#------------------------------------------------------------------------------
#$Date: 2019-11-02 05:25:10 +0200 (Sat, 02 Nov 2019) $
#$Revision: 220699 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/74/4127426.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_4127426
loop_
_publ_author_name
'Barman, Suman K.'
'Jones, Jason R.'
'Sun, Chen'
'Hill, Ethan A.'
'Ziller, Joseph W.'
'Borovik, A. S.'
_publ_section_title
;
 Regulating the Basicity of Metal-Oxido Complexes with a Single Hydrogen
 Bond and Its Effect on C-H Bond Cleavage.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11142
_journal_page_last               11150
_journal_paper_doi               10.1021/jacs.9b03688
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C57 H103 K4 Mn2 N17 O15'
_chemical_formula_weight         1532.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.7945(9)
_cell_angle_beta                 105.6649(8)
_cell_angle_gamma                94.1267(9)
_cell_formula_units_Z            2
_cell_length_a                   14.9408(10)
_cell_length_b                   14.9961(10)
_cell_length_c                   20.1209(13)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.47
_cell_volume                     4244.3(5)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52660
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         1.519
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.166
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         20897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0873
_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)+(0.1348P)²+9.7536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14060
_reflns_number_total             20897
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b03688_si_002.cif
_cod_data_source_block           asb503
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4127426
_shelx_shelxl_version_number     2014/7
_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_min   0.805
_shelx_estimated_absorpt_t_max   0.913
_exptl_absorpt_special_details
; 
Reflections not merged 
52666 Corrected reflections written to file asb503s.hkl 
Estimated minimum and maximum transmission:  0.6917  0.7458 
The ratio (0.9275) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
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
Mn1 Mn 0.97712(4) 0.70503(4) 0.76643(3) 0.02553(15) Uani 1 1 d . .
Mn2 Mn 0.52086(4) 0.77790(4) 0.73977(3) 0.02898(16) Uani 1 1 d . .
K1 K 1.30203(7) 0.72773(8) 0.62709(6) 0.0491(3) Uani 1 1 d . .
K2 K 0.63534(8) 0.50799(9) 0.51554(5) 0.0513(3) Uani 1 1 d . .
K3 K 0.87075(7) 1.01695(7) 0.95132(5) 0.0412(3) Uani 1 1 d . .
K4 K 0.18187(6) 0.75954(6) 0.89054(5) 0.0359(2) Uani 1 1 d . .
O1 O 1.0061(2) 0.62323(19) 0.82017(15) 0.0327(6) Uani 1 1 d . .
O2 O 1.2178(2) 0.6355(2) 0.6984(2) 0.0496(9) Uani 1 1 d . .
O3 O 1.3783(5) 0.3230(5) 0.8722(5) 0.148(3) Uani 1 1 d . .
O4 O 0.9760(2) 0.8899(2) 0.95281(14) 0.0343(7) Uani 1 1 d . .
O5 O 0.7369(2) 0.5253(2) 0.64128(17) 0.0422(8) Uani 1 1 d . .
O6 O 0.4623(2) 0.8562(2) 0.69272(17) 0.0421(7) Uani 1 1 d . .
O7 O 0.3338(2) 0.8221(3) 0.8676(2) 0.0535(10) Uani 1 1 d . .
O8 O 0.0978(5) 1.1413(4) 0.7346(4) 0.113(2) Uani 1 1 d . .
O9 O 0.7666(2) 0.9704(2) 0.82520(17) 0.0410(7) Uani 1 1 d . .
O10 O 0.5149(3) 0.6139(2) 0.54511(16) 0.0482(9) Uani 1 1 d . .
O11 O 0.7456(2) 1.0822(2) 1.00968(18) 0.0466(8) Uani 1 1 d . .
O12 O 1.2122(5) 0.5991(6) 0.5121(3) 0.140(3) Uani 1 1 d . .
O14 O 1.2018(8) 0.8299(7) 0.5548(6) 0.243(5) Uani 1 1 d . .
O15 O 0.2549(8) 0.6891(7) 0.9903(6) 0.243(5) Uani 1 1 d . .
N1 N 0.9503(2) 0.8041(2) 0.70409(17) 0.0308(7) Uani 1 1 d . .
N2 N 1.0910(2) 0.6970(3) 0.72519(18) 0.0342(8) Uani 1 1 d . .
N3 N 0.9922(2) 0.8179(2) 0.84669(17) 0.0278(7) Uani 1 1 d . .
N4 N 0.8485(2) 0.6467(2) 0.70244(17) 0.0299(7) Uani 1 1 d . .
N5 N 1.1537(3) 0.5856(3) 0.7799(2) 0.0435(9) Uani 1 1 d . .
H1 H 1.1087 0.5932 0.8001 0.052 Uiso 1 1 calc R U
N6 N 1.0017(3) 0.7407(2) 0.93667(18) 0.0396(9) Uani 1 1 d . .
H6 H 1.0278 0.7005 0.9132 0.048 Uiso 1 1 calc R U
N7 N 0.8440(3) 0.5139(3) 0.7445(2) 0.0495(11) Uani 1 1 d . .
