#------------------------------------------------------------------------------
#$Date: 2022-10-26 00:57:01 +0300 (Wed, 26 Oct 2022) $
#$Revision: 278779 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/08/7130893.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_7130893
loop_
_publ_author_name
'Karagiannis, Ageliki'
'Tyryshkin, Alexei M.'
'Lalancette, Roger A.'
'Spasyuk, Denis M.'
'Washington, Asmaa'
'Prokopchuk, Demyan E.'
_publ_section_title
;
 A Redox-active Manganate(0) Dicarbene Metalloradical
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04677F
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_sum            'C47 H68 B K Mn N6 O9'
_chemical_formula_weight         965.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-08 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.789(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1465(8)
_cell_length_b                   16.0225(15)
_cell_length_c                   20.4295(6)
_cell_measurement_reflns_used    14776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.096
_cell_measurement_theta_min      3.507
_cell_volume                     4853.3(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28203
_diffrn_reflns_point_group_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.691
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.380
_diffrn_reflns_theta_min         3.535
_exptl_absorpt_coefficient_mu    3.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.015(5)
_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     595
_refine_ls_number_reflns         7043
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0457
_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)+(0.0630P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.431
_reflns_Friedel_fraction_full    0.475
_reflns_Friedel_fraction_max     0.417
_reflns_number_gt                6323
_reflns_number_total             7043
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc04677f3.cif
_cod_data_source_block           211028RAL_AK_378_100K
_cod_original_cell_volume        4853.4(5)
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7130893
_shelx_shelxl_version_number     2018/3
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.757
_oxdiff_exptl_absorpt_empirical_full_max 1.186
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
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'
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 0.49880(4) 0.76628(4) 0.23624(3) 0.01566(15) Uani 1 1 d . . . . .
K1 K 0.19661(5) 0.76163(6) 0.36865(4) 0.01901(19) Uani 1 1 d . . . . .
O4 O 0.1129(2) 0.6833(2) 0.25026(16) 0.0247(7) Uani 1 1 d . . . . .
C29 C 0.3876(3) 0.7667(3) 0.2532(2) 0.0190(8) Uani 1 1 d . . . . .
O6 O 0.0722(2) 0.69897(19) 0.44928(15) 0.0216(6) Uani 1 1 d . . . . .
O2 O 0.5489(2) 0.8803(2) 0.35162(16) 0.0273(7) Uani 1 1 d . . . . .
O5 O 0.3221(2) 0.6453(2) 0.44214(16) 0.0236(6) Uani 1 1 d . . . . .
C9 C 0.5828(3) 0.6050(3) 0.1000(2) 0.0205(8) Uani 1 1 d . . . . .
H9 H 0.628038 0.591040 0.075847 0.025 Uiso 1 1 calc R U . . .
C25 C 0.8470(3) 0.8029(3) 0.2965(2) 0.0263(9) Uani 1 1 d . . . . .
H25 H 0.882209 0.850549 0.312478 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3810(3) 0.5606(3) 0.2338(2) 0.0215(9) Uani 1 1 d . . . . .
H13A H 0.324797 0.536358 0.241901 0.032 Uiso 1 1 calc R U . . .
H13B H 0.391132 0.614978 0.256013 0.032 Uiso 1 1 calc R U . . .
H13C H 0.431437 0.523292 0.251637 0.032 Uiso 1 1 calc R U . . .
C46 C 0.3843(3) 0.9026(3) 0.4398(2) 0.0257(10) Uani 1 1 d . . . . .
H46A H 0.449642 0.910250 0.441814 0.031 Uiso 1 1 calc R U . . .
H46B H 0.370534 0.922075 0.482614 0.031 Uiso 1 1 calc R U . . .
N6 N 0.2327(2) 0.9461(2) 0.37562(18) 0.0206(7) Uani 1 1 d . . . . .
C37 C 0.2024(3) 0.9880(3) 0.4316(2) 0.0240(9) Uani 1 1 d . . . . .
H37A H 0.194574 1.048337 0.421592 0.029 Uiso 1 1 calc R U . . .
H37B H 0.249613 0.981928 0.472686 0.029 Uiso 1 1 calc R U . . .
