# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ligand_L
_database_code_depnum_ccdc_archive 'CCDC 1836630'
_audit_update_record             
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_ligand_L            
;
PROBLEM: Short Inter D...A Contact  O23      ..O33A             2.71 Ang.
RESPONSE: The water molecule which acts as a hydrogen bond donor is disordered and close to a special position, hence no protons could be found from the Fourier difference map. It is also involved in multiple hydrogen bonding interactions to neighbouring carboxylic acid groups hence calculated hydrogens were not added. This caused problems when trying to use HTAB to add these interactions to the CIF.
;
# Added during the CSD deposition process: Thursday 12 April 2018 11:30 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 O14 Si3, C2 H4 O2, 0.5(H2O)'
_chemical_formula_sum            'C46 H41 O16.50 Si3'
_chemical_formula_weight         942.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   15.1118(4)
_cell_length_b                   15.4367(5)
_cell_length_c                   40.6572(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.516(3)
_cell_angle_gamma                90
_cell_volume                     9440.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    173.00(14)
_cell_measurement_reflns_used    6164
_cell_measurement_theta_min      4.0810
_cell_measurement_theta_max      73.4110

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_F_000             3928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.533
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_T_min  0.97847
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.927
_oxdiff_exptl_absorpt_empirical_full_max 1.096
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      173.00(14)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            29868
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         6.446
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_full        66.599
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):
 
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     17.00 100.00   1.00   14.03    --   41.86  38.00 -90.00   83
  2  ω     83.00 177.00   1.00   64.84    --  106.38  61.00-120.00   94
  3  ω     95.00 178.00   1.00   64.84    --  106.38  30.00 -30.00   83
  4  ω    125.00 176.00   1.00   64.84    --  106.38 125.00  90.00   51
  5  ω     73.00 101.00   1.00   64.84    --  106.38 125.00  90.00   28
  6  ω     33.00 133.00   1.00   64.84    --  106.38 -77.00 120.00  100
  7  ω    -73.00  19.00   1.00   14.03    --  -41.86  77.00  60.00   92
;
_diffrn_measurement_method       'ω scans'
_reflns_number_total             16505
_reflns_number_gt                12216
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    Olex-2
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'enCIFer, Platon'

_refine_special_details          
;
Refined as a 2-component twin. The water molecule was positionally disordered
over two sites with the occupancy left to vary, and no protons attached to
the water molecule could be found from the difference map. This explains the
PLATON alerts relating to F000, formula and molecular weight.

Owing to the multiple hydrogen bonding interactions involving the disordered 
water, protons were not added using calculated values. This created problems 
when trying to use HTAB to add these hydrogen bonds to the CIF. Therefore the 
PLAT430_ALERT_2_B alerts do reflect genuine hydrogen bonds, but the 
uncertainty regarding the position of the hydrogen atoms means that they are
not in the CIF.
 
One of the oxygen atoms required an isotropic restraint to retain a sensible
thermal parameter.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1230P)²+14.0199P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16505
_refine_ls_number_parameters     1197
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.2439
_refine_ls_wR_factor_gt          0.2181
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
C1 C 0.3546(3) 1.0782(3) 0.10474(12) 0.0385(10) Uani 1 1 d . . . . .
C2 C 0.3192(3) 1.0968(3) 0.07245(13) 0.0429(11) Uani 1 1 d . . . . .
H2 H 0.280990 1.055723 0.060908 0.051 Uiso 1 1 calc R U . . .
C3 C 0.3382(4) 1.1736(4) 0.05682(13) 0.0449(12) Uani 1 1 d . . . . .
H3 H 0.313102 1.184824 0.034914 0.054 Uiso 1 1 calc R U . . .
C4 C 0.3942(3) 1.2337(3) 0.07342(13) 0.0408(11) Uani 1 1 d . . . . .
C5 C 0.4301(4) 1.2174(4) 0.10533(14) 0.0468(12) Uani 1 1 d . . . . .
H5 H 0.468250 1.258873 0.116650 0.056 Uiso 1 1 calc R U . . .
C6 C 0.4107(4) 1.1412(3) 0.12084(13) 0.0448(12) Uani 1 1 d . . . . .
H6 H 0.435703 1.131033 0.142839 0.054 Uiso 1 1 calc R U . . .
C7 C 0.4185(4) 1.3166(4) 0.05811(14) 0.0480(12) Uani 1 1 d . . . . .
C8 C 0.2389(3) 1.0019(3) 0.15488(12) 0.0375(10) Uani 1 1 d . . . . .
C9 C 0.2595(3) 1.0572(4) 0.18193(13) 0.0442(11) Uani 1 1 d . . . . .
H9 H 0.316499 1.083552 0.185035 0.053 Uiso 1 1 calc R U . . .
C10 C 0.1981(4) 1.0737(4) 0.20401(13) 0.0486(13) Uani 1 1 d . . . . .
H10 H 0.212979 1.111312 0.222190 0.058 Uiso 1 1 calc R U . . .
