#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:49:18 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228741 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/93/1549312.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_1549312
loop_
_publ_author_name
'Halbach, Robert L.'
'Gygi, David'
'Bloch, Eric D.'
'Anderson, Bryce L.'
'Nocera, Daniel G.'
_publ_section_title
;
 Structurally characterized terminal manganese(iv) oxo tris(alkoxide)
 complex.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              4524
_journal_page_last               4528
_journal_paper_doi               10.1039/c8sc01164h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C38 H79 K Mn O5'
_chemical_formula_sum            'C38 H79 K Mn O5'
_chemical_formula_weight         710.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-12 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.0930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3234(12)
_cell_length_b                   15.9361(10)
_cell_length_c                   16.7710(11)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.847
_cell_measurement_theta_min      2.556
_cell_volume                     4148.8(5)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36865
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8188.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.424
_exptl_crystal_size_min          0.422
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0517
_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)+(0.0693P)²+7.9685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4277
_reflns_number_total             4972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8sc01164h2.cif
_cod_data_source_block           cmpd_1_mn(ditox)3k(thf)2
_cod_depositor_comments
'Adding full bibliography for 1549310--1549312.cif.'
_cod_database_code               1549312
_shelx_shelxl_version_number     2017/1
_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   0.831
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) =
Uanis(C16A) = Uanis(C17A) = Uanis(C18A) = Uanis(C19A) = Uanis(C20A) =
Uanis(C11B) = Uanis(C12B) = Uanis(C13B) = Uanis(C14B) = Uanis(C15B) =
Uanis(C16B) = Uanis(C17B) = Uanis(C18B) = Uanis(C19B) = Uanis(C20B)
Uanis(C31A) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A) = Uanis(C31B) =
Uanis(C32B) = Uanis(C33B) = Uanis(C34B)
3. Same fragment restrains
{C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A} sigma for 1-2:
0.02, 1-3: 0.04
{C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B} sigma for 1-2:
0.02, 1-3: 0.04
as
{C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A}
{O3A, C31A, C32A, C33A, C34A} sigma for 1-2: 0.02, 1-3: 0.04
{O3B, C31B, C32B, C33B, C34B} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3A, C31A, C32A, C33A, C34A}
4. Others
 Sof(O3B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(C11B)=Sof(C12B)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=
 Sof(C16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20B)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=0.5*(1-FVAR(2))
 Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14A)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20A)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=0.5*FVAR(2)
 Sof(O3A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=FVAR(1)
 Fixed Sof: O2A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C31B(H31C,
 H31D), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D)
5.b Me refined with riding coordinates and stretchable bonds:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13A(H13A,H13B,H13C),
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C17A(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 0.500000 -0.18712(2) -0.250000 0.02686(13) Uani 1 2 d S T P A .
K1 K 0.500000 -0.39979(4) -0.250000 0.03662(17) Uani 1 2 d S T P A .
O1 O 0.50826(9) -0.26854(9) -0.15708(10) 0.0310(3) Uani 1 1 d . . . . .
C1 C 0.50722(14) -0.25900(15) -0.07437(15) 0.0363(5) Uani 1 1 d . . . . .
C2 C 0.59897(16) -0.2885(2) 0.01043(19) 0.0606(8) Uani 1 1 d . . . . .
C3 C 0.6657(2) -0.2196(3) 0.0279(3) 0.0920(15) Uani 1 1 d . . . . .
H3A H 0.6492(5) -0.1679(15) 0.0427(5) 0.138 Uiso 1 1 calc GR . . . .
H3B H 0.7212(17) -0.2359(6) 0.0792(15) 0.138 Uiso 1 1 calc GR . . . .
H3C H 0.6678(2) -0.2126(4) -0.0273(16) 0.138 Uiso 1 1 calc GR . . . .
C4 C 0.6039(2) -0.3013(3) 0.1044(2) 0.0922(16) Uani 1 1 d . . . . .