O7 O 0.1297(2) 0.8683(2) 0.46347(16) 0.0235(7) Uani 1 1 d . . . . .
C17 C 0.7184(3) 0.7426(3) -0.0334(2) 0.0274(10) Uani 1 1 d . . . . .
H17 H 0.689663 0.751706 -0.078674 0.033 Uiso 1 1 calc R U . . .
C35 C 0.0576(3) 0.8365(3) 0.4905(3) 0.0288(10) Uani 1 1 d . . . . .
H35A H 0.000322 0.841832 0.457215 0.035 Uiso 1 1 calc R U . . .
H35B H 0.052009 0.868768 0.530740 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4068(3) 0.9671(3) 0.1447(2) 0.0193(8) Uani 1 1 d . . . . .
C3 C 0.5498(3) 0.9570(3) 0.0979(2) 0.0196(8) Uani 1 1 d . . . . .
H3 H 0.543809 1.008950 0.075031 0.024 Uiso 1 1 calc R U . . .
C20 C 0.8007(3) 0.7173(3) 0.0995(2) 0.0208(9) Uani 1 1 d . . . . .
H20 H 0.830501 0.708796 0.144665 0.025 Uiso 1 1 calc R U . . .
C39 C 0.1837(3) 0.9310(3) 0.2514(2) 0.0232(9) Uani 1 1 d . . . . .
H39A H 0.160633 0.964037 0.210553 0.028 Uiso 1 1 calc R U . . .
H39B H 0.245350 0.911670 0.249923 0.028 Uiso 1 1 calc R U . . .
N1 N 0.5982(2) 0.8334(2) 0.13676(17) 0.0175(7) Uani 1 1 d . . . . .
C38 C 0.1861(3) 0.9845(3) 0.3126(2) 0.0232(9) Uani 1 1 d . . . . .
H38A H 0.216378 1.037879 0.306525 0.028 Uiso 1 1 calc R U . . .
H38B H 0.123424 0.997545 0.316196 0.028 Uiso 1 1 calc R U . . .
C21 C 0.7205(3) 0.7419(3) 0.2172(2) 0.0176(8) Uani 1 1 d . . . . .
C45 C 0.4114(3) 0.7646(3) 0.4811(3) 0.0314(11) Uani 1 1 d . . . . .
H45A H 0.383324 0.764994 0.520830 0.038 Uiso 1 1 calc R U . . .
H45B H 0.474010 0.785392 0.494670 0.038 Uiso 1 1 calc R U . . .
O8 O 0.3614(2) 0.8168(2) 0.43007(16) 0.0266(7) Uani 1 1 d . . . . .
C11 C 0.3741(3) 0.5718(3) 0.1585(2) 0.0189(8) Uani 1 1 d . . . . .
C5 C 0.3915(3) 1.0463(3) 0.1019(3) 0.0282(10) Uani 1 1 d . . . . .
H5A H 0.389637 1.031961 0.055037 0.042 Uiso 1 1 calc R U . . .
H5B H 0.440805 1.085728 0.117368 0.042 Uiso 1 1 calc R U . . .
H5C H 0.334102 1.071993 0.106005 0.042 Uiso 1 1 calc R U . . .
C44 C 0.4114(3) 0.6783(3) 0.4540(3) 0.0329(11) Uani 1 1 d . . . . .
H44A H 0.452362 0.645495 0.477778 0.039 Uiso 1 1 d R U . . .
C14 C 0.3009(3) 0.6352(3) 0.1290(2) 0.0233(9) Uani 1 1 d . . . . .
H14A H 0.320029 0.691250 0.145193 0.035 Uiso 1 1 calc R U . . .
H14B H 0.244511 0.620837 0.142846 0.035 Uiso 1 1 calc R U . . .
H14C H 0.291224 0.634112 0.080076 0.035 Uiso 1 1 calc R U . . .
N4 N 0.4630(2) 0.6017(2) 0.14523(17) 0.0174(7) Uani 1 1 d . . . . .
B1 B 0.6515(3) 0.7485(3) 0.1455(2) 0.0185(9) Uani 1 1 d . . . . .
C19 C 0.8486(3) 0.7066(3) 0.0489(3) 0.0288(10) Uani 1 1 d . . . . .
