#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:45:00 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228925 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/12/7231279.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_7231279
loop_
_publ_author_name
'Delmas, Luke C.'
'White, Andrew J. P.'
'Pugh, David'
'Horton, Peter N.'
'Coles, Simon J.'
'Lickiss, Paul D.'
'Davies, Robert P.'
_publ_section_title
;
 Trisiloxane-centred metal--organic frameworks and hydrogen bonded
 assemblies
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              4541
_journal_paper_doi               10.1039/C8CE00662H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'0.25(C233.65 H254.52 Mn12 N19.22 O75.22 Si12), 5.2(C3 H7 N O)'
_chemical_formula_sum            'C74 H100 Mn3 N10 O24 Si3'
_chemical_formula_weight         1762.72
_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     dual
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.04 svn.r3437 for OlexSys, GUI svn.r5361)
;
_audit_update_record
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.476(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9725(6)
_cell_length_b                   19.7061(5)
_cell_length_c                   25.3721(5)
_cell_measurement_reflns_used    16467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3360
_cell_measurement_theta_min      2.1480
_cell_volume                     9382.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00  73.00   1.00   65.00    --  -16.70  57.00-120.00  125
  2  ω   -106.00  22.00   1.00   65.00    --  -16.70 -72.00  60.00  128
  3  ω    -50.00  73.00   1.00   65.00    --  -16.70  38.00-180.00  123
  4  ω    -52.00  73.00   1.00   65.00    --  -16.70  57.00 150.00  125
  5  ω    -50.00  10.00   1.00   65.00    --  -16.70  38.00  30.00   60
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139260000
_diffrn_orient_matrix_UB_12      -0.0326255000
_diffrn_orient_matrix_UB_13      0.0043165000
_diffrn_orient_matrix_UB_21      -0.0305417000
_diffrn_orient_matrix_UB_22      0.0151980000
_diffrn_orient_matrix_UB_23      0.0081234000
_diffrn_orient_matrix_UB_31      -0.0174661000
_diffrn_orient_matrix_UB_32      -0.0007052000
_diffrn_orient_matrix_UB_33      -0.0266920000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            59568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
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    1.248
_exptl_crystal_description       cone
_exptl_crystal_F_000             3692
_exptl_crystal_recrystallization_method
'The material was crystallised from DMF and acetic acid'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10752
_refine_ls_number_restraints     1938
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0833
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             10752
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00662h2.cif
_cod_data_source_block           IMP20
_cod_depositor_comments
'Adding full bibliography for 7231278--7231280.cif.'
_cod_database_code               7231279
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C44H30 O14 Si3 Mn3 (C3H7NO)8'
_chemical_oxdiff_usercomment     LD_TS_Mn_AcOH(cone)
_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.
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O41, N41, C41, C42, C43}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O231, N231, C231, C232, C233}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O241, N241, C241, C242, C243}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O91, N91, C91, C92, C93}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O261, N261, C261, C262, C263}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O51, N51, C51, C52, C53}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O251, N251, C251, C252, C253}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O61, N61, C61, C62, C63}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O71, N71, C71, C72, C73}
{O31, N31, C31, C32, C33} sigma for 1-2: 0.01, 1-3: 0.04
as
{O81, N81, C81, C82, C83}
6. Others
 1*[Sof(O71)+Sof(N71)+Sof(C71)+Sof(H71)+Sof(C72)+Sof(H72A)+Sof(H72B)+Sof(H72C)+
 Sof(C73)+Sof(H73A)+Sof(H73B)+Sof(H73C)]+1*[Sof(O81)+Sof(N81)+Sof(C81)+Sof(H81)+
 Sof(C82)+Sof(H82A)+Sof(H82B)+Sof(H82C)+Sof(C83)+Sof(H83A)+Sof(H83B)+Sof(H83C)]+
 1*[Sof(O91)+Sof(N91)+Sof(C91)+Sof(H23D)+Sof(C92)+Sof(H92A)+Sof(H92B)+Sof(H92C)+
 Sof(C93)+Sof(H93A)+Sof(H93B)+Sof(H93C)]=1 with esd of 0.000001
 Sof(O241)=Sof(N241)=Sof(C241)=Sof(H241)=Sof(C242)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C243)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(O41)=Sof(N41)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(O51)=Sof(N51)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=1-FVAR(2)
 Sof(O251)=Sof(N251)=Sof(C251)=Sof(H251)=Sof(C252)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C253)=Sof(H25D)=Sof(H25E)=Sof(H25F)=FVAR(2)
 Sof(O261)=Sof(N261)=Sof(C261)=Sof(H261)=Sof(C262)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C263)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(3)
 Sof(O61)=Sof(N61)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(3)
 Sof(O231)=Sof(N231)=Sof(C231)=Sof(H231)=Sof(C232)=Sof(H23A)=Sof(H23B)=
 Sof(H23C)=Sof(C233)=Sof(H23E)=Sof(H23F)=Sof(H23G)=1-FVAR(4)
 Sof(O31)=Sof(N31)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(4)
 Sof(O71)=Sof(N71)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(5)
 Sof(O81)=Sof(N81)=Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(6)
 Sof(O91)=Sof(N91)=Sof(C91)=Sof(H23D)=Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(H92C)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(7)
7.a Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C232(H23A,H23B,H23C), C233(H23E,H23F,H23G), C242(H24A,H24B,H24C),
 C243(H24D,H24E,H24F), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C262(H26A,H26B,
 H26C), C263(H26D,H26E,H26F), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C252(H25A,H25B,H25C), C253(H25D,H25E,H25F), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C82(H82A,H82B,H82C), C83(H83A,
 H83B,H83C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21), C31(H31), C41(H41), C231(H231),
 C241(H241), C91(H23D), C261(H261), C51(H51), C251(H251), C61(H61), C71(H71),
 C81(H81)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id LD_TS_Mn_AcOH
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.249
_oxdiff_exptl_absorpt_empirical_full_min 0.569
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 0.12888(3) 0.60949(3) 0.02256(2) 0.0521(2) Uani 1 1 d . U . . .
Mn2 Mn 0.2500 0.2500 0.5000 0.0390(2) Uani 1 2 d S TU P . .
Si1 Si 0.5000 0.46796(9) 0.2500 0.0762(5) Uani 1 2 d S TU P . .
Si2 Si 0.42805(6) 0.56739(5) 0.31764(4) 0.0544(3) Uani 1 1 d . U . . .
O1 O 0.48716(16) 0.51580(14) 0.29978(10) 0.0643(7) Uani 1 1 d . U . . .
O2 O 0.20830(18) 0.61991(16) 0.08643(11) 0.0768(9) Uani 1 1 d . U . . .
O3 O 0.26942(13) 0.71633(12) 0.08379(8) 0.0485(5) Uani 1 1 d . U . . .