H4A H 0.5846(6) -0.2510(15) 0.1198(5) 0.138 Uiso 1 1 calc GR . . . .
H4B H 0.5675(11) -0.3476(14) 0.0984(3) 0.138 Uiso 1 1 calc GR . . . .
H4C H 0.6626(18) -0.3131(5) 0.1536(15) 0.138 Uiso 1 1 calc GR . . . .
C5 C 0.62988(18) -0.3692(3) -0.0128(2) 0.0704(10) Uani 1 1 d . . . . .
H5A H 0.62720(19) -0.3622(3) -0.0703(14) 0.106 Uiso 1 1 calc GR . . A .
H5B H 0.6874(13) -0.3806(4) 0.0359(11) 0.106 Uiso 1 1 calc GR . . . .
H5C H 0.5941(8) -0.4145(11) -0.0182(3) 0.106 Uiso 1 1 calc GR . . . .
C6 C 0.42514(14) -0.30671(14) -0.08802(16) 0.0349(5) Uani 1 1 d . . . . .
C7 C 0.39856(17) -0.27816(19) -0.0191(2) 0.0492(6) Uani 1 1 d . . . . .
H7A H 0.3927(2) -0.2166(12) -0.0216(2) 0.074 Uiso 1 1 calc GR . . . .
H7B H 0.3430(11) -0.3042(5) -0.0370(4) 0.074 Uiso 1 1 calc GR . . . .
H7C H 0.4430(9) -0.2955(4) 0.0454(13) 0.074 Uiso 1 1 calc GR . . . .
C8 C 0.43324(17) -0.40272(16) -0.0809(2) 0.0503(6) Uani 1 1 d . . . . .
H8A H 0.4812(9) -0.4183(3) -0.0193(12) 0.075 Uiso 1 1 calc GR . . . .
H8B H 0.3807(10) -0.4266(5) -0.0903(3) 0.075 Uiso 1 1 calc GR . . . .
H8C H 0.4429(3) -0.4237(4) -0.1287(9) 0.075 Uiso 1 1 calc GR . . . .
C9 C 0.34780(14) -0.28753(15) -0.18753(17) 0.0402(5) Uani 1 1 d . . . . .
H9A H 0.3397(2) -0.2270(11) -0.1958(2) 0.060 Uiso 1 1 calc GR . . . .
H9B H 0.3587(2) -0.3103(4) -0.2342(9) 0.060 Uiso 1 1 calc GR . . . .
H9C H 0.2961(9) -0.3132(5) -0.1955(2) 0.060 Uiso 1 1 calc GR . . . .
C10 C 0.4946(2) -0.16500(18) -0.0619(2) 0.0567(7) Uani 1 1 d . . . . .
H10A H 0.4938(2) -0.1577(2) -0.0062(11) 0.085 Uiso 1 1 calc GR . . . .
H10B H 0.5407(9) -0.1335(7) -0.0573(2) 0.085 Uiso 1 1 calc GR . . . .
H10C H 0.4416(11) -0.1461(4) -0.1146(11) 0.085 Uiso 1 1 calc GR . . . .
O2A O 0.5095(14) -0.06938(15) -0.2396(13) 0.030(2) Uani 0.5 1 d . . . . .