C11 C 0.1148(3) 1.0359(4) 0.19992(12) 0.0428(11) Uani 1 1 d . . . . .
C12 C 0.0926(3) 0.9818(4) 0.17291(14) 0.0487(13) Uani 1 1 d . . . . .
H12 H 0.035158 0.956523 0.169697 0.058 Uiso 1 1 calc R U . . .
C13 C 0.1546(3) 0.9652(4) 0.15083(14) 0.0458(12) Uani 1 1 d . . . . .
H13 H 0.139295 0.927898 0.132569 0.055 Uiso 1 1 calc R U . . .
C14 C 0.0513(4) 1.0530(4) 0.22469(13) 0.0495(13) Uani 1 1 d . . . . .
C15 C 0.4269(3) 0.9380(3) 0.15311(12) 0.0377(10) Uani 1 1 d . . . . .
C16 C 0.5135(3) 0.9456(4) 0.14423(13) 0.0436(11) Uani 1 1 d . . . . .
H16 H 0.523227 0.973939 0.124144 0.052 Uiso 1 1 calc R U . . .
C17 C 0.5852(3) 0.9130(3) 0.16394(13) 0.0415(11) Uani 1 1 d . . . . .
H17 H 0.643306 0.917251 0.156955 0.050 Uiso 1 1 calc R U . . .
C18 C 0.5729(3) 0.8739(3) 0.19401(13) 0.0407(11) Uani 1 1 d . . . . .
C19 C 0.4876(4) 0.8661(4) 0.20312(13) 0.0473(12) Uani 1 1 d . . . . .
H19 H 0.478450 0.839568 0.223605 0.057 Uiso 1 1 calc R U . . .
C20 C 0.4158(3) 0.8960(4) 0.18306(13) 0.0472(12) Uani 1 1 d . . . . .
H20 H 0.357570 0.888100 0.189554 0.057 Uiso 1 1 calc R U . . .
C21 C 0.6494(3) 0.8453(4) 0.21703(13) 0.0431(11) Uani 1 1 d . . . . .
C22 C 0.2797(3) 0.5724(3) 0.09321(12) 0.0380(10) Uani 1 1 d . . . . .
C23 C 0.2386(4) 0.5837(4) 0.06084(13) 0.0473(12) Uani 1 1 d . . . . .
H23 H 0.236970 0.639796 0.051231 0.057 Uiso 1 1 calc R U . . .
C24 C 0.2005(4) 0.5150(3) 0.04277(13) 0.0460(12) Uani 1 1 d . . . . .
H24 H 0.173960 0.523922 0.020892 0.055 Uiso 1 1 calc R U . . .
C25 C 0.2014(3) 0.4328(3) 0.05677(13) 0.0401(11) Uani 1 1 d . . . . .
C26 C 0.2421(4) 0.4196(3) 0.08850(13) 0.0430(11) Uani 1 1 d . . . . .
H26 H 0.243273 0.363190 0.097872 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2812(3) 0.4886(3) 0.10673(13) 0.0414(11) Uani 1 1 d . . . . .
H27 H 0.309083 0.478835 0.128369 0.050 Uiso 1 1 calc R U . . .
C28 C 0.1619(3) 0.3585(3) 0.03753(13) 0.0424(11) Uani 1 1 d . . . . .
C29 C 0.4198(3) 0.6501(3) 0.14667(12) 0.0380(10) Uani 1 1 d . . . . .
C30 C 0.5038(3) 0.6801(3) 0.13945(12) 0.0414(11) Uani 1 1 d . . . . .
H30 H 0.509247 0.709480 0.119221 0.050 Uiso 1 1 calc R U . . .
C31 C 0.5789(3) 0.6673(4) 0.16155(13) 0.0440(11) Uani 1 1 d . . . . .
H31 H 0.635383 0.686305 0.155983 0.053 Uiso 1 1 calc R U . . .
C32 C 0.5717(3) 0.6267(3) 0.19174(12) 0.0391(10) Uani 1 1 d . . . . .
C33 C 0.4898(3) 0.5958(4) 0.19913(13) 0.0448(12) Uani 1 1 d . . . . .
H33 H 0.484438 0.567506 0.219584 0.054 Uiso 1 1 calc R U . . .
C34 C 0.4157(3) 0.6064(4) 0.17664(13) 0.0449(12) Uani 1 1 d . . . . .
H34 H 0.360337 0.583274 0.181716 0.054 Uiso 1 1 calc R U . . .
C35 C 0.6499(3) 0.6173(3) 0.21671(13) 0.0419(11) Uani 1 1 d . . . . .
C36 C 0.2209(3) 0.7035(3) 0.14098(12) 0.0408(11) Uani 1 1 d . . . . .
C37 C 0.2286(3) 0.7277(4) 0.17407(13) 0.0453(12) Uani 1 1 d . . . . .
H37 H 0.285806 0.730106 0.185991 0.054 Uiso 1 1 calc R U . . .