O4 O 0.27571(14) 0.34807(12) 0.47480(10) 0.0563(6) Uani 1 1 d . U . . .
O5 O 0.19381(15) 0.43045(13) 0.46894(11) 0.0639(7) Uani 1 1 d . U . . .
O6 O 0.63567(12) 0.77809(12) 0.49421(8) 0.0479(5) Uani 1 1 d . U . . .
O7 O 0.55237(15) 0.84907(13) 0.45827(11) 0.0628(7) Uani 1 1 d . U . . .
C1 C 0.4185(4) 0.4168(3) 0.2267(3) 0.114(2) Uani 1 1 d . U . . .
H1A H 0.4071 0.3883 0.2560 0.171 Uiso 1 1 calc GR . . . .
H1B H 0.4270 0.3880 0.1968 0.171 Uiso 1 1 calc GR . . . .
H1C H 0.3784 0.4473 0.2151 0.171 Uiso 1 1 calc GR . . . .
C2 C 0.3716(2) 0.60338(18) 0.25741(13) 0.0548(8) Uani 1 1 d . U . . .
C3 C 0.3930(2) 0.65870(18) 0.22941(13) 0.0512(8) Uani 1 1 d . U . . .
H3 H 0.4348 0.6830 0.2436 0.061 Uiso 1 1 calc R . . . .
C4 C 0.35463(19) 0.67898(17) 0.18115(12) 0.0491(7) Uani 1 1 d . U . . .
H4 H 0.3700 0.7172 0.1631 0.059 Uiso 1 1 calc R . . . .
C5 C 0.2939(2) 0.64369(19) 0.15910(13) 0.0536(8) Uani 1 1 d . U . . .
C6 C 0.2720(3) 0.5895(3) 0.18656(17) 0.0780(13) Uani 1 1 d . U . . .
H6 H 0.2311 0.5644 0.1717 0.094 Uiso 1 1 calc R . . . .
C7 C 0.3089(2) 0.5710(2) 0.23562(15) 0.0755(14) Uani 1 1 d . U . . .
H7 H 0.2909 0.5352 0.2549 0.091 Uiso 1 1 calc R . . . .
C8 C 0.2544(2) 0.66186(19) 0.10492(13) 0.0524(8) Uani 1 1 d . U . . .
C9 C 0.3719(2) 0.51809(18) 0.35918(14) 0.0550(8) Uani 1 1 d . U . . .
C10 C 0.3952(2) 0.45438(19) 0.37937(14) 0.0571(8) Uani 1 1 d . U . . .
H10 H 0.4383 0.4358 0.3708 0.068 Uiso 1 1 calc R . . . .
C11 C 0.3558(2) 0.41869(19) 0.41150(15) 0.0576(8) Uani 1 1 d . U . . .
H11 H 0.3720 0.3754 0.4247 0.069 Uiso 1 1 calc R . . . .
C12 C 0.2934(2) 0.44449(17) 0.42484(14) 0.0521(8) Uani 1 1 d . U . . .
C13 C 0.2708(2) 0.50802(19) 0.40546(16) 0.0610(9) Uani 1 1 d . U . . .
H13 H 0.2284 0.5271 0.4149 0.073 Uiso 1 1 calc R . . . .
C14 C 0.3096(2) 0.5437(2) 0.37252(16) 0.0618(9) Uani 1 1 d . U . . .
H14 H 0.2928 0.5866 0.3589 0.074 Uiso 1 1 calc R . . . .
C15 C 0.2508(2) 0.40458(17) 0.45922(14) 0.0529(8) Uani 1 1 d . U . . .
C16 C 0.4741(2) 0.63573(19) 0.36037(13) 0.0530(8) Uani 1 1 d . U . . .
C17 C 0.5334(2) 0.61973(19) 0.39809(14) 0.0565(9) Uani 1 1 d . U . . .
H17 H 0.5505 0.5744 0.4007 0.068 Uiso 1 1 calc R . . . .
C18 C 0.5677(2) 0.66927(18) 0.43199(14) 0.0518(8) Uani 1 1 d . U . . .
H18 H 0.6070 0.6575 0.4580 0.062 Uiso 1 1 calc R . . . .
C19 C 0.54366(19) 0.73570(18) 0.42719(13) 0.0508(8) Uani 1 1 d . U . . .
C20 C 0.4846(2) 0.75235(19) 0.38960(15) 0.0586(9) Uani 1 1 d . U . . .
H20 H 0.4678 0.7978 0.3865 0.070 Uiso 1 1 calc R . . . .
C21 C 0.4511(2) 0.7023(2) 0.35715(14) 0.0589(9) Uani 1 1 d . U . . .
H21 H 0.4110 0.7140 0.3318 0.071 Uiso 1 1 calc R . . . .
C22 C 0.57915(19) 0.79067(18) 0.46132(13) 0.0505(7) Uani 1 1 d . U . . .