H7 H 0.8892 0.5437 0.7811 0.059 Uiso 1 1 calc R U
N8 N 0.5816(3) 0.6789(2) 0.79329(17) 0.0306(7) Uani 1 1 d . .
N9 N 0.4431(3) 0.7790(3) 0.8109(2) 0.0378(8) Uani 1 1 d . .
N10 N 0.6550(2) 0.8443(2) 0.78143(17) 0.0279(7) Uani 1 1 d . .
N11 N 0.4981(3) 0.6700(2) 0.65438(17) 0.0337(8) Uani 1 1 d . .
N12 N 0.3525(3) 0.8868(3) 0.7744(2) 0.0479(10) Uani 1 1 d . .
H12 H 0.3816 0.8828 0.7416 0.057 Uiso 1 1 calc R U
N13 N 0.6194(3) 0.9838(3) 0.7574(2) 0.0442(10) Uani 1 1 d . .
H13 H 0.5606 0.9589 0.7432 0.053 Uiso 1 1 calc R U
N14 N 0.4671(3) 0.7541(3) 0.5680(2) 0.0464(10) Uani 1 1 d . .
H14 H 0.4359 0.7859 0.5930 0.056 Uiso 1 1 calc R U
N15 N 0.5938(3) 1.0302(3) 0.9500(2) 0.0418(9) Uani 1 1 d . .
N16 N 1.0555(4) 0.5685(4) 0.4448(3) 0.0721(15) Uiso 1 1 d . .
C1 C 0.9945(3) 0.7811(3) 0.6467(2) 0.0399(10) Uani 1 1 d . .
H1A H 0.9979 0.8339 0.6236 0.048 Uiso 1 1 calc R U
H1B H 0.9555 0.7292 0.6110 0.048 Uiso 1 1 calc R U
C2 C 1.0921(3) 0.7561(3) 0.6749(2) 0.0384(10) Uani 1 1 d . .
H2A H 1.1133 0.7242 0.6357 0.046 Uiso 1 1 calc R U
H2B H 1.1364 0.8120 0.6982 0.046 Uiso 1 1 calc R U
C3 C 0.9933(3) 0.8937(3) 0.7495(2) 0.0388(10) Uani 1 1 d . .
H3A H 0.9667 0.9429 0.7264 0.047 Uiso 1 1 calc R U
H3B H 1.0616 0.9006 0.7556 0.047 Uiso 1 1 calc R U
C4 C 0.9760(3) 0.9028(3) 0.8217(2) 0.0329(9) Uani 1 1 d . .
H4A H 1.0189 0.9543 0.8552 0.039 Uiso 1 1 calc R U
H4B H 0.9107 0.9150 0.8180 0.039 Uiso 1 1 calc R U
C5 C 0.8464(3) 0.7982(3) 0.6767(2) 0.0376(10) Uani 1 1 d . .
H5A H 0.8300 0.8316 0.6376 0.045 Uiso 1 1 calc R U
H5B H 0.8210 0.8272 0.7145 0.045 Uiso 1 1 calc R U
C6 C 0.8028(3) 0.6992(3) 0.6508(2) 0.0330(9) Uani 1 1 d . .
H6A H 0.7347 0.6945 0.6456 0.040 Uiso 1 1 calc R U
H6B H 0.8119 0.6753 0.6044 0.040 Uiso 1 1 calc R U
C7 C 1.1581(3) 0.6394(3) 0.7319(2) 0.0385(10) Uani 1 1 d . .
C8 C 1.2119(4) 0.5200(3) 0.8008(3) 0.0504(13) Uani 1 1 d . .
C9 C 1.2940(4) 0.5054(4) 0.7813(4) 0.0639(17) Uani 1 1 d . .
H9 H 1.3134 0.5414 0.7520 0.077 Uiso 1 1 calc R U
C10 C 1.3457(5) 0.4396(5) 0.8043(5) 0.091(3) Uani 1 1 d . .
H10 H 1.4007 0.4297 0.7904 0.109 Uiso 1 1 calc R U
C11 C 1.3192(5) 0.3868(5) 0.8478(6) 0.099(3) Uani 1 1 d . .
C12 C 1.2389(5) 0.4007(5) 0.8692(5) 0.083(2) Uani 1 1 d . .
H12A H 1.2212 0.3659 0.8999 0.100 Uiso 1 1 calc R U
C13 C 1.1858(4) 0.4667(4) 0.8444(4) 0.0641(16) Uani 1 1 d . .
H13A H 1.1301 0.4757 0.8574 0.077 Uiso 1 1 calc R U
C14 C 1.3503(9) 0.2646(8) 0.9108(13) 0.265(13) Uani 1 1 d . .
H14A H 1.4052 0.2534 0.9466 0.397 Uiso 1 1 calc R U
H14B H 1.3198 0.2068 0.8794 0.397 Uiso 1 1 calc R U
H14C H 1.3062 0.2922 0.9338 0.397 Uiso 1 1 calc R U
C15 C 0.9875(3) 0.8197(3) 0.9131(2) 0.0293(8) Uani 1 1 d . .