C38 C 0.1542(4) 0.7482(4) 0.18996(14) 0.0516(13) Uani 1 1 d . . . . .
H38 H 0.161208 0.763790 0.212669 0.062 Uiso 1 1 calc R U . . .
C39 C 0.0695(4) 0.7463(4) 0.17323(14) 0.0469(12) Uani 1 1 d . . . . .
C40 C 0.0614(4) 0.7245(4) 0.13993(14) 0.0528(14) Uani 1 1 d . . . . .
H40 H 0.004504 0.725109 0.127756 0.063 Uiso 1 1 calc R U . . .
C41 C 0.1350(4) 0.7022(4) 0.12449(14) 0.0495(13) Uani 1 1 d . . . . .
H41 H 0.127460 0.685217 0.101930 0.059 Uiso 1 1 calc R U . . .
C42 C -0.0117(4) 0.7685(5) 0.18958(16) 0.0576(16) Uani 1 1 d . . . . .
C43 C 0.2379(6) 0.8297(5) 0.03866(16) 0.075(2) Uani 1 1 d . . . . .
H43A H 0.248684 0.778296 0.025474 0.112 Uiso 1 1 calc R U . . .
H43B H 0.239462 0.881573 0.024824 0.112 Uiso 1 1 calc R U . . .
H43C H 0.179536 0.824985 0.047100 0.112 Uiso 1 1 calc R U . . .
C44 C 0.4333(5) 0.8739(4) 0.06100(18) 0.0709(19) Uani 1 1 d . . . . .
H44A H 0.475395 0.881590 0.080670 0.106 Uiso 1 1 calc R U . . .
H44B H 0.425687 0.929037 0.049118 0.106 Uiso 1 1 calc R U . . .
H44C H 0.456273 0.830214 0.046539 0.106 Uiso 1 1 calc R U . . .
C45 C 0.7931(3) 0.5828(3) 0.09917(12) 0.0394(11) Uani 1 1 d . . . . .
C46 C 0.7623(4) 0.5973(4) 0.06589(13) 0.0472(12) Uani 1 1 d . . . . .
H46 H 0.762109 0.550695 0.050628 0.057 Uiso 1 1 calc R U . . .
C47 C 0.7325(4) 0.6777(4) 0.05484(13) 0.0496(13) Uani 1 1 d . . . . .
H47 H 0.712416 0.685807 0.032180 0.059 Uiso 1 1 calc R U . . .
C48 C 0.7316(3) 0.7465(4) 0.07666(13) 0.0451(12) Uani 1 1 d . . . . .
C49 C 0.7641(4) 0.7354(4) 0.10954(14) 0.0496(13) Uani 1 1 d . . . . .
H49 H 0.765289 0.782708 0.124509 0.060 Uiso 1 1 calc R U . . .
C50 C 0.7946(4) 0.6553(4) 0.12024(12) 0.0453(12) Uani 1 1 d . . . . .
H50 H 0.817437 0.648564 0.142692 0.054 Uiso 1 1 calc R U . . .
C51 C 0.6963(4) 0.8316(4) 0.06545(14) 0.0500(13) Uani 1 1 d . . . . .
C52 C 0.7316(3) 0.4373(3) 0.13997(13) 0.0406(11) Uani 1 1 d . . . . .
C53 C 0.7432(4) 0.3939(4) 0.17015(15) 0.0545(14) Uani 1 1 d . . . . .
H53 H 0.801489 0.378180 0.179004 0.065 Uiso 1 1 calc R U . . .
C54 C 0.6710(4) 0.3730(4) 0.18763(15) 0.0562(15) Uani 1 1 d . . . . .
H54 H 0.680400 0.347105 0.208877 0.067 Uiso 1 1 calc R U . . .
C55 C 0.5852(3) 0.3903(4) 0.17372(14) 0.0450(12) Uani 1 1 d . . . . .
C56 C 0.5720(3) 0.4312(4) 0.14313(13) 0.0452(12) Uani 1 1 d . . . . .
H56 H 0.513521 0.442760 0.133405 0.054 Uiso 1 1 calc R U . . .
C57 C 0.6445(3) 0.4547(4) 0.12712(13) 0.0439(12) Uani 1 1 d . . . . .
H57 H 0.634863 0.483907 0.106524 0.053 Uiso 1 1 calc R U . . .
C58 C 0.5059(4) 0.3667(4) 0.19062(15) 0.0495(13) Uani 1 1 d . . . . .
C59 C 0.9278(3) 0.4893(3) 0.14661(12) 0.0379(10) Uani 1 1 d . . . . .
C60 C 1.0133(3) 0.4734(4) 0.13750(12) 0.0422(11) Uani 1 1 d . . . . .
H60 H 1.020456 0.453578 0.115791 0.051 Uiso 1 1 calc R U . . .
C61 C 1.0875(3) 0.4861(4) 0.15960(13) 0.0439(12) Uani 1 1 d . . . . .
