26A H 0.114063 0.589955 1.068730 0.055 Uiso 1 1 calc R U . . .
H26B H 0.127110 0.601186 0.983691 0.055 Uiso 1 1 calc R U . . .
H26C H 0.023983 0.653892 1.032240 0.055 Uiso 1 1 calc R U . . .
C27 C 0.5105(2) 0.9652(2) 0.58502(12) 0.0235(5) Uani 1 1 d . . . . .
C28 C 0.4214(3) 0.8533(2) 0.57591(14) 0.0305(5) Uani 1 1 d . . . . .
H28A H 0.465755 0.802690 0.546793 0.046 Uiso 1 1 calc R U . . .
H28B H 0.335037 0.849166 0.550297 0.046 Uiso 1 1 calc R U . . .
H28C H 0.403386 0.832774 0.624489 0.046 Uiso 1 1 calc R U . . .
C29 C 0.000000 0.500000 0.500000 0.158(8) Uani 0.5 2 d S . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0302
0 -1 0 0.0437
-1 0 -1 0.2165
2 0 -1 0.2247
0 0 -1 0.1147
0 0 1 0.1180
-1 0 2 0.1982
0 1 -2 0.0976
0 -1 2 0.0895
2 -1 2 0.2001
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 Mn1 Br1 172.77(4) . . ?
O1 Mn1 O5 92.26(5) . . ?
O2 Mn1 Br1 100.94(4) . . ?
O2 Mn1 O1 78.34(5) . . ?
O2 Mn1 O3 78.41(5) . . ?
O2 Mn1 O5 82.67(6) . . ?
O2 Mn1 N1 151.10(5) . . ?
O3 Mn1 Br1 92.24(4) . . ?
O3 Mn1 O1 80.55(5) . . ?
O3 Mn1 O5 160.75(6) . . ?
O3 Mn1 N1 106.85(6) . . ?
O5 Mn1 Br1 94.80(4) . . ?
N1 Mn1 Br1 107.12(4) . . ?
N1 Mn1 O1 74.69(5) . . ?
N1 Mn1 O5 88.15(6) . . ?
O2 Mn2 Br2 170.61(4) . . ?
O2 Mn2 N3 74.10(5) . . ?
O3 Mn2 Br2 106.10(4) . . ?
O3 Mn2 O2 78.01(5) . . ?
O3 Mn2 O4 78.36(5) . . ?
O3 Mn2 O6 84.12(6) . . ?
O3 Mn2 N3 150.56(5) . . ?
O4 Mn2 Br2 92.39(3) . . ?
O4 Mn2 O2 80.07(5) . . ?
O4 Mn2 O6 162.34(6) . . ?
O4 Mn2 N3 105.56(6) . . ?
O6 Mn2 Br2 94.56(5) . . ?
O6 Mn2 O2 94.26(6) . . ?
O6 Mn2 N3 88.69(6) . . ?
N3 Mn2 Br2 102.89(4) . . ?
O1 Mn3 Br3 94.30(3) . . ?
O1 Mn3 O3 80.47(5) . . ?
O1 Mn3 O7 161.85(6) . . ?
O1 Mn3 N5 104.08(6) . . ?
O3 Mn3 Br3 174.57(4) . . ?
O3 Mn3 O7 89.57(6) . . ?
O4 Mn3 Br3 102.50(4) . . ?
O4 Mn3 O1 78.96(5) . . ?
O4 Mn3 O3 78.04(5) . . ?
O4 Mn3 O7 84.18(6) . . ?
O4 Mn3 N5 150.92(6) . . ?
O7 Mn3 Br3 95.86(5) . . ?
N5 Mn3 Br3 106.04(5) . . ?
N5 Mn3 O3 74.08(6) . . ?
N5 Mn3 O7 87.49(6) . . ?
O1 Mn4 Br4 105.20(3) . . ?
O1 Mn4 O2 78.67(5) . . ?
O1 Mn4 O4 78.39(5) . . ?
O1 Mn4 O8 83.12(6) . . ?
O1 Mn4 N7 151.05(5) . . ?
O2 Mn4 Br4 93.13(4) . . ?
O2 Mn4 O4 79.98(5) . . ?
O2 Mn4 O8 161.33(6) . . ?
O2 Mn4 N7 106.03(6) . . ?