C16 C 0.9774(4) 0.7164(4) 0.9980(2) 0.0453(12) Uani 1 1 d . .
C17 C 0.9961(6) 0.6194(4) 0.9989(3) 0.073(2) Uani 1 1 d . .
H17A H 0.9570 0.5798 0.9552 0.110 Uiso 1 1 calc R U
H17B H 0.9811 0.6004 1.0392 0.110 Uiso 1 1 calc R U
H17C H 1.0623 0.6149 1.0026 0.110 Uiso 1 1 calc R U
C18 C 0.8733(4) 0.7274(6) 0.9921(3) 0.080(2) Uani 1 1 d . .
H18A H 0.8617 0.7892 0.9854 0.120 Uiso 1 1 calc R U
H18B H 0.8596 0.7172 1.0354 0.120 Uiso 1 1 calc R U
H18C H 0.8329 0.6828 0.9519 0.120 Uiso 1 1 calc R U
C19 C 1.0382(4) 0.7770(4) 1.0664(2) 0.0458(11) Uani 1 1 d . .
H19A H 1.1040 0.7804 1.0665 0.069 Uiso 1 1 calc R U
H19B H 1.0308 0.7511 1.1065 0.069 Uiso 1 1 calc R U
H19C H 1.0189 0.8383 1.0702 0.069 Uiso 1 1 calc R U
C20 C 0.8066(3) 0.5604(3) 0.6933(2) 0.0330(9) Uani 1 1 d . .
C21 C 0.8149(4) 0.4177(3) 0.7438(3) 0.0468(12) Uani 1 1 d . .
C22 C 0.7128(4) 0.4038(4) 0.7431(3) 0.0534(13) Uani 1 1 d . .
H22A H 0.7052 0.4399 0.7863 0.080 Uiso 1 1 calc R U
H22B H 0.6939 0.3391 0.7406 0.080 Uiso 1 1 calc R U
H22C H 0.6736 0.4236 0.7021 0.080 Uiso 1 1 calc R U
C23 C 0.8312(5) 0.3537(4) 0.6805(4) 0.0655(16) Uani 1 1 d . .
H23A H 0.7942 0.3688 0.6366 0.098 Uiso 1 1 calc R U
H23B H 0.8120 0.2903 0.6818 0.098 Uiso 1 1 calc R U
H23C H 0.8978 0.3615 0.6830 0.098 Uiso 1 1 calc R U
C24 C 0.8769(4) 0.3981(4) 0.8125(4) 0.0686(19) Uani 1 1 d . .
H24A H 0.9428 0.4072 0.8132 0.103 Uiso 1 1 calc R U
H24B H 0.8603 0.3349 0.8158 0.103 Uiso 1 1 calc R U
H24C H 0.8673 0.4396 0.8525 0.103 Uiso 1 1 calc R U
C25 C 0.5663(4) 0.6938(3) 0.8640(2) 0.0387(10) Uani 1 1 d . .
H25A H 0.6120 0.7447 0.8957 0.046 Uiso 1 1 calc R U
H25B H 0.5765 0.6382 0.8841 0.046 Uiso 1 1 calc R U
C26 C 0.4675(4) 0.7158(3) 0.8590(3) 0.0442(11) Uani 1 1 d . .
H26A H 0.4229 0.6591 0.8416 0.053 Uiso 1 1 calc R U
H26B H 0.4635 0.7439 0.9062 0.053 Uiso 1 1 calc R U
C27 C 0.6828(3) 0.6914(3) 0.7980(2) 0.0345(9) Uani 1 1 d . .
H27A H 0.6916 0.6679 0.7514 0.041 Uiso 1 1 calc R U
H27B H 0.7175 0.6564 0.8319 0.041 Uiso 1 1 calc R U
C28 C 0.7216(3) 0.7923(3) 0.8218(2) 0.0332(9) Uani 1 1 d . .
H28A H 0.7295 0.8120 0.8728 0.040 Uiso 1 1 calc R U
H28B H 0.7834 0.8026 0.8133 0.040 Uiso 1 1 calc R U
C29 C 0.5334(4) 0.5888(3) 0.7504(2) 0.0388(10) Uani 1 1 d . .
H29A H 0.4694 0.5793 0.7552 0.047 Uiso 1 1 calc R U
H29B H 0.5681 0.5396 0.7678 0.047 Uiso 1 1 calc R U
C30 C 0.5280(3) 0.5845(3) 0.6735(2) 0.0377(10) Uani 1 1 d . .
H30A H 0.5901 0.5765 0.6662 0.045 Uiso 1 1 calc R U
H30B H 0.4826 0.5322 0.6437 0.045 Uiso 1 1 calc R U
C31 C 0.3742(3) 0.8281(3) 0.8210(3) 0.0432(11) Uani 1 1 d . .
C32 C 0.2900(4) 0.9512(4) 0.7734(4) 0.0604(16) Uani 1 1 d . .
C33 C 0.2538(3) 0.9846(4) 0.8278(4) 0.0681(19) Uani 1 1 d . .
H33 H 0.2710 0.9644 0.8712 0.082 Uiso 1 1 calc R U
C34 C 0.1881(4) 1.0524(4) 0.8161(5) 0.079(2) Uani 1 1 d . .