H61 H 1.145097 0.475773 0.152930 0.053 Uiso 1 1 calc R U . . .
C62 C 1.0780(3) 0.5137(4) 0.19131(13) 0.0432(11) Uani 1 1 d . . . . .
C63 C 0.9947(3) 0.5308(5) 0.20082(13) 0.0549(15) Uani 1 1 d . . . . .
H63 H 0.988179 0.550380 0.222610 0.066 Uiso 1 1 calc R U . . .
C64 C 0.9204(3) 0.5194(4) 0.17844(13) 0.0502(14) Uani 1 1 d . . . . .
H64 H 0.863271 0.532381 0.185015 0.060 Uiso 1 1 calc R U . . .
C65 C 1.1555(3) 0.5231(4) 0.21661(14) 0.0477(12) Uani 1 1 d . . . . .
C66 C 0.9700(3) 0.1947(3) 0.12469(12) 0.0368(10) Uani 1 1 d . . . . .
C67 C 1.0492(3) 0.1828(4) 0.11037(13) 0.0423(11) Uani 1 1 d . . . . .
H67 H 1.048315 0.153879 0.089723 0.051 Uiso 1 1 calc R U . . .
C68 C 1.1288(3) 0.2124(4) 0.12568(13) 0.0424(11) Uani 1 1 d . . . . .
H68 H 1.181988 0.204871 0.115305 0.051 Uiso 1 1 calc R U . . .
C69 C 1.1315(3) 0.2531(3) 0.15625(12) 0.0393(10) Uani 1 1 d . . . . .
C70 C 1.0526(3) 0.2654(4) 0.17091(13) 0.0473(12) Uani 1 1 d . . . . .
H70 H 1.053393 0.293690 0.191684 0.057 Uiso 1 1 calc R U . . .
C71 C 0.9737(3) 0.2363(4) 0.15510(13) 0.0458(12) Uani 1 1 d . . . . .
H71 H 0.920257 0.244904 0.165225 0.055 Uiso 1 1 calc R U . . .
C72 C 1.2163(3) 0.2858(4) 0.17321(13) 0.0444(12) Uani 1 1 d . . . . .
C73 C 0.7818(3) 0.1398(3) 0.13465(12) 0.0418(11) Uani 1 1 d . . . . .
C74 C 0.8079(4) 0.0877(4) 0.16248(13) 0.0468(12) Uani 1 1 d . . . . .
H74 H 0.865130 0.061697 0.164555 0.056 Uiso 1 1 calc R U . . .
C75 C 0.7516(4) 0.0741(4) 0.18662(13) 0.0491(13) Uani 1 1 d . . . . .
H75 H 0.769954 0.038280 0.205018 0.059 Uiso 1 1 calc R U . . .
C76 C 0.6684(3) 0.1123(4) 0.18426(13) 0.0431(11) Uani 1 1 d . . . . .
C77 C 0.6409(4) 0.1645(4) 0.15677(14) 0.0491(13) Uani 1 1 d . . . . .
H77 H 0.583568 0.190377 0.154771 0.059 Uiso 1 1 calc R U . . .
C78 C 0.6983(4) 0.1778(4) 0.13267(13) 0.0466(12) Uani 1 1 d . . . . .
H78 H 0.680030 0.213870 0.114333 0.056 Uiso 1 1 calc R U . . .
C79 C 0.6071(3) 0.0967(4) 0.20996(13) 0.0474(13) Uani 1 1 d . . . . .
C80 C 0.8770(3) 0.0649(3) 0.07638(12) 0.0417(11) Uani 1 1 d . . . . .
C81 C 0.8642(5) 0.0699(4) 0.04239(15) 0.0660(18) Uani 1 1 d . . . . .
H81 H 0.847095 0.123750 0.032403 0.079 Uiso 1 1 calc R U . . .
C82 C 0.8755(6) -0.0011(4) 0.02230(16) 0.072(2) Uani 1 1 d . . . . .
H82 H 0.868133 0.004905 -0.001053 0.086 Uiso 1 1 calc R U . . .
C83 C 0.8975(4) -0.0802(4) 0.03630(14) 0.0490(13) Uani 1 1 d . . . . .
C84 C 0.9119(5) -0.0879(4) 0.06979(16) 0.0618(16) Uani 1 1 d . . . . .
H84 H 0.928584 -0.142102 0.079567 0.074 Uiso 1 1 calc R U . . .
C85 C 0.9018(5) -0.0154(4) 0.08955(15) 0.0603(16) Uani 1 1 d . . . . .
H85 H 0.912317 -0.021216 0.112863 0.072 Uiso 1 1 calc R U . . .
C86 C 0.9001(4) -0.1579(4) 0.01468(15) 0.0512(13) Uani 1 1 d . . . . .
C87 C 0.7163(4) 0.3519(4) 0.03804(16) 0.0582(15) Uani 1 1 d . . . . .
H87A H 0.703657 0.305604 0.021776 0.087 Uiso 1 1 calc R U . . .