O31 O 0.0534(5) 0.6510(3) 0.0757(3) 0.0846(19) Uani 0.627(10) 1 d D U . A 1
N31 N 0.0477(10) 0.7309(8) 0.1427(7) 0.183(6) Uani 0.627(10) 1 d D U . A 1
C31 C 0.0768(6) 0.6998(5) 0.1058(4) 0.111(3) Uani 0.627(10) 1 d D U . A 1
H31 H 0.1224 0.7162 0.1009 0.133 Uiso 0.627(10) 1 calc R . . A 1
C32 C -0.0082(12) 0.6874(11) 0.1637(9) 0.217(8) Uani 0.627(10) 1 d D U . A 1
H32A H -0.0286 0.7126 0.1912 0.326 Uiso 0.627(10) 1 calc R . . A 1
H32B H -0.0460 0.6761 0.1344 0.326 Uiso 0.627(10) 1 calc R . . A 1
H32C H 0.0140 0.6456 0.1791 0.326 Uiso 0.627(10) 1 calc R . . A 1
C33 C 0.0877(11) 0.7800(8) 0.1788(6) 0.196(7) Uani 0.627(10) 1 d D U . A 1
H33A H 0.0570 0.7977 0.2034 0.294 Uiso 0.627(10) 1 calc R . . A 1
H33B H 0.1292 0.7576 0.1990 0.294 Uiso 0.627(10) 1 calc R . . A 1
H33C H 0.1036 0.8174 0.1580 0.294 Uiso 0.627(10) 1 calc R . . A 1
O41 O 0.0802(5) 0.5166(4) 0.0342(5) 0.068(2) Uani 0.545(6) 1 d D U . A 1
N41 N 0.1365(5) 0.4128(4) 0.0437(5) 0.114(3) Uani 0.545(6) 1 d D U . A 1
C41 C 0.0844(5) 0.4535(4) 0.0264(4) 0.087(2) Uani 0.545(6) 1 d D U . A 1
H41 H 0.0444 0.4332 0.0052 0.104 Uiso 0.545(6) 1 calc R . . A 1
C42 C 0.2059(8) 0.4399(8) 0.0735(9) 0.170(7) Uani 0.545(6) 1 d D U . A 1
H42A H 0.2388 0.4021 0.0834 0.256 Uiso 0.545(6) 1 calc R . . A 1
H42B H 0.2273 0.4716 0.0506 0.256 Uiso 0.545(6) 1 calc R . . A 1
H42C H 0.1966 0.4635 0.1058 0.256 Uiso 0.545(6) 1 calc R . . A 1
C43 C 0.1318(7) 0.3430(6) 0.0244(8) 0.148(6) Uani 0.545(6) 1 d D U . A 1
H43A H 0.1741 0.3177 0.0403 0.222 Uiso 0.545(6) 1 calc R . . A 1
H43B H 0.0891 0.3215 0.0343 0.222 Uiso 0.545(6) 1 calc R . . A 1
H43C H 0.1290 0.3428 -0.0145 0.222 Uiso 0.545(6) 1 calc R . . A 1
O231 O 0.0576(12) 0.6227(10) 0.0774(7) 0.129(5) Uani 0.373(10) 1 d D U . A 2
N231 N 0.0587(16) 0.7086(12) 0.1485(11) 0.170(7) Uani 0.373(10) 1 d D U . A 2
C231 C 0.0479(16) 0.6540(12) 0.1195(10) 0.174(7) Uani 0.373(10) 1 d D U . A 2
H231 H 0.0205 0.6245 0.1381 0.208 Uiso 0.373(10) 1 calc R . . A 2
C232 C 0.1200(14) 0.7534(11) 0.1378(11) 0.165(8) Uani 0.373(10) 1 d D U . A 2
H23A H 0.1234 0.7928 0.1617 0.247 Uiso 0.373(10) 1 calc R . . A 2
H23B H 0.1645 0.7275 0.1442 0.247 Uiso 0.373(10) 1 calc R . . A 2
H23C H 0.1116 0.7689 0.1007 0.247 Uiso 0.373(10) 1 calc R . . A 2
C233 C 0.0180(19) 0.7315(15) 0.1900(12) 0.192(11) Uani 0.373(10) 1 d D U . A 2
H23E H 0.0381 0.7742 0.2052 0.289 Uiso 0.373(10) 1 calc R . . A 2
H23F H -0.0319 0.7385 0.1744 0.289 Uiso 0.373(10) 1 calc R . . A 2
H23G H 0.0207 0.6970 0.2181 0.289 Uiso 0.373(10) 1 calc R . . A 2
O241 O 0.1001(8) 0.5056(7) 0.0349(7) 0.105(4) Uani 0.455(6) 1 d D U . A 2
N241 N 0.0347(7) 0.4882(10) 0.1100(5) 0.167(6) Uani 0.455(6) 1 d D U . A 2
C241 C 0.0494(8) 0.4919(8) 0.0613(5) 0.125(4) Uani 0.455(6) 1 d D U . A 2
H241 H 0.0080 0.4804 0.0371 0.150 Uiso 0.455(6) 1 calc R . . A 2
C242 C 0.0927(11) 0.5061(16) 0.1554(7) 0.199(10) Uani 0.455(6) 1 d D U . A 2
H24A H 0.0745 0.5011 0.1893 0.299 Uiso 0.455(6) 1 calc R . . A 2
H24B H 0.1335 0.4756 0.1548 0.299 Uiso 0.455(6) 1 calc R . . A 2
H24C H 0.1079 0.5531 0.1514 0.299 Uiso 0.455(6) 1 calc R . . A 2
C243 C -0.0414(7) 0.5011(12) 0.1123(7) 0.150(6) Uani 0.455(6) 1 d D U . A 2
H24D H -0.0503 0.4979 0.1493 0.225 Uiso 0.455(6) 1 calc R . . A 2
H24E H -0.0540 0.5467 0.0986 0.225 Uiso 0.455(6) 1 calc R . . A 2
H24F H -0.0705 0.4674 0.0906 0.225 Uiso 0.455(6) 1 calc R . . A 2
O91 O 0.1159(18) 0.693(2) 0.2330(16) 0.331(14) Uani 0.402(3) 1 d D U . B 2
N91 N 0.2099(17) 0.7689(17) 0.2546(16) 0.324(13) Uani 0.402(3) 1 d D U . B 2
C91 C 0.1590(18) 0.7391(19) 0.2227(14) 0.300(13) Uani 0.402(3) 1 d D U . B 2
H23D H 0.1534 0.7537 0.1866 0.360 Uiso 0.402(3) 1 calc R . . B 2
C92 C 0.240(2) 0.722(2) 0.2993(16) 0.284(14) Uani 0.402(3) 1 d D U . B 2
H92A H 0.2784 0.7452 0.3228 0.426 Uiso 0.402(3) 1 calc R . . B 2
H92B H 0.2026 0.7086 0.3198 0.426 Uiso 0.402(3) 1 calc R . . B 2
H92C H 0.2597 0.6813 0.2844 0.426 Uiso 0.402(3) 1 calc R . . B 2
C93 C 0.2573(19) 0.816(2) 0.232(2) 0.330(17) Uani 0.402(3) 1 d D U . B 2
H93A H 0.2925 0.8339 0.2605 0.495 Uiso 0.402(3) 1 calc R . . B 2
H93B H 0.2818 0.7913 0.2062 0.495 Uiso 0.402(3) 1 calc R . . B 2
H93C H 0.2293 0.8529 0.2139 0.495 Uiso 0.402(3) 1 calc R . . B 2
O261 O 0.0391(8) 0.3328(8) 0.2494(10) 0.209(8) Uani 0.454(13) 1 d D U . C 2
N261 N 0.1547(12) 0.3761(12) 0.2873(7) 0.153(7) Uani 0.454(13) 1 d D U . C 2
C261 C 0.1029(11) 0.3526(18) 0.2535(9) 0.161(7) Uani 0.454(13) 1 d D U . C 2
H261 H 0.1184 0.3488 0.2197 0.193 Uiso 0.454(13) 1 calc R . . C 2
C262 C 0.1513(12) 0.3675(8) 0.3459(6) 0.143(8) Uani 0.454(13) 1 d D U . C 2
H26A H 0.1938 0.3876 0.3667 0.215 Uiso 0.454(13) 1 calc R . . C 2
H26B H 0.1086 0.3902 0.3548 0.215 Uiso 0.454(13) 1 calc R . . C 2
H26C H 0.1492 0.3191 0.3543 0.215 Uiso 0.454(13) 1 calc R . . C 2