H19 H 0.910232 0.690628 0.059933 0.035 Uiso 1 1 calc R U . . .
C23 C 0.8157(3) 0.6578(3) 0.3035(2) 0.0255(9) Uani 1 1 d . . . . .
H23 H 0.828754 0.605032 0.324461 0.031 Uiso 1 1 calc R U . . .
C42 C 0.2251(3) 0.5287(3) 0.4109(2) 0.0263(10) Uani 1 1 d . . . . .
H42A H 0.223599 0.471109 0.393151 0.032 Uiso 1 1 calc R U . . .
H42B H 0.217560 0.525344 0.457793 0.032 Uiso 1 1 calc R U . . .
C18 C 0.8079(3) 0.7188(3) -0.0171(2) 0.0293(11) Uani 1 1 d . . . . .
H18 H 0.841205 0.710876 -0.051312 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5058(3) 0.6751(3) 0.1656(2) 0.0187(8) Uani 1 1 d . . . . .
C34 C 0.0753(3) 0.7465(3) 0.5085(2) 0.0274(10) Uani 1 1 d . . . . .
H34A H 0.135292 0.740618 0.538327 0.033 Uiso 1 1 calc R U . . .
H34B H 0.029263 0.725632 0.532601 0.033 Uiso 1 1 calc R U . . .
C27 C 0.5411(3) 0.6911(3) 0.2995(2) 0.0212(9) Uani 1 1 d . . . . .
N2 N 0.4925(2) 0.9256(2) 0.13754(18) 0.0178(7) Uani 1 1 d . . . . .
O1 O 0.5670(2) 0.6451(2) 0.34368(16) 0.0263(7) Uani 1 1 d . . . . .
N5 N 0.1492(2) 0.5760(2) 0.37163(18) 0.0222(8) Uani 1 1 d . . . . .
C28 C 0.5310(3) 0.8386(3) 0.3031(2) 0.0226(9) Uani 1 1 d . . . . .
C7 C 0.3279(3) 0.9070(3) 0.1190(2) 0.0227(9) Uani 1 1 d . . . . .
H7A H 0.325832 0.894159 0.071764 0.034 Uiso 1 1 calc R U . . .
H7B H 0.271107 0.933296 0.123613 0.034 Uiso 1 1 calc R U . . .
H7C H 0.336621 0.855310 0.145138 0.034 Uiso 1 1 calc R U . . .
C43 C 0.3158(3) 0.5666(3) 0.4097(2) 0.0259(10) Uani 1 1 d . . . . .
H43A H 0.364374 0.529342 0.432931 0.031 Uiso 1 1 calc R U . . .
H43B H 0.322914 0.573597 0.362925 0.031 Uiso 1 1 calc R U . . .
H24B H 0.439(4) 0.679(4) 0.409(3) 0.031 Uiso 1 1 d . U . . .
C6 C 0.4124(3) 0.9913(3) 0.2174(2) 0.0239(9) Uani 1 1 d . . . . .
H6A H 0.357617 1.021578 0.221573 0.036 Uiso 1 1 calc R U . . .
H6B H 0.465123 1.027022 0.232354 0.036 Uiso 1 1 calc R U . . .
H6C H 0.417962 0.940790 0.244983 0.036 Uiso 1 1 calc R U . . .
O9 O 0.1261(2) 0.8607(2) 0.25422(15) 0.0227(7) Uani 1 1 d . . . . .
C16 C 0.6705(3) 0.7530(3) 0.0181(2) 0.0244(10) Uani 1 1 d . . . . .
H16 H 0.608973 0.769343 0.006517 0.029 Uiso 1 1 calc R U . . .
C12 C 0.3500(3) 0.4869(3) 0.1257(2) 0.0243(9) Uani 1 1 d . . . . .
H12A H 0.290725 0.469325 0.132930 0.036 Uiso 1 1 calc R U . . .
H12B H 0.395493 0.445687 0.145475 0.036 Uiso 1 1 calc R U . . .
H12C H 0.348195 0.491080 0.077561 0.036 Uiso 1 1 calc R U . . .
C22 C 0.7429(3) 0.6659(3) 0.2494(2) 0.0215(9) Uani 1 1 d . . . . .