H87B H 0.717079 0.407797 0.026637 0.087 Uiso 1 1 calc R U . . .
H87C H 0.670195 0.352597 0.053409 0.087 Uiso 1 1 calc R U . . .
C88 C 0.9182(5) 0.3298(5) 0.03460(16) 0.0638(16) Uani 1 1 d . . . . .
H88A H 0.973538 0.315010 0.047978 0.096 Uiso 1 1 calc R U . . .
H88B H 0.924304 0.386864 0.024464 0.096 Uiso 1 1 calc R U . . .
H88C H 0.905748 0.286250 0.017252 0.096 Uiso 1 1 calc R U . . .
C89 C 0.4720(5) 0.6434(4) 0.02698(19) 0.0680(17) Uani 1 1 d . . . . .
H89A H 0.428347 0.677342 0.037859 0.102 Uiso 1 1 calc R U . . .
H89B H 0.463244 0.653195 0.003070 0.102 Uiso 1 1 calc R U . . .
H89C H 0.532140 0.661486 0.035359 0.102 Uiso 1 1 calc R U . . .
C90 C 0.4601(4) 0.5491(4) 0.03409(15) 0.0544(14) Uani 1 1 d . . . . .
C91 C 0.5672(6) 0.1408(5) 0.0301(2) 0.085(2) Uani 1 1 d . . . . .
H91A H 0.504036 0.135497 0.022281 0.127 Uiso 1 1 calc R U . . .
H91B H 0.599646 0.164420 0.012374 0.127 Uiso 1 1 calc R U . . .
H91C H 0.573992 0.179782 0.049210 0.127 Uiso 1 1 calc R U . . .
C92 C 0.6038(4) 0.0532(4) 0.03995(16) 0.0588(15) Uani 1 1 d . . . . .
O1 O 0.2886(2) 0.9066(2) 0.09979(8) 0.0409(8) Uani 1 1 d . . . . .
O2 O 0.3394(2) 0.7437(2) 0.09107(8) 0.0430(8) Uani 1 1 d . . . . .
O3 O 0.3726(3) 1.3384(3) 0.03122(10) 0.0508(9) Uani 1 1 d . . . . .
H3A H 0.391089 1.386042 0.024600 0.076 Uiso 1 1 calc R U . . .
O4 O 0.4802(3) 1.3603(3) 0.07149(14) 0.0789(15) Uani 1 1 d . . . . .
O5 O 0.0751(3) 1.0989(4) 0.24924(11) 0.0734(14) Uani 1 1 d . . . . .
O6 O -0.0256(3) 1.0174(4) 0.22004(10) 0.0675(12) Uani 1 1 d . . . . .
H6A H -0.055969 1.031253 0.235462 0.101 Uiso 1 1 calc R U . . .
O7 O 0.6419(2) 0.8193(3) 0.24519(9) 0.0511(9) Uani 1 1 d . . . . .
O8 O 0.7262(2) 0.8506(3) 0.20477(10) 0.0532(10) Uani 1 1 d . . . . .
H8 H 0.766654 0.833339 0.218880 0.080 Uiso 1 1 calc R U . . .
O9 O 0.1334(3) 0.3725(3) 0.00713(10) 0.0560(10) Uani 1 1 d . . . . .
H9A H 0.112474 0.326452 -0.001417 0.084 Uiso 1 1 calc R U . . .
O10 O 0.1569(3) 0.2857(2) 0.05102(9) 0.0514(9) Uani 1 1 d . . . . .
O11 O 0.6410(2) 0.6005(3) 0.24571(9) 0.0563(10) Uani 1 1 d . . . . .
O12 O 0.7273(2) 0.6295(3) 0.20584(10) 0.0568(10) Uani 1 1 d . . . . .
H12A H 0.767421 0.623020 0.221440 0.085 Uiso 1 1 calc R U . . .
O13 O 0.0041(3) 0.7722(4) 0.22166(12) 0.0847(18) Uani 1 1 d . . . . .
H13A H -0.043102 0.784413 0.230000 0.127 Uiso 1 1 calc R U . . .
O14 O -0.0835(3) 0.7795(4) 0.17510(13) 0.0876(17) Uani 1 1 d . U . . .
O15 O 0.8474(2) 0.4086(2) 0.08837(9) 0.0452(8) Uani 1 1 d . . . . .
O16 O 0.8189(2) 0.2390(2) 0.07910(8) 0.0438(8) Uani 1 1 d . . . . .
O17 O 0.6777(3) 0.8454(3) 0.03496(10) 0.0634(11) Uani 1 1 d . . . . .
O18 O 0.6871(4) 0.8889(3) 0.08798(11) 0.0712(13) Uani 1 1 d . . . . .
H18 H 0.667050 0.934901 0.079095 0.107 Uiso 1 1 calc R U . . .
O19 O 0.4322(3) 0.3628(3) 0.17624(11) 0.0634(12) Uani 1 1 d . . . . .