O4 Mn4 Br4 171.55(4) . . ?
O4 Mn4 O8 92.38(5) . . ?
O4 Mn4 N7 74.50(5) . . ?
O8 Mn4 Br4 95.62(4) . . ?
O8 Mn4 N7 88.01(6) . . ?
N7 Mn4 Br4 103.05(4) . . ?
Mn3 O1 Mn1 98.01(5) . . ?
Mn4 O1 Mn1 100.35(5) . . ?
Mn4 O1 Mn3 100.69(5) . . ?
C4 O1 Mn1 110.17(11) . . ?
C4 O1 Mn3 120.69(12) . . ?
C4 O1 Mn4 122.60(11) . . ?
Mn1 O2 Mn2 100.93(5) . . ?
Mn1 O2 Mn4 101.19(6) . . ?
Mn4 O2 Mn2 98.40(5) . . ?
C10 O2 Mn1 120.82(11) . . ?
C10 O2 Mn2 109.71(11) . . ?
C10 O2 Mn4 121.81(11) . . ?
Mn1 O3 Mn3 97.91(5) . . ?
Mn2 O3 Mn1 101.17(5) . . ?
Mn2 O3 Mn3 100.56(5) . . ?
C16 O3 Mn1 120.50(12) . . ?
C16 O3 Mn2 122.23(11) . . ?
C16 O3 Mn3 110.24(12) . . ?
Mn2 O4 Mn4 98.26(5) . . ?
Mn3 O4 Mn2 101.63(5) . . ?
Mn3 O4 Mn4 100.45(5) . . ?
C22 O4 Mn2 121.35(12) . . ?
C22 O4 Mn3 121.53(12) . . ?
C22 O4 Mn4 109.45(10) . . ?
Mn1 O5 H5A 112.0(18) . . ?
Mn1 O5 H5B 120(3) . . ?
H5A O5 H5B 105(3) . . ?
Mn2 O6 H6A 121(2) . . ?
Mn2 O6 H6B 115(2) . . ?
H6A O6 H6B 106(3) . . ?
Mn3 O7 H7A 119(2) . . ?
Mn3 O7 H7B 113(2) . . ?
H7A O7 H7B 99(3) . . ?
Mn4 O8 H8A 110(2) . . ?
Mn4 O8 H8B 119(2) . . ?
H8A O8 H8B 107(3) . . ?
N2 N1 Mn1 111.91(12) . . ?
C1 N1 Mn1 142.59(14) . . ?
C1 N1 N2 105.26(16) . . ?
N1 N2 C4 118.43(16) . . ?
C3 N2 N1 111.96(16) . . ?
C3 N2 C4 129.16(16) . . ?
N4 N3 Mn2 111.26(12) . . ?
C7 N3 Mn2 143.39(14) . . ?
C7 N3 N4 105.08(16) . . ?
N3 N4 C10 118.56(16) . . ?
C9 N4 N3 112.45(16) . . ?
C9 N4 C10 128.75(17) . . ?
N6 N5 Mn3 111.84(12) . . ?
C13 N5 Mn3 142.77(14) . . ?
C13 N5 N6 105.38(16) . . ?
N5 N6 C16 119.20(15) . . ?
C15 N6 N5 112.02(17) . . ?
C15 N6 C16 128.61(17) . . ?
N8 N7 Mn4 110.89(11) . . ?
C19 N7 Mn4 143.50(13) . . ?
C19 N7 N8 105.44(15) . . ?
N7 N8 C22 118.72(15) . . ?
C21 N8 N7 111.92(16) . . ?
C21 N8 C22 128.69(16) . . ?
N1 C1 C2 110.18(18) . . ?
N1 C1 C5 121.43(19) . . ?
C2 C1 C5 128.4(2) . . ?
C1 C2 H2 126.8 . . ?
C3 C2 C1 106.34(18) . . ?
C3 C2 H2 126.8 . . ?
N2 C3 C2 106.25(17) . . ?
N2 C3 C6 122.56(18) . . ?
C2 C3 C6 131.2(2) . . ?
O1 C4 N2 109.30(14) . . ?
O1 C4 H4A 109.8 . . ?
O1 C4 H4B 109.8 . . ?
N2 C4 H4A 109.8 . . ?
N2 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
C1 C5 H5C 109.5 . . ?
C1 C5 H5D 109.5 . . ?