C263 C 0.1977(18) 0.4332(16) 0.2741(10) 0.206(12) Uani 0.454(13) 1 d D U . C 2
H26D H 0.2341 0.4437 0.3045 0.309 Uiso 0.454(13) 1 calc R . . C 2
H26E H 0.2208 0.4215 0.2432 0.309 Uiso 0.454(13) 1 calc R . . C 2
H26F H 0.1670 0.4729 0.2655 0.309 Uiso 0.454(13) 1 calc R . . C 2
O51 O 0.4552(13) 0.3564(11) 0.1075(8) 0.190(8) Uani 0.412(10) 1 d D U . D 1
N51 N 0.3970(13) 0.3725(9) 0.0244(7) 0.185(7) Uani 0.412(10) 1 d D U . D 1
C51 C 0.4327(19) 0.3345(11) 0.0608(8) 0.228(9) Uani 0.412(10) 1 d D U . D 1
H51 H 0.4423 0.2888 0.0524 0.274 Uiso 0.412(10) 1 calc R . . D 1
C52 C 0.4304(12) 0.4402(9) 0.0137(7) 0.116(5) Uani 0.412(10) 1 d D U . D 1
H52A H 0.3992 0.4645 -0.0143 0.174 Uiso 0.412(10) 1 calc R . . D 1
H52B H 0.4367 0.4675 0.0464 0.174 Uiso 0.412(10) 1 calc R . . D 1
H52C H 0.4768 0.4325 0.0022 0.174 Uiso 0.412(10) 1 calc R . . D 1
C53 C 0.3450(14) 0.3369(10) -0.0141(8) 0.167(8) Uani 0.412(10) 1 d D U . D 1
H53A H 0.3210 0.3695 -0.0399 0.250 Uiso 0.412(10) 1 calc R . . D 1
H53B H 0.3695 0.3028 -0.0329 0.250 Uiso 0.412(10) 1 calc R . . D 1
H53C H 0.3098 0.3146 0.0046 0.250 Uiso 0.412(10) 1 calc R . . D 1
O251 O 0.4105(16) 0.3362(11) 0.1101(9) 0.286(11) Uani 0.588(10) 1 d D U . D 2
N251 N 0.3629(12) 0.4317(9) 0.0611(8) 0.242(7) Uani 0.588(10) 1 d D U . D 2
C251 C 0.3685(16) 0.3854(12) 0.0976(9) 0.269(9) Uani 0.588(10) 1 d D U . D 2
H251 H 0.3330 0.3893 0.1203 0.322 Uiso 0.588(10) 1 calc R . . D 2
C252 C 0.4065(18) 0.4211(15) 0.0169(12) 0.257(11) Uani 0.588(10) 1 d D U . D 2
H25A H 0.3984 0.4589 -0.0084 0.386 Uiso 0.588(10) 1 calc R . . D 2
H25B H 0.4572 0.4191 0.0318 0.386 Uiso 0.588(10) 1 calc R . . D 2
H25C H 0.3924 0.3785 -0.0015 0.386 Uiso 0.588(10) 1 calc R . . D 2
C253 C 0.3017(17) 0.4767(15) 0.0577(11) 0.304(15) Uani 0.588(10) 1 d D U . D 2
H25D H 0.3033 0.5093 0.0288 0.456 Uiso 0.588(10) 1 calc R . . D 2
H25E H 0.2578 0.4499 0.0505 0.456 Uiso 0.588(10) 1 calc R . . D 2
H25F H 0.3027 0.5010 0.0915 0.456 Uiso 0.588(10) 1 calc R . . D 2
O61 O 0.1396(9) 0.3449(8) 0.1942(5) 0.223(7) Uani 0.546(13) 1 d D U . C 1
N61 N 0.1574(7) 0.3609(6) 0.2845(5) 0.115(4) Uani 0.546(13) 1 d D U . C 1
C61 C 0.1202(10) 0.3411(12) 0.2401(5) 0.156(6) Uani 0.546(13) 1 d D U . C 1
H61 H 0.0746 0.3220 0.2420 0.187 Uiso 0.546(13) 1 calc R . . C 1
C62 C 0.2332(9) 0.3819(13) 0.2806(8) 0.185(8) Uani 0.546(13) 1 d D U . C 1
H62A H 0.2569 0.3960 0.3158 0.277 Uiso 0.546(13) 1 calc R . . C 1
H62B H 0.2588 0.3434 0.2680 0.277 Uiso 0.546(13) 1 calc R . . C 1
H62C H 0.2328 0.4197 0.2556 0.277 Uiso 0.546(13) 1 calc R . . C 1
C63 C 0.1373(11) 0.3634(5) 0.3377(5) 0.123(5) Uani 0.546(13) 1 d D U . C 1
H63A H 0.1773 0.3809 0.3629 0.184 Uiso 0.546(13) 1 calc R . . C 1
H63B H 0.0960 0.3933 0.3375 0.184 Uiso 0.546(13) 1 calc R . . C 1
H63C H 0.1251 0.3177 0.3485 0.184 Uiso 0.546(13) 1 calc R . . C 1
O71 O 0.0237(16) 0.4574(10) 0.3649(8) 0.112(8) Uani 0.187(3) 1 d D U . E -1
N71 N 0.0269(18) 0.5317(17) 0.2918(9) 0.150(10) Uani 0.187(3) 1 d D U . E -1
C71 C 0.010(2) 0.5103(11) 0.3365(9) 0.114(9) Uani 0.187(3) 1 d D U . E -1
H71 H -0.0207 0.5411 0.3514 0.137 Uiso 0.187(3) 1 calc R . . E -1
C72 C 0.1054(18) 0.545(2) 0.2917(13) 0.154(12) Uani 0.187(3) 1 d D U . E -1
H72A H 0.1130 0.5606 0.2564 0.230 Uiso 0.187(3) 1 calc R . . E -1
H72B H 0.1220 0.5793 0.3184 0.230 Uiso 0.187(3) 1 calc R . . E -1
H72C H 0.1321 0.5026 0.3003 0.230 Uiso 0.187(3) 1 calc R . . E -1
C73 C -0.027(2) 0.556(3) 0.2490(17) 0.21(2) Uani 0.187(3) 1 d D U . E -1
H73A H -0.0044 0.5698 0.2185 0.317 Uiso 0.187(3) 1 calc R . . E -1
H73B H -0.0612 0.5191 0.2380 0.317 Uiso 0.187(3) 1 calc R . . E -1
H73C H -0.0525 0.5945 0.2617 0.317 Uiso 0.187(3) 1 calc R . . E -1
O81 O 0.1332(19) 0.5961(16) 0.2956(14) 0.305(14) Uani 0.411(3) 1 d D U . F 1
N81 N 0.1934(11) 0.6948(13) 0.3223(12) 0.240(10) Uani 0.411(3) 1 d D U . F 1
C81 C 0.1700(16) 0.6483(17) 0.2877(12) 0.258(10) Uani 0.411(3) 1 d D U . F 1
H81 H 0.1815 0.6539 0.2528 0.310 Uiso 0.411(3) 1 calc R . . F 1
C82 C 0.1846(19) 0.6795(14) 0.3795(12) 0.257(12) Uani 0.411(3) 1 d D U . F 1
H82A H 0.2037 0.7172 0.4024 0.386 Uiso 0.411(3) 1 calc R . . F 1
H82B H 0.1339 0.6735 0.3820 0.386 Uiso 0.411(3) 1 calc R . . F 1
H82C H 0.2105 0.6378 0.3911 0.386 Uiso 0.411(3) 1 calc R . . F 1
C83 C 0.2324(18) 0.7535(16) 0.3069(18) 0.266(13) Uani 0.411(3) 1 d D U . F 1
H83A H 0.2456 0.7828 0.3380 0.399 Uiso 0.411(3) 1 calc R . . F 1
H83B H 0.2755 0.7382 0.2934 0.399 Uiso 0.411(3) 1 calc R . . F 1
H83C H 0.2022 0.7789 0.2790 0.399 Uiso 0.411(3) 1 calc R . . F 1
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'
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'
Si Si 0.0817 0.0704 '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
O2 Mn1 O5 96.63(13) . 6_565
O2 Mn1 O6 94.63(10) . 8_465
O2 Mn1 O7 152.18(11) . 8_465
O2 Mn1 O31 87.1(3) . .