O20 O 0.5227(3) 0.3515(4) 0.22228(11) 0.0720(14) Uani 1 1 d . . . . .
H20A H 0.475235 0.338498 0.230309 0.108 Uiso 1 1 calc R U . . .
O21 O 1.2319(2) 0.5140(3) 0.20662(9) 0.0586(11) Uani 1 1 d . . . . .
H21 H 1.271000 0.520574 0.222564 0.088 Uiso 1 1 calc R U . . .
O22 O 1.1441(3) 0.5412(5) 0.24550(11) 0.0876(19) Uani 1 1 d . . . . .
O23 O 1.2238(3) 0.3084(4) 0.20199(11) 0.0745(15) Uani 1 1 d . . . . .
O24 O 1.2816(2) 0.2889(3) 0.15487(10) 0.0553(10) Uani 1 1 d . . . . .
H24A H 1.327217 0.307836 0.166038 0.083 Uiso 1 1 calc R U . . .
O25 O 0.5295(3) 0.1306(3) 0.20503(10) 0.0648(12) Uani 1 1 d . . . . .
H25 H 0.499888 0.118222 0.220838 0.097 Uiso 1 1 calc R U . . .
O26 O 0.6323(3) 0.0508(3) 0.23448(9) 0.0556(10) Uani 1 1 d . . . . .
O27 O 0.9190(3) -0.2302(3) 0.02673(12) 0.0673(12) Uani 1 1 d . . . . .
O28 O 0.8800(4) -0.1454(3) -0.01668(11) 0.0690(12) Uani 1 1 d . . . . .
H28 H 0.883243 -0.192578 -0.026800 0.103 Uiso 1 1 calc R U . . .
O29 O 0.4076(3) 0.5007(3) 0.01588(11) 0.0593(10) Uani 1 1 d . . . . .
O30 O 0.5035(3) 0.5227(3) 0.05962(12) 0.0735(13) Uani 1 1 d . . . . .
H30A H 0.493759 0.469589 0.062030 0.110 Uiso 1 1 calc R U . . .
O31 O 0.6183(4) 0.0009(3) 0.01716(11) 0.0752(14) Uani 1 1 d . . . . .
H31A H 0.638385 -0.045731 0.025494 0.113 Uiso 1 1 calc R U . . .
O32 O 0.6195(4) 0.0369(3) 0.07008(12) 0.0779(14) Uani 1 1 d . . . . .
O33A O 0.3685(12) 0.346(3) 0.2460(3) 0.052(8) Uani 0.42(8) 1 d . . P A 1
O33B O 0.3789(11) 0.295(4) 0.2439(4) 0.084(9) Uani 0.58(8) 1 d . . P A 2
SI1 Si 0.31779(9) 0.67003(9) 0.11788(3) 0.0362(3) Uani 1 1 d . . . . .
SI2 Si 0.32478(11) 0.83776(9) 0.07362(3) 0.0442(3) Uani 1 1 d . . . . .
SI3 Si 0.32667(8) 0.97833(8) 0.12688(3) 0.0352(3) Uani 1 1 d . . . . .
SI4 Si 0.82630(8) 0.47543(9) 0.11722(3) 0.0369(3) Uani 1 1 d . . . . .
SI5 Si 0.82575(8) 0.33253(9) 0.06121(3) 0.0353(3) Uani 1 1 d . . . . .
SI6 Si 0.86065(8) 0.16171(9) 0.10295(3) 0.0370(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.399(7) . ?
C1 C6 1.410(7) . ?
C1 SI3 1.854(5) . ?
C2 C3 1.388(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(8) . ?
C4 C7 1.485(8) . ?
C5 C6 1.379(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O4 1.235(7) . ?
C7 O3 1.282(7) . ?
C8 C13 1.390(7) . ?
C8 C9 1.403(7) . ?
C8 SI3 1.865(5) . ?
C9 C10 1.375(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(8) . ?
C11 C14 1.480(7) . ?
C12 C13 1.382(8) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 O5 1.249(7) . ?
C14 O6 1.283(7) . ?
C15 C16 1.395(7) . ?
C15 C20 1.404(7) . ?
C15 SI3 1.873(5) . ?
C16 C17 1.380(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(8) . ?
C18 C21 1.483(7) . ?
C19 C20 1.374(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 O7 1.229(6) . ?
C21 O8 1.310(6) . ?
C22 C27 1.405(7) . ?
C22 C23 1.411(7) . ?
C22 SI1 1.871(5) . ?
C23 C24 1.383(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(7) . ?
C25 C28 1.480(7) . ?
C26 C27 1.396(7) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 O10 1.256(7) . ?
C28 O9 1.287(7) . ?
C29 C34 1.399(7) . ?
C29 C30 1.407(7) . ?
C29 SI1 1.870(5) . ?
C30 C31 1.393(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.391(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.387(7) . ?
C32 C35 1.489(7) . ?
C33 C34 1.386(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 O11 1.227(7) . ?