H22 H 0.707713 0.618036 0.234090 0.026 Uiso 1 1 calc R U . . .
C32 C 0.0679(3) 0.5640(3) 0.3991(2) 0.0246(9) Uani 1 1 d . . . . .
H32A H 0.061141 0.503857 0.408211 0.030 Uiso 1 1 calc R U . . .
H32B H 0.014503 0.581481 0.365361 0.030 Uiso 1 1 calc R U . . .
C24 C 0.8684(3) 0.7259(3) 0.3266(2) 0.0242(9) Uani 1 1 d . . . . .
H24 H 0.918708 0.720146 0.362681 0.029 Uiso 1 1 calc R U . . .
C1 C 0.5236(3) 0.8494(3) 0.1632(2) 0.0176(8) Uani 1 1 d . . . . .
N3 N 0.5796(2) 0.6774(2) 0.13652(17) 0.0172(7) Uani 1 1 d . . . . .
O3 O 0.3204(2) 0.7655(2) 0.27359(16) 0.0249(7) Uani 1 1 d . . . . .
C15 C 0.7092(3) 0.7406(3) 0.0855(2) 0.0198(9) Uani 1 1 d . . . . .
C10 C 0.5110(3) 0.5581(3) 0.1047(2) 0.0204(8) Uani 1 1 d . . . . .
H10 H 0.495714 0.505291 0.084397 0.024 Uiso 1 1 calc R U . . .
C26 C 0.7745(3) 0.8105(3) 0.2432(2) 0.0219(9) Uani 1 1 d . . . . .
H26 H 0.760648 0.863885 0.223564 0.026 Uiso 1 1 calc R U . . .
C2 C 0.6147(3) 0.9004(3) 0.0983(2) 0.0202(8) Uani 1 1 d . . . . .
H2 H 0.663660 0.905256 0.075987 0.024 Uiso 1 1 calc R U . . .
C40 C 0.1153(3) 0.8127(3) 0.1949(2) 0.0236(9) Uani 1 1 d . . . . .
H40A H 0.175162 0.795929 0.186926 0.028 Uiso 1 1 calc R U . . .
H40B H 0.084728 0.846452 0.156276 0.028 Uiso 1 1 calc R U . . .
C41 C 0.0604(3) 0.7366(3) 0.2014(2) 0.0274(10) Uani 1 1 d . . . . .
H41A H 0.003955 0.752666 0.215460 0.033 Uiso 1 1 calc R U . . .
H41B H 0.044465 0.707394 0.157914 0.033 Uiso 1 1 calc R U . . .
C36 C 0.1158(3) 0.9530(3) 0.4438(2) 0.0233(9) Uani 1 1 d . . . . .
H36A H 0.095571 0.985245 0.479413 0.028 Uiso 1 1 calc R U . . .
H36B H 0.068503 0.956922 0.402548 0.028 Uiso 1 1 calc R U . . .
C31 C 0.1337(3) 0.5486(3) 0.3008(2) 0.0249(9) Uani 1 1 d . . . . .
H31A H 0.107611 0.491767 0.297539 0.030 Uiso 1 1 calc R U . . .
H31B H 0.192610 0.545324 0.287084 0.030 Uiso 1 1 calc R U . . .
C30 C 0.0724(3) 0.6044(3) 0.2527(2) 0.0274(10) Uani 1 1 d . . . . .
H30A H 0.060282 0.578926 0.207560 0.033 Uiso 1 1 calc R U . . .
H30B H 0.014196 0.610841 0.267032 0.033 Uiso 1 1 calc R U . . .
C47 C 0.3309(3) 0.9528(3) 0.3826(2) 0.0239(9) Uani 1 1 d . . . . .
H47A H 0.348376 1.012202 0.389184 0.029 Uiso 1 1 calc R U . . .
H47B H 0.347182 0.933973 0.340481 0.029 Uiso 1 1 calc R U . . .
C33 C 0.0702(3) 0.6123(3) 0.4623(2) 0.0238(9) Uani 1 1 d . . . . .
H33A H 0.016274 0.598764 0.480614 0.029 Uiso 1 1 calc R U . . .
H33B H 0.124381 0.596369 0.495972 0.029 Uiso 1 1 calc R U . . .