O2 Mn1 O41 105.3(4) . .
O2 Mn1 O231 86.2(6) . .
O2 Mn1 O241 98.8(5) . .
O5 Mn1 O6 95.21(10) 6_565 8_465
O5 Mn1 O7 92.57(11) 6_565 8_465
O5 Mn1 O31 176.3(3) 6_565 .
O5 Mn1 O241 85.6(4) 6_565 .
O7 Mn1 O6 58.32(9) 8_465 8_465
O7 Mn1 O31 84.2(3) 8_465 .
O31 Mn1 O6 84.8(2) . 8_465
O41 Mn1 O5 94.4(2) . 6_565
O41 Mn1 O6 156.7(3) . 8_465
O41 Mn1 O7 100.1(4) . 8_465
O41 Mn1 O31 84.3(3) . .
O231 Mn1 O5 165.2(5) . 6_565
O231 Mn1 O6 99.0(6) . 8_465
O231 Mn1 O7 91.5(6) . 8_465
O231 Mn1 O241 79.6(7) . .
O241 Mn1 O6 166.4(5) . 8_465
O241 Mn1 O7 108.1(5) . 8_465
O3 Mn2 O3 180.0 4_545 6_566
O3 Mn2 O6 89.34(8) 4_545 3_445
O3 Mn2 O6 90.66(8) 4_545 5_666
O3 Mn2 O6 89.34(8) 6_566 5_666
O3 Mn2 O6 90.66(8) 6_566 3_445
O4 Mn2 O3 89.81(9) 7_556 6_566
O4 Mn2 O3 90.19(9) . 6_566
O4 Mn2 O3 89.81(9) . 4_545
O4 Mn2 O3 90.19(9) 7_556 4_545
O4 Mn2 O4 180.0 7_556 .
O4 Mn2 O6 91.07(9) 7_556 5_666
O4 Mn2 O6 88.93(10) . 5_666
O4 Mn2 O6 88.93(10) 7_556 3_445
O4 Mn2 O6 91.07(9) . 3_445
O6 Mn2 O6 180.0 5_666 3_445
O1 Si1 O1 109.0(2) . 2_655
O1 Si1 C1 106.2(3) 2_655 .
O1 Si1 C1 110.3(3) . .
O1 Si1 C1 106.2(3) . 2_655
O1 Si1 C1 110.3(3) 2_655 2_655
C1 Si1 C1 114.7(5) . 2_655
O1 Si2 C2 110.17(17) . .
O1 Si2 C9 107.73(16) . .
O1 Si2 C16 109.29(17) . .
C2 Si2 C9 110.54(17) . .
C16 Si2 C2 111.34(16) . .
C16 Si2 C9 107.67(16) . .
Si1 O1 Si2 140.22(18) . .
C8 O2 Mn1 139.2(2) . .
C8 O3 Mn2 130.9(2) . 4
C15 O4 Mn2 144.7(3) . .
C15 O5 Mn1 125.2(2) . 6_566
Mn2 O6 Mn1 108.24(9) 3 8_566
C22 O6 Mn1 86.5(2) . 8_566
C22 O6 Mn2 143.7(2) . 3
C22 O7 Mn1 94.5(2) . 8_566
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 Si2 122.5(3) . .
C7 C2 Si2 120.3(3) . .
C7 C2 C3 116.9(3) . .
C2 C3 H3 119.3 . .
C4 C3 C2 121.3(3) . .
C4 C3 H3 119.3 . .
C3 C4 H4 119.8 . .
C3 C4 C5 120.5(3) . .
C5 C4 H4 119.8 . .
C4 C5 C8 121.3(3) . .
C6 C5 C4 118.7(3) . .
C6 C5 C8 120.0(3) . .
C5 C6 H6 119.6 . .
C5 C6 C7 120.7(4) . .
C7 C6 H6 119.6 . .
C2 C7 H7 119.1 . .
C6 C7 C2 121.8(4) . .
C6 C7 H7 119.1 . .
O2 C8 O3 126.9(3) . .
O2 C8 C5 114.4(3) . .
O3 C8 C5 118.7(3) . .
C10 C9 Si2 119.7(3) . .
C14 C9 Si2 121.9(3) . .
C14 C9 C10 118.3(3) . .
C9 C10 H10 119.8 . .
C11 C10 C9 120.3(4) . .
C11 C10 H10 119.8 . .
C10 C11 H11 119.4 . .
C12 C11 C10 121.2(3) . .
C12 C11 H11 119.4 . .
C11 C12 C13 118.6(4) . .
C11 C12 C15 120.5(3) . .
C13 C12 C15 120.9(4) . .
C12 C13 H13 119.7 . .
C14 C13 C12 120.5(4) . .
C14 C13 H13 119.7 . .
C9 C14 C13 121.0(3) . .
C9 C14 H14 119.5 . .
C13 C14 H14 119.5 . .
O4 C15 O5 126.7(3) . .
O4 C15 C12 116.1(4) . .
O5 C15 C12 117.2(3) . .
C17 C16 Si2 119.7(3) . .
C21 C16 Si2 122.4(3) . .
C21 C16 C17 117.9(3) . .
C16 C17 H17 119.4 . .