C35 O12 1.304(6) . ?
C36 C37 1.390(7) . ?
C36 C41 1.403(7) . ?
C36 SI1 1.886(5) . ?
C37 C38 1.386(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.391(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.389(8) . ?
C39 C42 1.490(8) . ?
C40 C41 1.372(8) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 O14 1.197(7) . ?
C42 O13 1.304(8) . ?
C43 SI2 1.844(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 SI2 1.851(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.406(7) . ?
C45 C50 1.408(7) . ?
C45 SI4 1.862(6) . ?
C46 C47 1.380(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(8) . ?
C47 H47 0.9500 . ?
C48 C49 1.390(8) . ?
C48 C51 1.472(8) . ?
C49 C50 1.376(8) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 O17 1.263(7) . ?
C51 O18 1.291(7) . ?
C52 C57 1.394(7) . ?
C52 C53 1.395(8) . ?
C52 SI4 1.872(5) . ?
C53 C54 1.396(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.389(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.392(8) . ?
C55 C58 1.483(7) . ?
C56 C57 1.375(7) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 O19 1.209(7) . ?
C58 O20 1.309(7) . ?
C59 C64 1.389(7) . ?
C59 C60 1.399(7) . ?
C59 SI4 1.865(5) . ?
C60 C61 1.381(7) . ?
C60 H60 0.9500 . ?
C61 C62 1.378(7) . ?
C61 H61 0.9500 . ?
C62 C63 1.378(8) . ?
C62 C65 1.490(7) . ?
C63 C64 1.386(7) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
C65 O22 1.236(7) . ?
C65 O21 1.268(7) . ?
C66 C71 1.389(7) . ?
C66 C67 1.393(7) . ?
C66 SI6 1.868(5) . ?
C67 C68 1.378(7) . ?
C67 H67 0.9500 . ?
C68 C69 1.390(7) . ?
C68 H68 0.9500 . ?
C69 C70 1.397(7) . ?
C69 C72 1.484(7) . ?
C70 C71 1.374(7) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C72 O23 1.216(7) . ?
C72 O24 1.294(6) . ?
C73 C78 1.388(8) . ?
C73 C74 1.413(7) . ?
C73 SI6 1.868(5) . ?
C74 C75 1.375(8) . ?
C74 H74 0.9500 . ?
C75 C76 1.385(8) . ?
C75 H75 0.9500 . ?
C76 C77 1.408(8) . ?
C76 C79 1.481(7) . ?
C77 C78 1.385(8) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
C79 O26 1.251(7) . ?
C79 O25 1.282(7) . ?
C80 C81 1.379(8) . ?
C80 C85 1.388(8) . ?
C80 SI6 1.874(6) . ?
C81 C82 1.388(9) . ?
C81 H81 0.9500 . ?
C82 C83 1.374(9) . ?
C82 H82 0.9500 . ?
C83 C84 1.363(9) . ?
C83 C86 1.490(8) . ?
C84 C85 1.394(9) . ?
C84 H84 0.9500 . ?
C85 H85 0.9500 . ?
C86 O27 1.241(7) . ?
C86 O28 1.297(7) . ?
C87 SI5 1.847(6) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 SI5 1.848(6) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 C90 1.499(9) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 O30 1.242(8) . ?
C90 O29 1.275(8) . ?
C91 C92 1.501(10) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 O32 1.251(8) . ?
C92 O31 1.264(8) . ?
O1 SI3 1.628(3) . ?
O1 SI2 1.634(4) . ?
O2 SI2 1.621(4) . ?
O2 SI1 1.630(4) . ?
O3 H3A 0.8400 . ?
O6 H6A 0.8400 . ?
O8 H8 0.8400 . ?
O9 H9A 0.8400 . ?
O12 H12A 0.8400 . ?
O13 H13A 0.8400 . ?
O15 SI4 1.616(4) . ?
O15 SI5 1.624(4) . ?
O16 SI5 1.625(4) . ?
O16 SI6 1.626(4) . ?
O18 H18 0.8400 . ?
O20 H20A 0.8400 . ?
O21 H21 0.8400 . ?
O24 H24A 0.8400 . ?
O25 H25 0.8400 . ?
O28 H28 0.8400 . ?
O30 H30A 0.8400 . ?
O31 H31A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 116.9(5) . . ?
C2 C1 SI3 122.8(4) . . ?
C6 C1 SI3 120.2(4) . . ?
C3 C2 C1 121.8(5) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 C7 117.4(5) . . ?
C3 C4 C7 122.5(5) . . ?
C6 C5 C4 120.2(5) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 121.4(5) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
O4 C7 O3 123.8(5) . . ?
O4 C7 C4 119.5(5) . . ?
O3 C7 C4 116.6(5) . . ?
C13 C8 C9 118.2(5) . . ?
C13 C8 SI3 123.1(4) . . ?
C9 C8 SI3 118.7(4) . . ?
C10 C9 C8 120.7(5) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 120.5(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C12 119.6(5) . . ?