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'
K K 0.3868 1.0657 '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'
B B 0.0090 0.0039 '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
3 -2 11 0.0658
2 3 -13 0.0446
9 2 -6 0.0524
6 8 2 0.0277
-8 6 1 0.0436
4 9 2 0.0243
-6 -8 -2 0.0079
10 0 0 0.0561
5 6 7 0.0395
-9 -4 7 0.0238
4 -8 4 0.0674
-7 -8 2 0.0105
7 -6 -7 0.0614
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
C28 Mn1 C27 83.3(2) . . ?
C28 Mn1 C29 88.25(19) . . ?
C27 Mn1 C29 94.34(19) . . ?
C28 Mn1 C8 161.45(18) . . ?
C27 Mn1 C8 88.07(18) . . ?
C29 Mn1 C8 108.80(18) . . ?
C28 Mn1 C1 94.11(18) . . ?
C27 Mn1 C1 148.77(18) . . ?
C29 Mn1 C1 116.74(17) . . ?
C8 Mn1 C1 84.84(17) . . ?
O8 K1 O4 139.73(10) . . ?
O8 K1 O9 110.77(10) . . ?
O4 K1 O9 60.74(9) . . ?
O8 K1 O5 61.15(9) . . ?
O4 K1 O5 107.33(10) . . ?
O9 K1 O5 153.16(9) . . ?
O8 K1 O7 85.01(10) . . ?
O4 K1 O7 132.98(9) . . ?
O9 K1 O7 95.50(9) . . ?
O5 K1 O7 108.48(9) . . ?
O8 K1 O6 119.41(10) . . ?
O4 K1 O6 95.90(9) . . ?
O9 K1 O6 118.54(9) . . ?
O5 K1 O6 85.18(9) . . ?
O7 K1 O6 58.35(9) . . ?
O8 K1 O3 69.48(10) . . ?
O4 K1 O3 71.20(9) . . ?
O9 K1 O3 68.38(9) . . ?
O5 K1 O3 85.18(9) . . ?
O7 K1 O3 140.85(9) . . ?
O6 K1 O3 160.72(9) . . ?
O8 K1 N6 60.94(10) . . ?
O4 K1 N6 122.01(10) . . ?
O9 K1 N6 61.60(10) . . ?
O5 K1 N6 121.42(10) . . ?
O7 K1 N6 58.43(9) . . ?
O6 K1 N6 116.32(10) . . ?
O3 K1 N6 82.93(10) . . ?
O8 K1 N5 120.40(10) . . ?
O4 K1 N5 60.88(10) . . ?
O9 K1 N5 120.52(10) . . ?
O5 K1 N5 59.33(9) . . ?
O7 K1 N5 116.19(9) . . ?
O6 K1 N5 58.30(9) . . ?
O3 K1 N5 102.45(10) . . ?
N6 K1 N5 174.61(10) . . ?
C30 O4 C41 112.2(3) . . ?
C30 O4 K1 119.8(3) . . ?
C41 O4 K1 115.2(3) . . ?
O3 C29 Mn1 170.6(4) . . ?
C33 O6 C34 111.3(3) . . ?
C33 O6 K1 118.9(2) . . ?
C34 O6 K1 112.5(3) . . ?
C43 O5 C44 112.3(3) . . ?
C43 O5 K1 111.1(2) . . ?
C44 O5 K1 110.7(3) . . ?
C10 C9 N3 108.2(4) . . ?
C26 C25 C24 120.2(4) . . ?
O8 C46 C47 109.3(4) . . ?
C47 N6 C38 110.5(3) . . ?
C47 N6 C37 111.1(3) . . ?
C38 N6 C37 108.6(3) . . ?
C47 N6 K1 104.3(3) . . ?
C38 N6 K1 108.6(3) . . ?
C37 N6 K1 113.7(3) . . ?
N6 C37 C36 112.4(4) . . ?
C35 O7 C36 111.8(3) . . ?
C35 O7 K1 116.7(3) . . ?
C36 O7 K1 115.1(2) . . ?
C18 C17 C16 119.0(4) . . ?
O7 C35 C34 109.2(4) . . ?
N2 C4 C6 109.5(3) . . ?