H34 H 0.1624 1.0787 0.8522 0.095 Uiso 1 1 calc R U
C35 C 0.1646(5) 1.0768(5) 0.7502(5) 0.079(2) Uani 1 1 d . .
C36 C 0.2011(6) 1.0486(6) 0.6983(5) 0.093(2) Uani 1 1 d . .
H36 H 0.1856 1.0711 0.6558 0.111 Uiso 1 1 calc R U
C37 C 0.2630(5) 0.9848(5) 0.7094(5) 0.078(2) Uani 1 1 d . .
H37 H 0.2890 0.9621 0.6726 0.093 Uiso 1 1 calc R U
C38 C 0.0620(7) 1.1703(5) 0.7893(5) 0.114(4) Uani 1 1 d . .
H38A H 0.0262 1.2212 0.7794 0.171 Uiso 1 1 calc R U
H38B H 0.1134 1.1905 0.8327 0.171 Uiso 1 1 calc R U
H38C H 0.0207 1.1200 0.7948 0.171 Uiso 1 1 calc R U
C39 C 0.6855(3) 0.9334(3) 0.7893(2) 0.0330(9) Uani 1 1 d . .
C40 C 0.6389(4) 1.0756(3) 0.7450(3) 0.0497(13) Uani 1 1 d . .
C41 C 0.7060(6) 1.0774(5) 0.7025(4) 0.083(2) Uani 1 1 d . .
H41A H 0.7675 1.0662 0.7302 0.125 Uiso 1 1 calc R U
H41B H 0.7113 1.1372 0.6895 0.125 Uiso 1 1 calc R U
H41C H 0.6834 1.0299 0.6597 0.125 Uiso 1 1 calc R U
C42 C 0.6749(5) 1.1448(3) 0.8136(3) 0.0588(15) Uani 1 1 d . .
H42A H 0.6284 1.1448 0.8399 0.088 Uiso 1 1 calc R U
H42B H 0.6859 1.2056 0.8034 0.088 Uiso 1 1 calc R U
H42C H 0.7337 1.1286 0.8418 0.088 Uiso 1 1 calc R U
C43 C 0.5436(5) 1.0999(4) 0.7033(4) 0.0712(19) Uani 1 1 d . .
H43A H 0.5177 1.0541 0.6599 0.107 Uiso 1 1 calc R U
H43B H 0.5527 1.1601 0.6916 0.107 Uiso 1 1 calc R U
H43C H 0.5000 1.1009 0.7321 0.107 Uiso 1 1 calc R U
C44 C 0.4966(3) 0.6762(3) 0.5875(2) 0.0393(11) Uani 1 1 d . .
C45 C 0.4842(5) 0.7888(4) 0.5079(3) 0.070(2) Uani 1 1 d . .
C46 C 0.4418(7) 0.8806(5) 0.5094(3) 0.100(3) Uani 1 1 d . .
H46A H 0.3740 0.8690 0.5019 0.151 Uiso 1 1 calc R U
H46B H 0.4539 0.9096 0.4720 0.151 Uiso 1 1 calc R U
H46C H 0.4707 0.9210 0.5552 0.151 Uiso 1 1 calc R U
C47 C 0.4306(8) 0.7248(5) 0.4388(3) 0.112(4) Uani 1 1 d . .
H47A H 0.4575 0.6671 0.4355 0.168 Uiso 1 1 calc R U
H47B H 0.4354 0.7531 0.3992 0.168 Uiso 1 1 calc R U
H47C H 0.3646 0.7132 0.4372 0.168 Uiso 1 1 calc R U
C48 C 0.5865(6) 0.8067(6) 0.5168(4) 0.103(3) Uani 1 1 d . .
H48A H 0.6171 0.8459 0.5629 0.154 Uiso 1 1 calc R U
H48B H 0.5965 0.8371 0.4796 0.154 Uiso 1 1 calc R U
H48C H 0.6131 0.7488 0.5140 0.154 Uiso 1 1 calc R U
C49 C 0.6644(3) 1.0944(3) 0.9826(3) 0.0423(11) Uani 1 1 d . .
H49 H 0.6514 1.1558 0.9855 0.051 Uiso 1 1 calc R U
C50 C 0.5036(4) 1.0495(4) 0.9118(3) 0.0590(15) Uani 1 1 d . .
H50A H 0.5017 1.1156 0.9201 0.088 Uiso 1 1 calc R U
H50B H 0.4548 1.0200 0.9279 0.088 Uiso 1 1 calc R U
H50C H 0.4926 1.0261 0.8614 0.088 Uiso 1 1 calc R U
C51 C 0.6078(4) 0.9342(3) 0.9430(3) 0.0523(13) Uani 1 1 d . .
H51A H 0.6149 0.9117 0.8963 0.078 Uiso 1 1 calc R U
H51B H 0.5535 0.8990 0.9488 0.078 Uiso 1 1 calc R U
H51C H 0.6643 0.9274 0.9792 0.078 Uiso 1 1 calc R U
C52 C 1.1472(7) 0.5512(7) 0.4653(5) 0.102(3) Uiso 1 1 d . .