C18 C17 C16 121.2(3) . .
C18 C17 H17 119.4 . .
C17 C18 H18 120.4 . .
C19 C18 C17 119.3(3) . .
C19 C18 H18 120.4 . .
C18 C19 C20 120.1(3) . .
C18 C19 C22 121.5(3) . .
C20 C19 C22 118.4(3) . .
C19 C20 H20 120.3 . .
C21 C20 C19 119.4(3) . .
C21 C20 H20 120.3 . .
C16 C21 H21 119.0 . .
C20 C21 C16 122.1(3) . .
C20 C21 H21 119.0 . .
O6 C22 C19 120.2(3) . .
O7 C22 O6 120.6(3) . .
O7 C22 C19 119.2(3) . .
C31 O31 Mn1 116.0(7) . .
C31 N31 C32 112.2(11) . .
C31 N31 C33 121.5(13) . .
C33 N31 C32 118.5(13) . .
O31 C31 N31 129.8(11) . .
O31 C31 H31 115.1 . .
N31 C31 H31 115.1 . .
N31 C32 H32A 109.5 . .
N31 C32 H32B 109.5 . .
N31 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
N31 C33 H33A 109.5 . .
N31 C33 H33B 109.5 . .
N31 C33 H33C 109.5 . .
H33A C33 H33B 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C41 O41 Mn1 143.1(7) . .
C41 N41 C42 121.0(9) . .
C41 N41 C43 117.5(10) . .
C43 N41 C42 120.4(10) . .
O41 C41 N41 128.1(10) . .
O41 C41 H41 116.0 . .
N41 C41 H41 116.0 . .
N41 C42 H42A 109.5 . .
N41 C42 H42B 109.5 . .
N41 C42 H42C 109.5 . .
H42A C42 H42B 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
N41 C43 H43A 109.5 . .
N41 C43 H43B 109.5 . .
N41 C43 H43C 109.5 . .
H43A C43 H43B 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C231 O231 Mn1 143.9(19) . .
C231 N231 C232 116.2(15) . .
C231 N231 C233 127.2(17) . .
C233 N231 C232 116.6(15) . .
O231 C231 N231 148(2) . .
O231 C231 H231 106.1 . .
N231 C231 H231 106.1 . .
N231 C232 H23A 109.5 . .
N231 C232 H23B 109.5 . .
N231 C232 H23C 109.5 . .
H23A C232 H23B 109.5 . .
H23A C232 H23C 109.5 . .
H23B C232 H23C 109.5 . .
N231 C233 H23E 109.5 . .
N231 C233 H23F 109.5 . .
N231 C233 H23G 109.5 . .
H23E C233 H23F 109.5 . .
H23E C233 H23G 109.5 . .
H23F C233 H23G 109.5 . .
C241 O241 Mn1 120.2(12) . .
C241 N241 C242 118.2(12) . .
C241 N241 C243 112.0(13) . .
C243 N241 C242 122.5(13) . .
O241 C241 N241 142.0(16) . .
O241 C241 H241 109.0 . .
N241 C241 H241 109.0 . .
N241 C242 H24A 109.5 . .
N241 C242 H24B 109.5 . .
N241 C242 H24C 109.5 . .
H24A C242 H24B 109.5 . .
H24A C242 H24C 109.5 . .
H24B C242 H24C 109.5 . .
N241 C243 H24D 109.5 . .
N241 C243 H24E 109.5 . .
N241 C243 H24F 109.5 . .
H24D C243 H24E 109.5 . .
H24D C243 H24F 109.5 . .
H24E C243 H24F 109.5 . .
C91 N91 C92 111(2) . .
C91 N91 C93 119(2) . .
C93 N91 C92 119(2) . .
O91 C91 N91 129(3) . .
O91 C91 H23D 115.4 . .
N91 C91 H23D 115.4 . .
N91 C92 H92A 109.5 . .
N91 C92 H92B 109.5 . .
N91 C92 H92C 109.5 . .
H92A C92 H92B 109.5 . .
H92A C92 H92C 109.5 . .
H92B C92 H92C 109.5 . .
N91 C93 H93A 109.5 . .
N91 C93 H93B 109.5 . .
N91 C93 H93C 109.5 . .
H93A C93 H93B 109.5 . .
H93A C93 H93C 109.5 . .
H93B C93 H93C 109.5 . .
C261 N261 C262 118.4(16) . .
C261 N261 C263 121.4(18) . .
C263 N261 C262 114.9(14) . .
O261 C261 N261 142(2) . .
O261 C261 H261 108.8 . .
N261 C261 H261 108.8 . .
N261 C262 H26A 109.5 . .
N261 C262 H26B 109.5 . .
N261 C262 H26C 109.5 . .
H26A C262 H26B 109.5 . .
H26A C262 H26C 109.5 . .
H26B C262 H26C 109.5 . .
N261 C263 H26D 109.5 . .
N261 C263 H26E 109.5 . .
N261 C263 H26F 109.5 . .
H26D C263 H26E 109.5 . .
H26D C263 H26F 109.5 . .
H26E C263 H26F 109.5 . .
C51 N51 C52 116.5(17) . .
C51 N51 C53 115.4(15) . .
C53 N51 C52 124.1(14) . .
O51 C51 N51 122.4(19) . .
O51 C51 H51 118.8 . .
N51 C51 H51 118.8 . .
N51 C52 H52A 109.5 . .
N51 C52 H52B 109.5 . .
N51 C52 H52C 109.5 . .
H52A C52 H52B 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
N51 C53 H53A 109.5 . .
N51 C53 H53B 109.5 . .
N51 C53 H53C 109.5 . .
H53A C53 H53B 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
C251 N251 C252 116.1(16) . .
C251 N251 C253 117.0(17) . .
C253 N251 C252 124.2(16) . .
O251 C251 N251 135(2) . .
O251 C251 H251 112.7 . .
N251 C251 H251 112.7 . .
N251 C252 H25A 109.5 . .
N251 C252 H25B 109.5 . .
N251 C252 H25C 109.5 . .
H25A C252 H25B 109.5 . .
H25A C252 H25C 109.5 . .
H25B C252 H25C 109.5 . .
N251 C253 H25D 109.5 . .
N251 C253 H25E 109.5 . .
N251 C253 H25F 109.5 . .
H25D C253 H25E 109.5 . .
H25D C253 H25F 109.5 . .
H25E C253 H25F 109.5 . .
C61 N61 C62 115.3(12) . .
C61 N61 C63 129.1(12) . .
C63 N61 C62 115.6(10) . .
O61 C61 N61 125.6(13) . .
O61 C61 H61 117.2 . .
N61 C61 H61 117.2 . .
N61 C62 H62A 109.5 . .
N61 C62 H62B 109.5 . .