C1 C5 H5E 109.5 . . ?
H5C C5 H5D 109.5 . . ?
H5C C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
C3 C6 H6C 109.5 . . ?
C3 C6 H6D 109.5 . . ?
C3 C6 H6E 109.5 . . ?
H6C C6 H6D 109.5 . . ?
H6C C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
N3 C7 C8 110.34(18) . . ?
N3 C7 C12 121.33(19) . . ?
C8 C7 C12 128.3(2) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 C7 106.15(19) . . ?
C9 C8 H8 126.9 . . ?
N4 C9 C8 105.97(18) . . ?
N4 C9 C11 122.58(19) . . ?
C8 C9 C11 131.4(2) . . ?
O2 C10 N4 108.53(15) . . ?
O2 C10 H10A 110.0 . . ?
O2 C10 H10B 110.0 . . ?
N4 C10 H10A 110.0 . . ?
N4 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 C14 109.71(19) . . ?
N5 C13 C18 121.21(18) . . ?
C14 C13 C18 129.1(2) . . ?
C13 C14 H14 126.8 . . ?
C15 C14 C13 106.50(19) . . ?
C15 C14 H14 126.8 . . ?
N6 C15 C14 106.36(18) . . ?
N6 C15 C17 121.6(2) . . ?
C14 C15 C17 132.0(2) . . ?
O3 C16 N6 109.15(15) . . ?
O3 C16 H16A 109.9 . . ?
O3 C16 H16B 109.9 . . ?
N6 C16 H16A 109.9 . . ?
N6 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C19 C20 109.89(18) . . ?
N7 C19 C24 121.96(18) . . ?
C20 C19 C24 128.14(19) . . ?
C19 C20 H20 126.9 . . ?
C21 C20 C19 106.29(18) . . ?
C21 C20 H20 126.9 . . ?
N8 C21 C20 106.44(17) . . ?
N8 C21 C23 122.43(19) . . ?
C20 C21 C23 131.13(19) . . ?
O4 C22 N8 108.92(15) . . ?
O4 C22 H22A 109.9 . . ?
O4 C22 H22B 109.9 . . ?
N8 C22 H22A 109.9 . . ?
N8 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H11D N11 H11E 112.7 . . ?
H11D N11 H11F 111.4 . . ?
H11E N11 H11F 117.4 . . ?
C29 N11 H11D 102.4 . . ?
C29 N11 H11E 106.1 . . ?
C29 N11 H11F 105.2 . . ?
N9 C25 C26 178.2(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N10 C27 C28 179.6(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N11 C29 N11 180.0 . 2_566 ?
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
Br1 Mn1 2.5981(3) . ?
Br2 Mn2 2.6153(3) . ?
Br3 Mn3 2.5697(3) . ?
Br4 Mn4 2.5957(3) . ?
Mn1 O1 2.2301(13) . ?
Mn1 O2 2.1920(14) . ?
Mn1 O3 2.2131(13) . ?
Mn1 O5 2.2330(15) . ?
Mn1 N1 2.2185(17) . ?
Mn2 O2 2.2261(13) . ?
Mn2 O3 2.1976(14) . ?
Mn2 O4 2.2095(13) . ?
Mn2 O6 2.2195(16) . ?
Mn2 N3 2.2409(17) . ?
Mn3 O1 2.2135(13) . ?
Mn3 O3 2.2337(14) . ?
Mn3 O4 2.1880(14) . ?
Mn3 O7 2.2625(16) . ?
Mn3 N5 2.2198(17) . ?
Mn4 O1 2.1977(14) . ?
Mn4 O2 2.2092(13) . ?
Mn4 O4 2.2307(13) . ?
Mn4 O8 2.2424(15) . ?
Mn4 N7 2.2447(17) . ?
O1 C4 1.391(2) . ?
O2 C10 1.393(2) . ?
O3 C16 1.389(2) . ?
O4 C22 1.394(2) . ?
O5 H5A 0.81(3) . ?
O5 H5B 0.79(4) . ?
O6 H6A 0.77(3) . ?
O6 H6B 0.82(3) . ?
O7 H7A 0.78(3) . ?
O7 H7B 0.85(4) . ?
O8 H8A 0.86(3) . ?
O8 H8B 0.78(3) . ?
N1 N2 1.368(2) . ?