H52 H 1.1620 0.4969 0.4408 0.122 Uiso 1 1 calc R U
C53 C 0.9977(7) 0.4978(6) 0.3898(5) 0.103(3) Uiso 1 1 d . .
H53A H 1.0343 0.4479 0.3806 0.154 Uiso 1 1 calc R U
H53B H 0.9749 0.5222 0.3470 0.154 Uiso 1 1 calc R U
H53C H 0.9442 0.4749 0.4043 0.154 Uiso 1 1 calc R U
C54 C 1.0178(9) 0.6461(9) 0.4718(7) 0.150(5) Uiso 1 1 d . .
H54A H 0.9877 0.6756 0.4331 0.226 Uiso 1 1 calc R U
H54B H 1.0683 0.6891 0.5062 0.226 Uiso 1 1 calc R U
H54C H 0.9715 0.6272 0.4947 0.226 Uiso 1 1 calc R U
O13 O 0.7223(8) 0.5997(7) 0.4476(7) 0.247(6) Uiso 1 1 d G .
C55 C 0.7541(7) 0.6113(6) 0.3996(6) 0.260(10) Uiso 1 1 d G .
H55 H 0.7540 0.5588 0.3657 0.312 Uiso 1 1 calc R U
N17 N 0.7899(6) 0.6928(6) 0.3901(5) 0.250(7) Uiso 1 1 d G .
C56 C 0.7927(12) 0.7765(6) 0.4395(8) 0.258(10) Uiso 1 1 d G .
H56A H 0.7441 0.8120 0.4181 0.386 Uiso 1 1 calc R U
H56B H 0.8543 0.8123 0.4515 0.386 Uiso 1 1 calc R U
H56C H 0.7814 0.7615 0.4824 0.386 Uiso 1 1 calc R U
C57 C 0.8262(10) 0.6995(10) 0.3310(7) 0.208(7) Uiso 1 1 d G .
H57A H 0.8904 0.7307 0.3483 0.312 Uiso 1 1 calc R U
H57B H 0.7867 0.7342 0.3001 0.312 Uiso 1 1 calc R U
H57C H 0.8259 0.6382 0.3045 0.312 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 0.0033 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'
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'
K K 0.2009 0.2494 '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'
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
O1 Mn1 N4 101.02(14) . .
O1 Mn1 N3 97.71(13) . .
N4 Mn1 N3 121.45(14) . .
O1 Mn1 N2 96.38(15) . .
N4 Mn1 N2 117.97(14) . .
N3 Mn1 N2 114.22(14) . .
O1 Mn1 N1 177.01(14) . .
N4 Mn1 N1 81.72(13) . .
N3 Mn1 N1 81.74(13) . .
N2 Mn1 N1 81.22(15) . .
O1 Mn1 K4 65.42(9) . 1_655
N4 Mn1 K4 166.35(10) . 1_655
N3 Mn1 K4 61.69(10) . 1_655
N2 Mn1 K4 67.44(10) . 1_655
N1 Mn1 K4 111.86(10) . 1_655
O6 Mn2 N10 102.42(14) . .
O6 Mn2 N9 97.26(16) . .
N10 Mn2 N9 114.82(14) . .
O6 Mn2 N11 97.16(15) . .
N10 Mn2 N11 116.98(14) . .
N9 Mn2 N11 121.16(14) . .
O6 Mn2 N8 176.03(14) . .
N10 Mn2 N8 81.55(13) . .
N9 Mn2 N8 80.95(15) . .
N11 Mn2 N8 80.86(14) . .
O6 Mn2 K1 56.34(11) . 1_455
N10 Mn2 K1 156.79(10) . 1_455
N9 Mn2 K1 79.94(11) . 1_455
N11 Mn2 K1 62.53(11) . 1_455
N8 Mn2 K1 119.75(10) . 1_455
O14 K1 O2 115.9(3) . .
O14 K1 O12 81.5(3) . .
O2 K1 O12 86.89(16) . .
O14 K1 O6 98.0(2) . 1_655
O2 K1 O6 122.61(11) . 1_655
O12 K1 O6 145.74(15) . 1_655
O5 K2 O10 95.88(11) . .
O5 K2 O13 109.1(3) . .
O10 K2 O13 103.5(3) . .
O5 K2 O10 124.98(11) . 2_666
O10 K2 O10 84.07(12) . 2_666
O13 K2 O10 124.4(3) . 2_666
O9 K3 O4 99.35(10) . .
O9 K3 O11 98.32(11) . .
O4 K3 O11 141.44(12) . .
O9 K3 O4 151.10(11) . 2_777
O4 K3 O4 82.13(10) . 2_777
O11 K3 O4 97.99(10) . 2_777
O15 K4 O7 97.6(3) . .
O15 K4 O11 81.8(3) . 2_677
O7 K4 O11 73.16(11) . 2_677
O15 K4 N3 130.4(4) . 1_455
O7 K4 N3 128.34(12) . 1_455
O11 K4 N3 93.46(10) 2_677 1_455
Mn1 O1 N5 94.56(16) . .