N61 C62 H62C 109.5 . .
H62A C62 H62B 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
N61 C63 H63A 109.5 . .
N61 C63 H63B 109.5 . .
N61 C63 H63C 109.5 . .
H63A C63 H63B 109.5 . .
H63A C63 H63C 109.5 . .
H63B C63 H63C 109.5 . .
C71 N71 C72 115.8(19) . .
C71 N71 C73 121(2) . .
C73 N71 C72 122.0(19) . .
O71 C71 N71 134(2) . .
O71 C71 H71 112.8 . .
N71 C71 H71 112.8 . .
N71 C72 H72A 109.5 . .
N71 C72 H72B 109.5 . .
N71 C72 H72C 109.5 . .
H72A C72 H72B 109.5 . .
H72A C72 H72C 109.5 . .
H72B C72 H72C 109.5 . .
N71 C73 H73A 109.5 . .
N71 C73 H73B 109.5 . .
N71 C73 H73C 109.5 . .
H73A C73 H73B 109.5 . .
H73A C73 H73C 109.5 . .
H73B C73 H73C 109.5 . .
C81 N81 C82 115.5(18) . .
C81 N81 C83 121(2) . .
C83 N81 C82 123.1(19) . .
O81 C81 N81 127(2) . .
O81 C81 H81 116.4 . .
N81 C81 H81 116.4 . .
N81 C82 H82A 109.5 . .
N81 C82 H82B 109.5 . .
N81 C82 H82C 109.5 . .
H82A C82 H82B 109.5 . .
H82A C82 H82C 109.5 . .
H82B C82 H82C 109.5 . .
N81 C83 H83A 109.5 . .
N81 C83 H83B 109.5 . .
N81 C83 H83C 109.5 . .
H83A C83 H83B 109.5 . .
H83A C83 H83C 109.5 . .
H83B C83 H83C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.054(3) .
Mn1 O5 2.117(3) 6_565
Mn1 O6 2.339(2) 8_465
Mn1 O7 2.177(3) 8_465
Mn1 O31 2.260(7) .
Mn1 O41 2.091(9) .
Mn1 O231 2.094(18) .
Mn1 O241 2.153(13) .
Mn2 O3 2.205(2) 4_545
Mn2 O3 2.205(2) 6_566
Mn2 O4 2.115(2) .
Mn2 O4 2.115(2) 7_556
Mn2 O6 2.222(2) 5_666
Mn2 O6 2.222(2) 3_445
Si1 O1 1.623(3) 2_655
Si1 O1 1.623(3) .
Si1 C1 1.868(6) 2_655
Si1 C1 1.868(6) .
Si2 O1 1.627(3) .
Si2 C2 1.872(4) .
Si2 C9 1.876(4) .
Si2 C16 1.864(4) .
O2 C8 1.243(4) .
O3 Mn2 2.206(2) 4
O3 C8 1.252(4) .
O4 C15 1.251(4) .
O5 Mn1 2.117(3) 6_566
O5 C15 1.252(5) .
O6 Mn1 2.339(2) 8_566
O6 Mn2 2.222(2) 3
O6 C22 1.282(4) .
O7 Mn1 2.176(3) 8_566
O7 C22 1.256(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.394(5) .
C2 C7 1.390(5) .
C3 H3 0.9500 .
C3 C4 1.388(5) .
C4 H4 0.9500 .
C4 C5 1.391(5) .
C5 C6 1.372(5) .
C5 C8 1.509(5) .
C6 H6 0.9500 .
C6 C7 1.384(6) .
C7 H7 0.9500 .
C9 C10 1.402(5) .
C9 C14 1.374(6) .
C10 H10 0.9500 .
C10 C11 1.377(5) .
C11 H11 0.9500 .
C11 C12 1.375(6) .
C12 C13 1.390(5) .
C12 C15 1.497(5) .
C13 H13 0.9500 .
C13 C14 1.383(6) .
C14 H14 0.9500 .
C16 C17 1.401(5) .
C16 C21 1.381(6) .
C17 H17 0.9500 .
C17 C18 1.397(5) .
C18 H18 0.9500 .
C18 C19 1.386(5) .
C19 C20 1.399(5) .
C19 C22 1.485(5) .
C20 H20 0.9500 .
C20 C21 1.378(5) .
C21 H21 0.9500 .
O31 C31 1.268(9) .
N31 C31 1.306(9) .
N31 C32 1.519(12) .
N31 C33 1.465(11) .
C31 H31 0.9500 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
O41 C41 1.265(9) .
N41 C41 1.298(8) .
N41 C42 1.515(11) .
N41 C43 1.460(10) .
C41 H41 0.9500 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
O231 C231 1.271(10) .
N231 C231 1.302(9) .
N231 C232 1.516(12) .
N231 C233 1.465(11) .
C231 H231 0.9500 .
C232 H23A 0.9800 .
C232 H23B 0.9800 .
C232 H23C 0.9800 .
C233 H23E 0.9800 .
C233 H23F 0.9800 .
C233 H23G 0.9800 .
O241 C241 1.280(10) .
N241 C241 1.309(9) .
N241 C242 1.513(11) .
N241 C243 1.475(11) .
C241 H241 0.9500 .
C242 H24A 0.9800 .
C242 H24B 0.9800 .
C242 H24C 0.9800 .
C243 H24D 0.9800 .
C243 H24E 0.9800 .
C243 H24F 0.9800 .
O91 C91 1.273(10) .
N91 C91 1.304(10) .
N91 C92 1.513(12) .
N91 C93 1.463(12) .
C91 H23D 0.9500 .
C92 H92A 0.9800 .
C92 H92B 0.9800 .
C92 H92C 0.9800 .
C93 H93A 0.9800 .
C93 H93B 0.9800 .
C93 H93C 0.9800 .
O261 C261 1.261(10) .
N261 C261 1.292(9) .
N261 C262 1.507(12) .
N261 C263 1.458(11) .
C261 H261 0.9500 .
C262 H26A 0.9800 .
C262 H26B 0.9800 .
C262 H26C 0.9800 .
C263 H26D 0.9800 .
C263 H26E 0.9800 .
C263 H26F 0.9800 .
O51 C51 1.273(10) .
N51 C51 1.299(10) .
N51 C52 1.520(12) .
N51 C53 1.461(11) .
C51 H51 0.9500 .
C52 H52A 0.9800 .
C52 H52B 0.9800 .
C52 H52C 0.9800 .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
O251 C251 1.266(10) .
N251 C251 1.293(9) .
N251 C252 1.504(12) .
N251 C253 1.453(11) .
C251 H251 0.9500 .
C252 H25A 0.9800 .
C252 H25B 0.9800 .
C252 H25C 0.9800 .
C253 H25D 0.9800 .
C253 H25E 0.9800 .