C11A C 0.5049(7) 0.0146(11) -0.2262(9) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
C12A C 0.5841(10) 0.0535(9) -0.2294(10) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
C13A C 0.6608(7) -0.0070(7) -0.1831(9) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H13A H 0.681(2) -0.0160(12) -0.113(7) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H13B H 0.6426(19) -0.064(6) -0.218(4) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H13C H 0.711(5) 0.018(3) -0.1866(10) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C14A C 0.6091(10) 0.1394(8) -0.1784(12) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H14A H 0.6277(15) 0.1299(10) -0.094(6) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H14B H 0.674(4) 0.169(2) -0.1775(12) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H14C H 0.546(4) 0.190(3) -0.221(3) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C15A C 0.5612(7) 0.0618(7) -0.3307(8) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H15A H 0.509(5) 0.103(4) -0.368(4) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H15B H 0.614(5) 0.086(2) -0.3312(8) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H15C H 0.5450(18) 0.003(6) -0.363(3) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C16A C 0.4135(10) 0.0524(10) -0.2880(10) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
C17A C 0.3698(7) 0.0232(7) -0.3940(8) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H17A H 0.409(3) 0.0426(17) -0.421(2) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H17B H 0.3635(9) -0.044(5) -0.3977(8) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H17C H 0.307(5) 0.051(2) -0.436(3) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C18A C 0.3523(7) 0.0217(7) -0.2583(10) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H18A H 0.290(5) 0.049(2) -0.303(4) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H18B H 0.3468(8) -0.045(6) -0.2644(10) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H18C H 0.377(2) 0.0395(16) -0.187(6) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C19A C 0.4091(8) 0.1527(7) -0.2845(10) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H19A H 0.446(4) 0.177(2) -0.3024(17) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H19B H 0.351(5) 0.1709(19) -0.327(4) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H19C H 0.4273(19) 0.1700(18) -0.222(6) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C20A C 0.5341(7) 0.0245(8) -0.1205(9) 0.0419(5) Uani 0.234(3) 1 d D . . A -1
H20A H 0.5318(7) 0.093(6) -0.1045(16) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H20B H 0.490(4) -0.013(3) -0.1065(14) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
H20C H 0.602(6) 0.000(2) -0.074(4) 0.063 Uiso 0.234(3) 1 calc GR . . A -1
C11B C 0.4981(7) 0.0159(9) -0.2683(9) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
C12B C 0.4096(7) 0.0437(7) -0.2789(9) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
C13B C 0.3439(6) -0.0277(6) -0.3294(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H13D H 0.3376(8) -0.0391(12) -0.391(5) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H13E H 0.3644(19) -0.079(4) -0.290(3) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H13F H 0.288(5) -0.0108(15) -0.3398(12) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C14B C 0.3687(7) 0.1243(6) -0.3365(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H14D H 0.3654(9) 0.1209(7) -0.380(5) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H14E H 0.327(5) 0.1296(8) -0.3441(12) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H14F H 0.394(3) 0.159(4) -0.312(3) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C15B C 0.4142(6) 0.0560(6) -0.1860(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H15D H 0.441(2) 0.004(4) -0.145(3) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H15E H 0.451(3) 0.107(4) -0.152(3) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H15F H 0.354(5) 0.0647(9) -0.1991(13) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C16B C 0.5825(6) 0.0630(6) -0.1949(7) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