N1 C1 1.339(3) . ?
N2 C3 1.346(3) . ?
N2 C4 1.469(2) . ?
N3 N4 1.363(2) . ?
N3 C7 1.340(3) . ?
N4 C9 1.346(3) . ?
N4 C10 1.470(3) . ?
N5 N6 1.364(2) . ?
N5 C13 1.343(3) . ?
N6 C15 1.348(3) . ?
N6 C16 1.471(3) . ?
N7 N8 1.365(2) . ?
N7 C19 1.341(3) . ?
N8 C21 1.347(2) . ?
N8 C22 1.467(2) . ?
C1 C2 1.398(3) . ?
C1 C5 1.491(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.381(3) . ?
C3 C6 1.492(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5C 0.9800 . ?
C5 H5D 0.9800 . ?
C5 H5E 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6D 0.9800 . ?
C6 H6E 0.9800 . ?
C7 C8 1.400(3) . ?
C7 C12 1.495(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(3) . ?
C9 C11 1.490(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.405(3) . ?
C13 C18 1.493(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.374(3) . ?
C15 C17 1.494(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.404(3) . ?
C19 C24 1.491(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(3) . ?
C21 C23 1.489(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N9 C25 1.146(4) . ?
N10 C27 1.137(3) . ?
N11 H11D 0.9932 . ?
N11 H11E 0.9287 . ?
N11 H11F 0.9439 . ?
N11 C29 1.367(12) . ?
C25 C26 1.456(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.455(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5A Br4 0.81(3) 2.54(3) 3.3440(17) 169(2) . yes
O5 H5B Br4 0.79(4) 2.47(4) 3.2563(17) 170(3) 2_667 yes
O6 H6A N10 0.77(3) 2.09(3) 2.856(3) 171(3) 1_545 yes
O6 H6B Br1 0.82(3) 2.49(3) 3.2862(18) 163(3) . yes
O7 H7A Br2 0.78(3) 2.58(3) 3.3548(17) 173(3) 2_666 yes
O7 H7B Br2 0.85(4) 2.50(4) 3.3366(19) 169(3) . yes
O8 H8A Br3 0.86(3) 2.45(3) 3.2936(17) 171(3) . yes
O8 H8B Br1 0.78(3) 2.53(3) 3.2877(16) 165(3) 1_455 yes
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 C4 N2 42.97(17) . . . . ?
Mn1 O2 C10 N4 -162.69(11) . . . . ?
Mn1 O3 C16 N6 -70.01(18) . . . . ?
Mn1 N1 N2 C3 -177.09(12) . . . . ?
Mn1 N1 N2 C4 9.90(19) . . . . ?
Mn1 N1 C1 C2 174.34(16) . . . . ?
Mn1 N1 C1 C5 -4.7(3) . . . . ?
Mn2 O2 C10 N4 -46.06(16) . . . . ?
Mn2 O3 C16 N6 160.39(11) . . . . ?
Mn2 O4 C22 N8 67.60(17) . . . . ?
Mn2 N3 N4 C9 176.40(13) . . . . ?
Mn2 N3 N4 C10 -8.8(2) . . . . ?
Mn2 N3 C7 C8 -173.87(17) . . . . ?
Mn2 N3 C7 C12 6.9(3) . . . . ?
Mn3 O1 C4 N2 -70.03(17) . . . . ?
Mn3 O3 C16 N6 42.78(17) . . . . ?
Mn3 O4 C22 N8 -161.81(11) . . . . ?
Mn3 N5 N6 C15 178.99(13) . . . . ?
Mn3 N5 N6 C16 3.3(2) . . . . ?
Mn3 N5 C13 C14 -179.69(17) . . . . ?
Mn3 N5 C13 C18 1.7(3) . . . . ?
Mn4 O1 C4 N2 160.50(11) . . . . ?
Mn4 O2 C10 N4 67.82(17) . . . . ?
Mn4 O4 C22 N8 -45.56(16) . . . . ?
Mn4 N7 N8 C21 177.91(13) . . . . ?
Mn4 N7 N8 C22 -10.65(19) . . . . ?
Mn4 N7 C19 C20 -175.34(17) . . . . ?
Mn4 N7 C19 C24 4.1(3) . . . . ?
N1 N2 C3 C2 1.3(2) . . . . ?