N2 C4 C5 110.3(3) . . ?
C6 C4 C5 108.5(4) . . ?
N2 C4 C7 108.5(3) . . ?
C6 C4 C7 112.1(3) . . ?
C5 C4 C7 107.9(4) . . ?
C2 C3 N2 107.2(4) . . ?
C19 C20 C15 121.5(4) . . ?
O9 C39 C38 109.0(3) . . ?
C1 N1 C2 109.8(3) . . ?
C1 N1 B1 124.1(3) . . ?
C2 N1 B1 126.0(3) . . ?
N6 C38 C39 114.5(4) . . ?
C22 C21 C26 115.9(4) . . ?
C22 C21 B1 122.3(4) . . ?
C26 C21 B1 120.6(4) . . ?
O8 C45 C44 108.2(4) . . ?
C46 O8 C45 112.7(3) . . ?
C46 O8 K1 123.8(3) . . ?
C45 O8 K1 116.7(3) . . ?
N4 C11 C12 110.3(3) . . ?
N4 C11 C13 109.8(3) . . ?
C12 C11 C13 107.3(4) . . ?
N4 C11 C14 108.7(3) . . ?
C12 C11 C14 109.2(4) . . ?
C13 C11 C14 111.6(4) . . ?
O5 C44 C45 109.6(4) . . ?
C8 N4 C10 109.9(3) . . ?
C8 N4 C11 127.3(3) . . ?
C10 N4 C11 122.7(4) . . ?
N3 B1 N1 106.7(3) . . ?
N3 B1 C21 111.4(4) . . ?
N1 B1 C21 112.4(3) . . ?
N3 B1 C15 108.6(3) . . ?
N1 B1 C15 108.6(3) . . ?
C21 B1 C15 109.0(3) . . ?
C18 C19 C20 121.0(4) . . ?
C24 C23 C22 120.4(4) . . ?
N5 C42 C43 113.4(4) . . ?
C19 C18 C17 119.7(4) . . ?
N4 C8 N3 105.6(3) . . ?
N4 C8 Mn1 137.0(3) . . ?
N3 C8 Mn1 116.5(3) . . ?
O6 C34 C35 109.4(4) . . ?
O1 C27 Mn1 175.7(4) . . ?
C1 N2 C3 109.7(3) . . ?
C1 N2 C4 126.6(3) . . ?
C3 N2 C4 123.5(3) . . ?
C32 N5 C42 110.4(4) . . ?
C32 N5 C31 110.8(4) . . ?
C42 N5 C31 109.3(4) . . ?
C32 N5 K1 110.7(3) . . ?
C42 N5 K1 110.5(3) . . ?
C31 N5 K1 105.0(3) . . ?
O2 C28 Mn1 172.8(4) . . ?
O5 C43 C42 109.0(4) . . ?
C40 O9 C39 111.0(3) . . ?
C40 O9 K1 111.0(2) . . ?
C39 O9 K1 110.0(2) . . ?
C15 C16 C17 123.0(4) . . ?
C21 C22 C23 122.1(4) . . ?
N5 C32 C33 112.8(4) . . ?
C23 C24 C25 119.1(4) . . ?
N1 C1 N2 105.1(3) . . ?
N1 C1 Mn1 116.4(3) . . ?
N2 C1 Mn1 137.8(3) . . ?
C8 N3 C9 109.4(3) . . ?
C8 N3 B1 125.5(4) . . ?
C9 N3 B1 125.0(3) . . ?
C29 O3 K1 160.4(3) . . ?
C16 C15 C20 115.8(4) . . ?
C16 C15 B1 122.9(4) . . ?
C20 C15 B1 121.2(4) . . ?
C9 C10 N4 106.8(4) . . ?
C25 C26 C21 122.3(4) . . ?
C3 C2 N1 108.2(4) . . ?
O9 C40 C41 109.6(4) . . ?
O4 C41 C40 108.1(4) . . ?
O7 C36 C37 108.7(3) . . ?
N5 C31 C30 114.6(4) . . ?
O4 C30 C31 110.0(4) . . ?
N6 C47 C46 114.1(4) . . ?
O6 C33 C32 110.0(4) . . ?
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 C28 1.782(5) . ?