Mn1 O1 N6 92.33(14) . .
N5 O1 N6 127.15(17) . .
Mn1 O1 N7 90.28(14) . .
N5 O1 N7 115.01(17) . .
N6 O1 N7 117.28(18) . .
Mn1 O1 K4 82.72(10) . 1_655
N5 O1 K4 64.59(11) . 1_655
N6 O1 K4 64.51(11) . 1_655
N7 O1 K4 172.90(14) . 1_655
C7 O2 K1 143.1(3) . .
C14 O3 C11 119.2(8) . .
C15 O4 K3 140.3(3) . .
C15 O4 K3 116.8(2) . 2_777
K3 O4 K3 97.87(10) . 2_777
C20 O5 K2 153.7(3) . .
Mn2 O6 N12 93.71(17) . .
Mn2 O6 N14 91.10(16) . .
N12 O6 N14 141.92(18) . .
Mn2 O6 N13 88.12(14) . .
N12 O6 N13 104.16(17) . .
N14 O6 N13 113.74(17) . .
Mn2 O6 K1 92.23(13) . 1_455
N12 O6 K1 75.59(12) . 1_455
N14 O6 K1 66.48(12) . 1_455
N13 O6 K1 179.58(17) . 1_455
C31 O7 K4 144.5(3) . .
C38 O8 C35 112.8(8) . .
C39 O9 K3 141.9(3) . .
C44 O10 K2 148.1(3) . .
C44 O10 K2 109.9(3) . 2_666
K2 O10 K2 95.93(11) . 2_666
C49 O11 K3 130.2(3) . .
C49 O11 K4 103.7(3) . 2_677
K3 O11 K4 112.30(12) . 2_677
C52 O12 K1 159.6(7) . .
C52 O12 K2 96.5(6) . 2_766
K1 O12 K2 103.5(2) . 2_766
C3 N1 C1 111.0(3) . .
C3 N1 C5 112.6(4) . .
C1 N1 C5 112.0(3) . .
C3 N1 Mn1 107.5(3) . .
C1 N1 Mn1 107.0(3) . .
C5 N1 Mn1 106.3(2) . .
C7 N2 C2 115.1(4) . .
C7 N2 Mn1 130.7(3) . .
C2 N2 Mn1 113.8(3) . .
C7 N2 K4 83.0(2) . 1_655
C2 N2 K4 123.9(3) . 1_655
Mn1 N2 K4 75.24(10) . 1_655
C15 N3 C4 114.7(3) . .
C15 N3 Mn1 128.4(3) . .
C4 N3 Mn1 113.8(2) . .
C15 N3 K4 88.0(2) . 1_655
C4 N3 K4 122.7(2) . 1_655
Mn1 N3 K4 80.22(11) . 1_655
C20 N4 C6 115.1(3) . .
C20 N4 Mn1 128.7(3) . .
C6 N4 Mn1 115.2(3) . .
C7 N5 C8 128.2(4) . .
C7 N5 O1 105.5(3) . .
C8 N5 O1 126.2(3) . .
C7 N5 K4 88.1(2) . 1_655
C8 N5 K4 114.6(3) . 1_655
O1 N5 K4 64.70(11) . 1_655
C15 N6 C16 125.8(4) . .
C15 N6 O1 102.8(3) . .
C16 N6 O1 126.2(3) . .
C15 N6 K4 83.4(3) . 1_655
C16 N6 K4 135.8(3) . 1_655
O1 N6 K4 63.26(11) . 1_655
C20 N7 C21 125.4(4) . .
C20 N7 O1 102.8(3) . .
C21 N7 O1 129.7(3) . .
C25 N8 C27 111.7(3) . .
C25 N8 C29 111.0(3) . .
C27 N8 C29 112.5(3) . .
C25 N8 Mn2 108.6(3) . .
C27 N8 Mn2 106.3(2) . .
C29 N8 Mn2 106.5(3) . .
C31 N9 C26 114.2(4) . .
C31 N9 Mn2 131.3(4) . .
C26 N9 Mn2 114.5(3) . .
C39 N10 C28 115.1(3) . .
C39 N10 Mn2 129.0(3) . .
C28 N10 Mn2 114.4(2) . .
C44 N11 C30 113.3(4) . .
C44 N11 Mn2 126.7(3) . .
C30 N11 Mn2 114.3(2) . .
C44 N11 K1 89.4(3) . 1_455
C30 N11 K1 127.7(3) . 1_455
Mn2 N11 K1 80.13(12) . 1_455
C31 N12 C32 127.6(5) . .
C31 N12 O6 104.9(3) . .
C32 N12 O6 127.5(4) . .
C31 N12 K1 96.6(3) . 1_455
C32 N12 K1 114.5(3) . 1_455
O6 N12 K1 54.79(11) . 1_455
C39 N13 C40 125.3(4) . .
C39 N13 O6 103.7(3) . .
C40 N13 O6 128.9(3) . .
C44 N14 C45 124.2(5) . .
C44 N14 O6 102.2(3) . .
C45 N14 O6 126.5(4) . .