N1 N2 C3 C6 -179.19(18) . . . . ?
N1 N2 C4 O1 -36.2(2) . . . . ?
N1 C1 C2 C3 -0.1(2) . . . . ?
N2 N1 C1 C2 0.8(2) . . . . ?
N2 N1 C1 C5 -178.22(18) . . . . ?
N3 N4 C9 C8 -0.5(2) . . . . ?
N3 N4 C9 C11 -179.36(18) . . . . ?
N3 N4 C10 O2 37.4(2) . . . . ?
N3 C7 C8 C9 0.6(2) . . . . ?
N4 N3 C7 C8 -0.9(2) . . . . ?
N4 N3 C7 C12 179.86(18) . . . . ?
N5 N6 C15 C14 1.3(2) . . . . ?
N5 N6 C15 C17 -177.48(18) . . . . ?
N5 N6 C16 O3 -31.5(2) . . . . ?
N5 C13 C14 C15 -0.7(2) . . . . ?
N6 N5 C13 C14 1.5(2) . . . . ?
N6 N5 C13 C18 -177.10(17) . . . . ?
N7 N8 C21 C20 -1.4(2) . . . . ?
N7 N8 C21 C23 179.21(18) . . . . ?
N7 N8 C22 O4 38.7(2) . . . . ?
N7 C19 C20 C21 0.3(2) . . . . ?
N8 N7 C19 C20 -1.1(2) . . . . ?
N8 N7 C19 C24 178.30(18) . . . . ?
C1 N1 N2 C3 -1.3(2) . . . . ?
C1 N1 N2 C4 -174.36(16) . . . . ?
C1 C2 C3 N2 -0.7(2) . . . . ?
C1 C2 C3 C6 179.8(2) . . . . ?
C3 N2 C4 O1 152.13(18) . . . . ?
C4 N2 C3 C2 173.36(18) . . . . ?
C4 N2 C3 C6 -7.1(3) . . . . ?
C5 C1 C2 C3 178.9(2) . . . . ?
C7 N3 N4 C9 0.9(2) . . . . ?
C7 N3 N4 C10 175.73(16) . . . . ?
C7 C8 C9 N4 0.0(2) . . . . ?
C7 C8 C9 C11 178.6(2) . . . . ?
C9 N4 C10 O2 -148.68(19) . . . . ?
C10 N4 C9 C8 -174.72(18) . . . . ?
C10 N4 C9 C11 6.4(3) . . . . ?
C12 C7 C8 C9 179.8(2) . . . . ?
C13 N5 N6 C15 -1.8(2) . . . . ?
C13 N5 N6 C16 -177.44(16) . . . . ?
C13 C14 C15 N6 -0.4(2) . . . . ?
C13 C14 C15 C17 178.3(2) . . . . ?
C15 N6 C16 O3 153.59(18) . . . . ?
C16 N6 C15 C14 176.51(18) . . . . ?
C16 N6 C15 C17 -2.3(3) . . . . ?
C18 C13 C14 C15 177.7(2) . . . . ?
C19 N7 N8 C21 1.6(2) . . . . ?
C19 N7 N8 C22 173.01(16) . . . . ?
C19 C20 C21 N8 0.7(2) . . . . ?
C19 C20 C21 C23 180.0(2) . . . . ?
C21 N8 C22 O4 -151.54(18) . . . . ?
C22 N8 C21 C20 -171.79(18) . . . . ?
C22 N8 C21 C23 8.8(3) . . . . ?
C24 C19 C20 C21 -179.1(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0010 0.9979 0.0005 -0.0545 -0.0172 0.0114
-0.0010 -0.9979 -0.0005 0.0545 0.0172 -0.0114
-0.9980 0.0010 -0.9991 0.0002 0.0440 -0.0717
1.9974 -0.0029 -0.9962 -0.0145 0.0284 0.1441
0.0005 -0.0003 -0.9981 -0.0047 0.0388 0.0003
-0.0005 0.0003 0.9981 0.0047 -0.0388 -0.0003
-0.9994 0.0019 1.9953 0.0143 -0.0724 -0.0724
0.0020 0.9973 -1.9957 -0.0639 0.0604 0.0119
-0.0020 -0.9973 1.9957 0.0639 -0.0604 -0.0119
1.9949 -0.9999 1.9977 0.0540 -0.0708 0.1320