C17B C 0.6134(6) 0.0381(6) -0.0914(7) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H17D H 0.571(3) 0.0500(11) -0.0800(12) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H17E H 0.6254(11) -0.018(4) -0.0832(10) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H17F H 0.662(4) 0.068(2) -0.051(3) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C18B C 0.6574(6) 0.0407(6) -0.2068(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H18D H 0.6406(13) 0.0562(13) -0.277(5) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H18E H 0.714(4) 0.075(3) -0.157(4) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H18F H 0.6706(11) -0.025(5) -0.1950(12) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C19B C 0.5750(7) 0.1625(6) -0.1957(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H19D H 0.524(4) 0.1793(14) -0.1876(11) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H19E H 0.632(4) 0.188(2) -0.140(4) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H19F H 0.5634(11) 0.1859(18) -0.260(5) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
C20B C 0.4893(6) 0.0268(7) -0.3654(8) 0.0419(5) Uani 0.266(3) 1 d D . . A -2
H20D H 0.4825(8) 0.080(4) -0.3806(15) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H20E H 0.536(4) 0.0083(16) -0.3618(8) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
H20F H 0.445(4) -0.001(2) -0.408(4) 0.063 Uiso 0.266(3) 1 calc GR . . A -2
O3A O 0.6151(6) -0.5231(6) -0.2155(6) 0.0499(19) Uani 0.467(7) 1 d D . . A 1
C31A C 0.6977(5) -0.5072(5) -0.1965(7) 0.0636(7) Uani 0.467(7) 1 d D . . A 1
H31A H 0.721478 -0.455570 -0.158331 0.076 Uiso 0.467(7) 1 calc R . . A 1
H31B H 0.696492 -0.499943 -0.255820 0.076 Uiso 0.467(7) 1 calc R . . A 1
C32A C 0.7522(7) -0.5830(6) -0.1423(10) 0.0636(7) Uani 0.467(7) 1 d D . . A 1
H32A H 0.771541 -0.613544 -0.179284 0.076 Uiso 0.467(7) 1 calc R . . A 1
H32B H 0.803380 -0.565694 -0.081465 0.076 Uiso 0.467(7) 1 calc R . . A 1
C33A C 0.6929(6) -0.6365(7) -0.1272(11) 0.0636(7) Uani 0.467(7) 1 d D . . A 1
H33A H 0.693600 -0.695113 -0.146364 0.076 Uiso 0.467(7) 1 calc R . . A 1
H33B H 0.711696 -0.636272 -0.059899 0.076 Uiso 0.467(7) 1 calc R . . A 1
C34A C 0.6122(5) -0.6040(5) -0.1803(7) 0.0636(7) Uani 0.467(7) 1 d D . . A 1
H34A H 0.586196 -0.599124 -0.141743 0.076 Uiso 0.467(7) 1 calc R . . A 1
H34B H 0.575769 -0.642056 -0.233693 0.076 Uiso 0.467(7) 1 calc R . . A 1
O3B O 0.6245(6) -0.5081(6) -0.1821(6) 0.059(2) Uani 0.533(7) 1 d D . . A 2
C31B C 0.6283(4) -0.5815(4) -0.1393(6) 0.0636(7) Uani 0.533(7) 1 d D . . A 2
H31C H 0.573462 -0.612639 -0.176909 0.076 Uiso 0.533(7) 1 calc R . . A 2
H31D H 0.638509 -0.570862 -0.076046 0.076 Uiso 0.533(7) 1 calc R . . A 2
C32B C 0.7065(6) -0.6351(6) -0.1310(9) 0.0636(7) Uani 0.533(7) 1 d D . . A 2
H32C H 0.742473 -0.660872 -0.068021 0.076 Uiso 0.533(7) 1 calc R . . A 2
H32D H 0.685607 -0.679223 -0.179880 0.076 Uiso 0.533(7) 1 calc R . . A 2
C33B C 0.7545(6) -0.5669(5) -0.1471(9) 0.0636(7) Uani 0.533(7) 1 d D . . A 2
H33C H 0.815652 -0.565630 -0.095053 0.076 Uiso 0.533(7) 1 calc R . . A 2
H33D H 0.751752 -0.576421 -0.206983 0.076 Uiso 0.533(7) 1 calc R . . A 2
C34B C 0.7139(4) -0.4924(4) -0.1507(6) 0.0636(7) Uani 0.533(7) 1 d D . . A 2
H34C H 0.716754 -0.452988 -0.194620 0.076 Uiso 0.533(7) 1 calc R . . A 2
H34D H 0.743736 -0.466193 -0.087528 0.076 Uiso 0.533(7) 1 calc R . . A 2
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'
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 K1 48.83(4) 2_654 .
O1 Mn1 K1 48.83(4) . .
O1 Mn1 O1 97.66(8) 2_654 .
O2A Mn1 K1 174.9(4) 2_654 .
O2A Mn1 K1 174.9(4) . .
O2A Mn1 O1 128.2(8) 2_654 2_654
O2A Mn1 O1 133.9(9) . 2_654
O2A Mn1 O1 128.2(8) . .
O2A Mn1 O1 133.9(8) 2_654 .
O2A Mn1 O2A 10.3(9) 2_654 .
Mn1 K1 C5 81.79(7) . 2_654
Mn1 K1 C5 81.79(7) . .