C44 N14 K1 89.5(3) . 1_455
C45 N14 K1 136.6(4) . 1_455
O6 N14 K1 58.18(11) . 1_455
C49 N15 C50 122.8(5) . .
C49 N15 C51 120.5(4) . .
C50 N15 C51 116.2(4) . .
C52 N16 C54 126.8(9) . .
C52 N16 C53 112.2(7) . .
C54 N16 C53 120.9(8) . .
N1 C1 C2 111.0(4) . .
N2 C2 C1 109.3(3) . .
N1 C3 C4 111.3(3) . .
N3 C4 C3 108.6(3) . .
N1 C5 C6 110.6(4) . .
N4 C6 C5 108.1(3) . .
O2 C7 N2 124.5(5) . .
O2 C7 N5 123.0(4) . .
N2 C7 N5 112.5(4) . .
O2 C7 K4 127.5(3) . 1_655
N2 C7 K4 72.8(2) . 1_655
N5 C7 K4 67.4(2) . 1_655
C13 C8 N5 116.8(5) . .
C13 C8 C9 118.5(5) . .
N5 C8 C9 124.6(5) . .
C10 C9 C8 120.2(6) . .
C9 C10 C11 120.9(6) . .
C10 C11 C12 120.4(6) . .
C10 C11 O3 117.9(7) . .
C12 C11 O3 121.7(8) . .
C13 C12 C11 118.2(7) . .
C12 C13 C8 121.8(6) . .
O4 C15 N3 123.7(4) . .
O4 C15 N6 121.0(4) . .
N3 C15 N6 115.2(4) . .
O4 C15 K4 127.7(3) . 1_655
N3 C15 K4 67.2(2) . 1_655
N6 C15 K4 71.9(2) . 1_655
O4 C15 K3 44.06(19) . 2_777
N3 C15 K3 119.5(2) . 2_777
N6 C15 K3 103.5(2) . 2_777
K4 C15 K3 84.53(9) 1_655 2_777
N6 C16 C17 106.7(4) . .
N6 C16 C19 111.2(4) . .
C17 C16 C19 108.8(4) . .
N6 C16 C18 110.2(4) . .
C17 C16 C18 111.6(5) . .
C19 C16 C18 108.5(5) . .
C16 C19 K3 114.8(3) . 2_777
O5 C20 N4 122.8(4) . .
O5 C20 N7 121.8(4) . .
N4 C20 N7 115.4(4) . .
N7 C21 C22 110.5(4) . .
N7 C21 C24 105.3(4) . .
C22 C21 C24 109.3(5) . .
N7 C21 C23 111.3(5) . .
C22 C21 C23 110.6(4) . .
C24 C21 C23 109.7(5) . .
N8 C25 C26 110.4(4) . .
N9 C26 C25 109.3(3) . .
N8 C27 C28 110.2(3) . .
N10 C28 C27 108.0(3) . .
N8 C29 C30 110.3(3) . .
N11 C30 C29 108.2(3) . .
O7 C31 N9 124.1(5) . .
O7 C31 N12 123.2(5) . .
N9 C31 N12 112.8(4) . .
C33 C32 N12 126.2(7) . .
C33 C32 C37 118.9(6) . .
N12 C32 C37 114.9(6) . .
C32 C33 C34 117.9(7) . .
C35 C34 C33 117.6(7) . .
C36 C35 C34 125.7(7) . .
C36 C35 O8 113.9(8) . .
C34 C35 O8 120.4(7) . .
C35 C36 C37 116.5(9) . .
C36 C37 C32 123.3(8) . .
O9 C39 N10 124.1(4) . .
O9 C39 N13 121.2(4) . .
N10 C39 N13 114.7(4) . .
N13 C40 C41 111.0(5) . .
N13 C40 C42 111.5(4) . .
C41 C40 C42 110.6(5) . .
N13 C40 C43 105.7(4) . .
C41 C40 C43 109.5(5) . .
C42 C40 C43 108.3(5) . .
O10 C44 N11 123.8(5) . .
O10 C44 N14 121.7(4) . .
N11 C44 N14 114.4(4) . .
O10 C44 K2 49.1(2) . 2_666
N11 C44 K2 106.4(3) . 2_666
N14 C44 K2 112.2(3) . 2_666
O10 C44 K1 134.1(3) . 1_455
N11 C44 K1 66.5(3) . 1_455
N14 C44 K1 66.3(3) . 1_455
K2 C44 K1 85.19(10) 2_666 1_455
N14 C45 C48 110.8(5) . .
N14 C45 C47 110.6(5) . .
C48 C45 C47 113.4(7) . .
N14 C45 C46 104.9(6) . .
C48 C45 C46 109.1(6) . .
C47 C45 C46 107.7(6) . .
O11 C49 N15 126.1(5) . .
O11 C49 K4 55.0(2) . 2_677
N15 C49 K4 160.7(4) . 2_677
O12 C52 N16 126.6(10) . .
O12 C52 K2 62.1(6) . 2_766
N16 C52 K2 169.7(6) . 2_766
C55 O13 K2 155.9(5) . .
O13 C55 N17 126.0 . .
C55 N17 C57 121.8 . .