Mn1 C27 1.787(5) . ?
Mn1 C29 1.788(4) . ?
Mn1 C8 2.072(4) . ?
Mn1 C1 2.090(4) . ?
K1 O8 2.703(3) . ?
K1 O4 2.789(3) . ?
K1 O9 2.847(3) . ?
K1 O5 2.859(3) . ?
K1 O7 2.916(3) . ?
K1 O6 2.922(3) . ?
K1 O3 2.963(3) . ?
K1 N6 3.005(4) . ?
K1 N5 3.063(4) . ?
O4 C30 1.410(6) . ?
O4 C41 1.426(5) . ?
C29 O3 1.175(5) . ?
O6 C33 1.416(5) . ?
O6 C34 1.422(5) . ?
O2 C28 1.180(6) . ?
O5 C43 1.419(6) . ?
O5 C44 1.426(6) . ?
C9 C10 1.342(6) . ?
C9 N3 1.384(6) . ?
C25 C26 1.385(6) . ?
C25 C24 1.388(7) . ?
C13 C11 1.531(6) . ?
C46 O8 1.422(6) . ?
C46 C47 1.510(6) . ?
N6 C47 1.468(6) . ?
N6 C38 1.470(5) . ?
N6 C37 1.477(5) . ?
C37 C36 1.495(6) . ?
O7 C35 1.416(5) . ?
O7 C36 1.420(5) . ?
C17 C18 1.382(7) . ?
C17 C16 1.404(6) . ?
C35 C34 1.499(7) . ?
C4 N2 1.492(5) . ?
C4 C6 1.520(6) . ?
C4 C5 1.532(6) . ?
C4 C7 1.541(6) . ?
C3 C2 1.337(6) . ?
C3 N2 1.396(5) . ?
C20 C19 1.390(6) . ?
C20 C15 1.408(6) . ?
C39 O9 1.433(5) . ?
C39 C38 1.509(6) . ?
N1 C1 1.372(5) . ?
N1 C2 1.382(5) . ?
N1 B1 1.575(6) . ?
C21 C22 1.393(6) . ?
C21 C26 1.408(6) . ?
C21 B1 1.619(6) . ?
C45 O8 1.427(6) . ?
C45 C44 1.490(7) . ?
C11 N4 1.505(5) . ?
C11 C12 1.528(6) . ?
C11 C14 1.534(6) . ?
N4 C8 1.365(6) . ?
N4 C10 1.395(5) . ?
B1 N3 1.561(6) . ?
B1 C15 1.649(6) . ?
C19 C18 1.377(7) . ?
C23 C24 1.377(7) . ?
C23 C22 1.398(6) . ?
C42 N5 1.470(6) . ?
C42 C43 1.506(6) . ?
C8 N3 1.369(5) . ?
C27 O1 1.169(6) . ?
N2 C1 1.373(5) . ?
N5 C32 1.468(5) . ?
N5 C31 1.484(6) . ?
O9 C40 1.417(5) . ?
C16 C15 1.397(6) . ?
C32 C33 1.499(6) . ?
C40 C41 1.496(7) . ?
C31 C30 1.501(7) . ?
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
2.7909 -1.9640 11.4283 0.8482 -0.2043 0.4887
2.0429 2.6682 -12.8120 -0.9727 0.2318 -0.0089
9.3972 1.9239 -5.5518 -0.4574 0.1050 0.8830
5.5589 8.1204 1.8829 -0.2448 -0.7048 0.6659
-8.0118 5.9473 0.8387 -0.2138 -0.5960 -0.7740
4.1533 9.0749 2.0121 -0.2795 -0.8012 0.5291
-5.9227 -7.8114 -1.8370 0.2339 0.6741 -0.7006
9.6664 0.0118 -0.2944 -0.0212 0.0878 0.9959
4.5590 6.0171 7.4340 0.2197 -0.7262 0.6515
-8.5024 -4.0135 6.5030 0.6155 0.0460 -0.7868
4.1860 -8.2767 4.4660 0.6726 0.5791 0.4608
-6.7795 -7.5214 2.1172 0.4835 0.5068 -0.7137
7.1836 -5.6264 -7.4124 -0.2374 0.7881 0.5680