O1 K1 Mn1 35.35(3) . .
O1 K1 Mn1 35.35(3) 2_654 .
O1 K1 O1 70.69(6) 2_654 .
O1 K1 C5 111.78(8) . 2_654
O1 K1 C5 52.85(7) . .
O1 K1 C5 111.78(8) 2_654 .
O1 K1 C5 52.85(7) 2_654 2_654
O1 K1 O3A 120.6(2) 2_654 .
O1 K1 O3A 132.3(2) . .
O1 K1 O3A 132.3(2) 2_654 2_654
O1 K1 O3A 120.6(2) . 2_654
O1 K1 O3B 124.4(2) . 2_654
O1 K1 O3B 121.5(2) . .
O1 K1 O3B 121.5(2) 2_654 2_654
O1 K1 O3B 124.4(2) 2_654 .
C5 K1 C5 163.58(14) . 2_654
O3A K1 Mn1 136.5(2) . .
O3A K1 Mn1 136.5(2) 2_654 .
O3A K1 C5 82.71(19) 2_654 2_654
O3A K1 C5 109.51(18) 2_654 .
O3A K1 C5 82.71(19) . .
O3A K1 C5 109.51(18) . 2_654
O3A K1 O3A 87.0(5) 2_654 .
O3B K1 Mn1 131.8(3) 2_654 .
O3B K1 Mn1 131.8(3) . .
O3B K1 C5 120.85(18) 2_654 .
O3B K1 C5 71.18(19) . .
O3B K1 O3B 96.5(5) 2_654 .
Mn1 O1 K1 95.82(5) . .
C1 O1 Mn1 132.34(13) . .
C1 O1 K1 131.35(13) . .
O1 C1 C2 106.76(18) . .
O1 C1 C6 108.30(17) . .
O1 C1 C10 108.62(18) . .
C6 C1 C2 117.2(2) . .
C10 C1 C2 109.1(2) . .
C10 C1 C6 106.56(18) . .
C3 C2 C1 108.2(3) . .
C4 C2 C1 114.4(2) . .
C4 C2 C3 106.7(3) . .
C5 C2 C1 112.2(2) . .
C5 C2 C3 106.3(3) . .
C5 C2 C4 108.6(3) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4B 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
K1 C5 H5A 37.1 . .
K1 C5 H5B 138.2 . .
K1 C5 H5C 76.2 . .
C2 C5 K1 106.97(16) . .
C2 C5 H5A 109.5 . .
C2 C5 H5B 109.5 . .
C2 C5 H5C 109.5 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 C1 113.7(2) . .
C8 C6 C1 114.85(18) . .
C8 C6 C7 106.97(19) . .
C8 C6 C9 106.1(2) . .
C9 C6 C1 108.45(17) . .
C9 C6 C7 106.17(18) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C1 C10 H10A 109.5 . .
C1 C10 H10B 109.5 . .
C1 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O2A O2A Mn1 84.9(4) 2_654 .
O2A O2A C11A 93(2) 2_654 .
O2A O2A C11B 76.4(19) 2_654 .
C11A O2A Mn1 168(2) . .
C11B O2A Mn1 158.8(13) . .
O2A C11A C12A 103.7(16) . .
O2A C11A C16A 114.2(13) . .
O2A C11A C20A 105.7(13) . .
C16A C11A C12A 120.2(10) . .
C16A C11A C20A 108.5(10) . .
C20A C11A C12A 103.1(10) . .
C13A C12A C11A 110.0(10) . .
C13A C12A C14A 110.7(11) . .
C14A C12A C11A 109.3(10) . .
C15A C12A C11A 110.6(11) . .
C15A C12A C13A 104.7(10) . .
C15A C12A C14A 111.4(11) . .
C12A C13A H13A 109.5 . .
C12A C13A H13B 109.5 . .
C12A C13A H13C 109.5 . .
H13A C13A H13B 109.5 . .
H13A C13A H13C 109.5 . .
H13B C13A H13C 109.5 . .