C55 N17 C56 120.5 . .
C57 N17 C56 117.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 1.771(3) .
Mn1 N4 2.039(3) .
Mn1 N3 2.084(3) .
Mn1 N2 2.087(3) .
Mn1 N1 2.095(4) .
Mn1 K4 3.3291(11) 1_655
Mn2 O6 1.766(3) .
Mn2 N10 2.058(3) .
Mn2 N9 2.072(4) .
Mn2 N11 2.084(3) .
Mn2 N8 2.097(4) .
Mn2 K1 3.3850(12) 1_455
K1 O14 2.572(7) .
K1 O2 2.637(4) .
K1 O12 2.703(5) .
K1 O6 2.820(3) 1_655
K2 O5 2.533(3) .
K2 O10 2.604(4) .
K2 O13 2.606(11) .
K2 O10 2.653(3) 2_666
K3 O9 2.541(3) .
K3 O4 2.554(3) .
K3 O11 2.625(3) .
K3 O4 2.675(3) 2_777
K4 O15 2.458(7) .
K4 O7 2.579(4) .
K4 O11 2.769(3) 2_677
K4 N3 2.974(4) 1_455
O1 N5 2.613(5) .
O1 N6 2.701(5) .
O1 N7 2.732(5) .
O1 K4 3.052(3) 1_655
O2 C7 1.253(5) .
O3 C14 1.377(16) .
O3 C11 1.408(9) .
O4 C15 1.262(5) .
O4 K3 2.675(3) 2_777
O5 C20 1.265(5) .
O6 N12 2.629(6) .
O6 N14 2.730(6) .
O6 N13 2.779(5) .
O6 K1 2.820(3) 1_455
O7 C31 1.257(6) .
O8 C38 1.369(9) .
O8 C35 1.450(9) .
O9 C39 1.262(5) .
O10 C44 1.252(6) .
O10 K2 2.653(3) 2_666
O11 C49 1.228(6) .
O11 K4 2.769(3) 2_677
O12 C52 1.233(10) .
O12 K2 2.997(8) 2_766
N1 C3 1.481(5) .
N1 C1 1.481(5) .
N1 C5 1.491(6) .
N2 C7 1.364(6) .
N2 C2 1.455(6) .
N2 K4 3.179(4) 1_655
N3 C15 1.352(5) .
N3 C4 1.459(5) .
N3 K4 2.974(4) 1_655
N4 C20 1.357(5) .
N4 C6 1.462(5) .
N5 C7 1.372(7) .
N5 C8 1.403(6) .
N5 K4 3.049(4) 1_655
N6 C15 1.358(6) .
N6 C16 1.472(6) .
N6 K4 3.085(4) 1_655
N7 C20 1.361(6) .
N7 C21 1.473(6) .
N8 C25 1.484(5) .
N8 C27 1.485(6) .
N8 C29 1.490(5) .
N9 C31 1.347(6) .
N9 C26 1.462(6) .
N10 C39 1.348(5) .
N10 C28 1.467(5) .
N11 C44 1.358(5) .
N11 C30 1.467(6) .
N11 K1 3.048(4) 1_455
N12 C31 1.384(7) .
N12 C32 1.389(7) .
N12 K1 3.343(4) 1_455
N13 C39 1.375(6) .
N13 C40 1.462(6) .
N14 C44 1.361(7) .
N14 C45 1.469(6) .
N14 K1 3.043(5) 1_455
N15 C49 1.318(6) .
N15 C50 1.437(7) .
N15 C51 1.459(7) .
N16 C52 1.377(11) .
N16 C54 1.418(12) .
N16 C53 1.431(10) .
C1 C2 1.515(7) .
C3 C4 1.528(6) .
C5 C6 1.520(6) .
C7 K4 3.302(4) 1_655
C8 C13 1.392(8) .
C8 C9 1.406(8) .
C9 C10 1.363(9) .
C10 C11 1.389(11) .
C11 C12 1.398(10) .
C12 C13 1.389(9) .
C15 K4 3.225(4) 1_655
C15 K3 3.434(4) 2_777
C16 C17 1.502(8) .
C16 C19 1.525(6) .
C16 C18 1.550(9) .
C19 K3 3.400(6) 2_777
C21 C22 1.521(8) .
C21 C24 1.529(7) .
C21 C23 1.545(8) .
C25 C26 1.517(7) .
C27 C28 1.526(6) .
C29 C30 1.517(6) .
C32 C33 1.382(9) .
C32 C37 1.432(10) .
C33 C34 1.467(10) .
C34 C35 1.395(11) .
C35 C36 1.326(11) .
C36 C37 1.381(10) .
C40 C41 1.485(9) .
C40 C42 1.517(7) .
C40 C43 1.548(9) .
C44 K2 3.298(4) 2_666
C44 K1 3.323(5) 1_455
C45 C48 1.488(11) .
C45 C47 1.527(8) .
C45 C46 1.555(11) .
C49 K4 3.285(5) 2_677
C52 K2 3.368(10) 2_766
O13 C55 1.2164 .
C55 N17 1.3627 .
N17 C57 1.4498 .
N17 C56 1.4532 .