C253 H25F 0.9800 .
O61 C61 1.273(10) .
N61 C61 1.298(8) .
N61 C62 1.512(12) .
N61 C63 1.458(11) .
C61 H61 0.9500 .
C62 H62A 0.9800 .
C62 H62B 0.9800 .
C62 H62C 0.9800 .
C63 H63A 0.9800 .
C63 H63B 0.9800 .
C63 H63C 0.9800 .
O71 C71 1.272(10) .
N71 C71 1.298(10) .
N71 C72 1.511(12) .
N71 C73 1.461(12) .
C71 H71 0.9500 .
C72 H72A 0.9800 .
C72 H72B 0.9800 .
C72 H72C 0.9800 .
C73 H73A 0.9800 .
C73 H73B 0.9800 .
C73 H73C 0.9800 .
O81 C81 1.275(10) .
N81 C81 1.300(10) .
N81 C82 1.515(12) .
N81 C83 1.456(12) .
C81 H81 0.9500 .
C82 H82A 0.9800 .
C82 H82B 0.9800 .
C82 H82C 0.9800 .
C83 H83A 0.9800 .
C83 H83B 0.9800 .
C83 H83C 0.9800 .
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
Mn1 O2 C8 O3 -5.6(8) .
Mn1 O2 C8 C5 173.1(3) .
Mn1 O5 C15 O4 7.7(5) 6_566
Mn1 O5 C15 C12 -173.2(2) 6_566
Mn1 O6 C22 O7 2.9(3) 8_566
Mn1 O6 C22 C19 -175.8(3) 8_566
Mn1 O7 C22 O6 -3.1(4) 8_566
Mn1 O7 C22 C19 175.6(3) 8_566
Mn1 O31 C31 N31 -175.2(16) .
Mn1 O41 C41 N41 60(2) .
Mn1 O231 C231 N231 32(9) .
Mn1 O241 C241 N241 -78(3) .
Mn2 O3 C8 O2 -20.8(6) 4
Mn2 O3 C8 C5 160.6(2) 4
Mn2 O4 C15 O5 25.5(6) .
Mn2 O4 C15 C12 -153.6(3) .
Mn2 O6 C22 O7 -113.6(4) 3
Mn2 O6 C22 C19 67.8(5) 3
Si2 C2 C3 C4 171.6(3) .
Si2 C2 C7 C6 -169.3(4) .
Si2 C9 C10 C11 177.7(3) .
Si2 C9 C14 C13 -176.6(3) .
Si2 C16 C17 C18 -177.8(3) .
Si2 C16 C21 C20 178.7(3) .
O1 Si1 O1 Si2 70.0(2) 2_655
O1 Si2 C2 C3 -82.5(4) .
O1 Si2 C2 C7 90.9(4) .
O1 Si2 C9 C10 14.6(3) .
O1 Si2 C9 C14 -168.2(3) .
O1 Si2 C16 C17 -39.7(3) .
O1 Si2 C16 C21 141.6(3) .
C1 Si1 O1 Si2 -46.3(4) .
C1 Si1 O1 Si2 -171.2(3) 2_655
C2 Si2 O1 Si1 -24.5(3) .
C2 Si2 C9 C10 135.0(3) .
C2 Si2 C9 C14 -47.8(4) .
C2 Si2 C16 C17 -161.6(3) .
C2 Si2 C16 C21 19.7(4) .
C2 C3 C4 C5 -0.9(6) .
C3 C2 C7 C6 4.5(7) .
C3 C4 C5 C6 1.4(6) .
C3 C4 C5 C8 -175.7(4) .
C4 C5 C6 C7 1.1(8) .
C4 C5 C8 O2 169.0(4) .
C4 C5 C8 O3 -12.2(5) .
C5 C6 C7 C2 -4.1(8) .
C6 C5 C8 O2 -8.0(6) .
C6 C5 C8 O3 170.8(4) .
C7 C2 C3 C4 -2.0(6) .
C8 C5 C6 C7 178.1(5) .
C9 Si2 O1 Si1 96.1(3) .
C9 Si2 C2 C3 158.6(3) .
C9 Si2 C2 C7 -28.0(4) .
C9 Si2 C16 C17 77.0(3) .
C9 Si2 C16 C21 -101.6(3) .
C9 C10 C11 C12 -0.4(6) .
C10 C9 C14 C13 0.6(6) .
C10 C11 C12 C13 -0.4(6) .
C10 C11 C12 C15 179.2(3) .
C11 C12 C13 C14 1.4(6) .
C11 C12 C15 O4 0.6(5) .
C11 C12 C15 O5 -178.6(3) .
C12 C13 C14 C9 -1.5(6) .
C13 C12 C15 O4 -179.8(3) .
C13 C12 C15 O5 1.0(5) .
C14 C9 C10 C11 0.3(6) .
C15 C12 C13 C14 -178.2(3) .
C16 Si2 O1 Si1 -147.1(3) .
C16 Si2 C2 C3 38.9(4) .
C16 Si2 C2 C7 -147.7(4) .
C16 Si2 C9 C10 -103.2(3) .
C16 Si2 C9 C14 74.0(3) .
C16 C17 C18 C19 -1.7(6) .
C17 C16 C21 C20 0.0(6) .
C17 C18 C19 C20 1.5(6) .
C17 C18 C19 C22 -178.6(3) .
C18 C19 C20 C21 -0.6(6) .
C18 C19 C22 O6 3.9(5) .
C18 C19 C22 O7 -174.8(3) .
C19 C20 C21 C16 -0.2(6) .
C20 C19 C22 O6 -176.2(3) .
C20 C19 C22 O7 5.1(5) .
C21 C16 C17 C18 0.9(6) .
C22 C19 C20 C21 179.5(4) .
C32 N31 C31 O31 22(3) .
C33 N31 C31 O31 171.0(15) .
C42 N41 C41 O41 -6(2) .
C43 N41 C41 O41 -173.5(12) .
C232 N231 C231 O231 -20(8) .
C233 N231 C231 O231 160(5) .
C242 N241 C241 O241 1(4) .
C243 N241 C241 O241 152(2) .
C92 N91 C91 O91 30(6) .
C93 N91 C91 O91 174(4) .
C262 N261 C261 O261 18(7) .
C263 N261 C261 O261 -135(5) .
C52 N51 C51 O51 52(4) .
C53 N51 C51 O51 -149(3) .
C252 N251 C251 O251 12(6) .
C253 N251 C251 O251 175(4) .
C62 N61 C61 O61 -8(3) .
C63 N61 C61 O61 175(2) .
C72 N71 C71 O71 -63(6) .
C73 N71 C71 O71 130(5) .
C82 N81 C81 O81 9(5) .
C83 N81 C81 O81 -177(4) .