C12A C14A H14A 109.5 . .
C12A C14A H14B 109.5 . .
C12A C14A H14C 109.5 . .
H14A C14A H14B 109.5 . .
H14A C14A H14C 109.5 . .
H14B C14A H14C 109.5 . .
C12A C15A H15A 109.5 . .
C12A C15A H15B 109.5 . .
C12A C15A H15C 109.5 . .
H15A C15A H15B 109.5 . .
H15A C15A H15C 109.5 . .
H15B C15A H15C 109.5 . .
C11A C16A C17A 111.1(10) . .
C11A C16A C19A 114.9(12) . .
C17A C16A C19A 109.3(10) . .
C18A C16A C11A 112.1(10) . .
C18A C16A C17A 104.5(11) . .
C18A C16A C19A 104.3(10) . .
C16A C17A H17A 109.5 . .
C16A C17A H17B 109.5 . .
C16A C17A H17C 109.5 . .
H17A C17A H17B 109.5 . .
H17A C17A H17C 109.5 . .
H17B C17A H17C 109.5 . .
C16A C18A H18A 109.5 . .
C16A C18A H18B 109.5 . .
C16A C18A H18C 109.5 . .
H18A C18A H18B 109.5 . .
H18A C18A H18C 109.5 . .
H18B C18A H18C 109.5 . .
C16A C19A H19A 109.5 . .
C16A C19A H19B 109.5 . .
C16A C19A H19C 109.5 . .
H19A C19A H19B 109.5 . .
H19A C19A H19C 109.5 . .
H19B C19A H19C 109.5 . .
C11A C20A H20A 109.5 . .
C11A C20A H20B 109.5 . .
C11A C20A H20C 109.5 . .
H20A C20A H20B 109.5 . .
H20A C20A H20C 109.5 . .
H20B C20A H20C 109.5 . .
O2A C11B C12B 105.1(15) . .
O2A C11B C16B 106.7(10) . .
O2A C11B C20B 112.1(14) . .
C16B C11B C12B 118.3(9) . .
C20B C11B C12B 108.5(9) . .
C20B C11B C16B 106.2(8) . .
C13B C12B C11B 107.8(9) . .
C14B C12B C11B 115.3(9) . .
C14B C12B C13B 107.0(9) . .
C15B C12B C11B 114.8(9) . .
C15B C12B C13B 105.0(8) . .
C15B C12B C14B 106.2(9) . .
C12B C13B H13D 109.5 . .
C12B C13B H13E 109.5 . .
C12B C13B H13F 109.5 . .
H13D C13B H13E 109.5 . .
H13D C13B H13F 109.5 . .
H13E C13B H13F 109.5 . .
C12B C14B H14D 109.5 . .
C12B C14B H14E 109.5 . .
C12B C14B H14F 109.5 . .
H14D C14B H14E 109.5 . .
H14D C14B H14F 109.5 . .
H14E C14B H14F 109.5 . .
C12B C15B H15D 109.5 . .
C12B C15B H15E 109.5 . .
C12B C15B H15F 109.5 . .
H15D C15B H15E 109.5 . .
H15D C15B H15F 109.5 . .
H15E C15B H15F 109.5 . .
C11B C16B C19B 115.2(8) . .
C17B C16B C11B 112.0(8) . .
C17B C16B C19B 103.9(8) . .
C18B C16B C11B 111.5(8) . .
C18B C16B C17B 105.4(8) . .
C18B C16B C19B 108.1(7) . .
C16B C17B H17D 109.5 . .
C16B C17B H17E 109.5 . .
C16B C17B H17F 109.5 . .
H17D C17B H17E 109.5 . .
H17D C17B H17F 109.5 . .
H17E C17B H17F 109.5 . .
C16B C18B H18D 109.5 . .
C16B C18B H18E 109.5 . .
C16B C18B H18F 109.5 . .
H18D C18B H18E 109.5 . .
H18D C18B H18F 109.5 . .
H18E C18B H18F 109.5 . .
C16B C19B H19D 109.5 . .
C16B C19B H19E 109.5 . .
C16B C19B H19F 109.5 . .
H19D C19B H19E 109.5 . .
H19D C19B H19F 109.5 . .
H19E C19B H19F 109.5 . .
C11B C20B H20D 109.5 . .
C11B C20B H20E 109.5 . .
C11B C20B H20F 109.5 . .
H20D C20B H20E 109.5 . .
H20D C20B H20F 109.5 . .
H20E C20B H20F 109.5 . .
C31A O3A K1 122.9(6) . .
C31A O3A C34A 110.1(6) . .
C34A O3A K1 123.2(6) . .
O3A C31A H31A 110.5 . .
O3A C31A H31B 110.5 . .
O3A C31A C32A 106.3(7) . .
H31A C31A H31B 108.7 . .
C32A C31A H31A 110.5 . .
C32A C31A H31B 110.5 . .
C31A C32A H32A 110.9 . .
C31A C32A H32B 110.9 . .
H32A C32A H32B 108.9 . .
C33A C32A C31A 104.3(8) . .
C33A C32A H32A 110.9 . .
C33A C32A H32B 110.9 . .
C32A C33A H33A 110.2 . .
C32A C33A H33B 110.2 . .
H33A C33A H33B 108.5 . .
C34A C33A C32A 107.7(8) . .
C34A C33A H33A 110.2 . .
C34A C33A H33B 110.2 . .
O3A C34A H34A 109.6 . .
O3A C34A H34B 109.6 . .
C33A C34A O3A 110.4(7) . .
C33A C34A H34A 109.6 . .
C33A C34A H34B 109.6 . .
H34A C34A H34B 108.1 . .
C31B O3B K1 126.5(6) . .
C31B O3B C34B 103.1(6) . .
C34B O3B K1 127.2(6) . .
O3B C31B H31C 110.3 . .
O3B C31B H31D 110.3 . .
O3B C31B C32B 107.3(6) . .
H31C C31B H31D 108.5 . .
C32B C31B H31C 110.3 . .
C32B C31B H31D 110.3 . .
C31B C32B H32C 111.7 . .
C31B C32B H32D 111.7 . .
H32C C32B H32D 109.5 . .
C33B C32B C31B 100.3(7) . .
C33B C32B H32C 111.7 . .
C33B C32B H32D 111.7 . .
C32B C33B H33C 110.5 . .
C32B C33B H33D 110.5 . .
H33C C33B H33D 108.7 . .
C34B C33B C32B 106.0(8) . .
C34B C33B H33C 110.5 . .
C34B C33B H33D 110.5 . .
O3B C34B H34C 109.6 . .
O3B C34B H34D 109.6 . .
C33B C34B O3B 110.1(6) . .
C33B C34B H34C 109.6 . .
C33B C34B H34D 109.6 . .
H34C C34B H34D 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 K1 3.3891(7) .
Mn1 O1 1.9708(14) 2_654
Mn1 O1 1.9709(14) .
Mn1 O2A 1.884(3) .
Mn1 O2A 1.884(3) 2_654
K1 O1 2.5643(15) .
K1 O1 2.5643(15) 2_654
K1 C5 3.416(3) 2_654
K1 C5 3.416(3) .
K1 O3A 2.711(8) 2_654
K1 O3A 2.711(8) .
K1 O3B 2.592(8) 2_654
K1 O3B 2.592(8) .
O1 C1 1.406(2) .
C1 C2 1.590(4) .
C1 C6 1.590(3) .
C1 C10 1.547(4) .
C2 C3 1.551(5) .
C2 C4 1.543(4) .
C2 C5 1.536(5) .
C3 H3A 0.95(3) .
C3 H3B 0.95(3) .
C3 H3C 0.95(3) .
C4 H4A 0.96(3) .
C4 H4B 0.96(3) .
C4 H4C 0.96(3) .
C5 H5A 0.95(2) .
C5 H5B 0.95(2) .
C5 H5C 0.95(2) .
C6 C7 1.542(3) .
C6 C8 1.536(3) .
C6 C9 1.541(3) .
C7 H7A 0.986(19) .
C7 H7B 0.986(19) .
C7 H7C 0.986(19) .
C8 H8A 0.967(18) .
C8 H8B 0.967(18) .
C8 H8C 0.967(18) .
C9 H9A 0.974(17) .
C9 H9B 0.974(17) .
C9 H9C 0.974(17) .
C10 H10A 0.950(19) .
C10 H10B 0.950(19) .
C10 H10C 0.950(19) .
O2A O2A 0.34(3) 2_654
O2A C11A 1.367(18) .
O2A C11B 1.419(16) .
C11A C12A 1.605(14) .
C11A C16A 1.548(15) .
C11A C20A 1.564(12) .
C12A C13A 1.532(14) .
C12A C14A 1.549(14) .
C12A C15A 1.524(13) .
C13A H13A 1.04(10) .
C13A H13B 1.04(10) .
C13A H13C 1.04(10) .
C14A H14A 1.27(8) .
C14A H14B 1.27(8) .
C14A H14C 1.27(9) .
C15A H15A 1.05(10) .
C15A H15B 1.05(10) .
C15A H15C 1.05(10) .
C16A C17A 1.582(15) .
C16A C18A 1.531(13) .
C16A C19A 1.602(15) .
C17A H17A 1.08(9) .
C17A H17B 1.08(9) .
C17A H17C 1.08(9) .
C18A H18A 1.07(9) .
C18A H18B 1.07(9) .
C18A H18C 1.07(9) .
C19A H19A 0.95(9) .
C19A H19B 0.95(9) .
C19A H19C 0.95(9) .
C20A H20A 1.13(9) .
C20A H20B 1.13(9) .
C20A H20C 1.13(9) .
C11B C12B 1.598(12) .
C11B C16B 1.565(13) .
C11B C20B 1.559(11) .
C12B C13B 1.542(13) .
C12B C14B 1.541(12) .
C12B C15B 1.526(13) .
C13B H13D 0.99(8) .
C13B H13E 0.99(8) .
C13B H13F 0.99(8) .
C14B H14D 0.70(8) .
C14B H14E 0.70(8) .
C14B H14F 0.70(8) .
C15B H15D 1.02(8) .
C15B H15E 1.02(8) .
C15B H15F 1.02(8) .
C16B C17B 1.564(12) .
C16B C18B 1.530(11) .
C16B C19B 1.592(12) .
C17B H17D 0.91(7) .
C17B H17E 0.91(7) .
C17B H17F 0.91(7) .
C18B H18D 1.07(8) .
C18B H18E 1.07(8) .
C18B H18F 1.07(8) .
C19B H19D 1.05(7) .
C19B H19E 1.05(7) .
C19B H19F 1.05(7) .
C20B H20D 0.87(7) .
C20B H20E 0.87(7) .
C20B H20F 0.87(7) .
O3A C31A 1.396(12) .
O3A C34A 1.429(12) .
C31A H31A 0.9900 .
C31A H31B 0.9900 .
C31A C32A 1.522(10) .
C32A H32A 0.9900 .
C32A H32B 0.9900 .
C32A C33A 1.506(8) .
C33A H33A 0.9900 .
C33A H33B 0.9900 .
C33A C34A 1.359(11) .
C34A H34A 0.9900 .
C34A H34B 0.9900 .
O3B C31B 1.354(11) .
O3B C34B 1.452(12) .
C31B H31C 0.9900 .
C31B H31D 0.9900 .
C31B C32B 1.609(10) .
C32B H32C 0.9900 .
C32B H32D 0.9900 .
C32B C33B 1.509(7) .
C33B H33C 0.9900 .
C33B H33D 0.9900 .
C33B C34B 1.386(10) .
C34B H34C 0.9900 .
C34B H34D 0.9900 .