C10 C11 C14 119.0(5) . . ?
C12 C11 C14 121.4(5) . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C8 121.2(5) . . ?
C12 C13 H13 119.4 . . ?
C8 C13 H13 119.4 . . ?
O5 C14 O6 123.2(5) . . ?
O5 C14 C11 119.3(5) . . ?
O6 C14 C11 117.4(5) . . ?
C16 C15 C20 117.2(4) . . ?
C16 C15 SI3 123.5(4) . . ?
C20 C15 SI3 119.3(4) . . ?
C17 C16 C15 121.5(5) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 118.8(5) . . ?
C19 C18 C21 119.7(5) . . ?
C17 C18 C21 121.4(5) . . ?
C20 C19 C18 121.1(5) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C15 121.1(5) . . ?
C19 C20 H20 119.5 . . ?
C15 C20 H20 119.5 . . ?
O7 C21 O8 122.6(5) . . ?
O7 C21 C18 123.3(5) . . ?
O8 C21 C18 114.0(5) . . ?
C27 C22 C23 117.9(5) . . ?
C27 C22 SI1 122.6(4) . . ?
C23 C22 SI1 119.1(4) . . ?
C24 C23 C22 121.6(5) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 119.7(5) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 120.0(5) . . ?
C26 C25 C28 119.8(5) . . ?
C24 C25 C28 120.2(5) . . ?
C25 C26 C27 120.6(5) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C22 120.3(5) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
O10 C28 O9 122.7(5) . . ?
O10 C28 C25 120.0(5) . . ?
O9 C28 C25 117.3(5) . . ?
C34 C29 C30 117.2(5) . . ?
C34 C29 SI1 121.4(4) . . ?
C30 C29 SI1 121.4(4) . . ?
C31 C30 C29 121.0(5) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C32 C31 C30 120.3(5) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 119.5(5) . . ?
C33 C32 C35 119.0(5) . . ?
C31 C32 C35 121.4(5) . . ?
C34 C33 C32 119.9(5) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 122.0(5) . . ?
C33 C34 H34 119.0 . . ?
C29 C34 H34 119.0 . . ?
O11 C35 O12 122.7(5) . . ?
O11 C35 C32 121.6(5) . . ?
O12 C35 C32 115.7(5) . . ?
C37 C36 C41 117.0(5) . . ?
C37 C36 SI1 123.9(4) . . ?
C41 C36 SI1 119.0(4) . . ?
C38 C37 C36 121.1(5) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C37 C38 C39 121.1(5) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C40 C39 C38 118.2(5) . . ?
C40 C39 C42 119.4(5) . . ?
C38 C39 C42 122.4(5) . . ?
C41 C40 C39 120.5(5) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C36 122.1(5) . . ?
C40 C41 H41 119.0 . . ?
C36 C41 H41 119.0 . . ?
O14 C42 O13 123.7(6) . . ?
O14 C42 C39 124.1(6) . . ?
O13 C42 C39 112.2(5) . . ?
SI2 C43 H43A 109.5 . . ?
SI2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
SI2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
SI2 C44 H44A 109.5 . . ?
SI2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
SI2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C50 116.3(5) . . ?
C46 C45 SI4 125.0(4) . . ?
C50 C45 SI4 118.7(4) . . ?
C47 C46 C45 121.6(5) . . ?
C47 C46 H46 119.2 . . ?
C45 C46 H46 119.2 . . ?
C46 C47 C48 120.3(5) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C47 C48 C49 119.8(5) . . ?
C47 C48 C51 120.7(5) . . ?
C49 C48 C51 119.5(5) . . ?
C50 C49 C48 119.5(5) . . ?
C50 C49 H49 120.3 . . ?
C48 C49 H49 120.3 . . ?
C49 C50 C45 122.5(5) . . ?
C49 C50 H50 118.8 . . ?
C45 C50 H50 118.8 . . ?
O17 C51 O18 123.5(6) . . ?
O17 C51 C48 119.6(5) . . ?
O18 C51 C48 116.9(5) . . ?
C57 C52 C53 117.2(5) . . ?
C57 C52 SI4 119.5(4) . . ?
C53 C52 SI4 123.2(4) . . ?
C52 C53 C54 121.3(5) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
C55 C54 C53 119.5(5) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C54 C55 C56 119.9(5) . . ?
C54 C55 C58 121.9(5) . . ?
C56 C55 C58 118.2(5) . . ?
C57 C56 C55 119.3(5) . . ?
C57 C56 H56 120.3 . . ?
C55 C56 H56 120.3 . . ?
C56 C57 C52 122.5(5) . . ?
C56 C57 H57 118.7 . . ?
C52 C57 H57 118.7 . . ?
O19 C58 O20 123.3(5) . . ?
O19 C58 C55 122.4(5) . . ?
O20 C58 C55 114.3(5) . . ?
C64 C59 C60 117.7(4) . . ?
C64 C59 SI4 120.0(4) . . ?
C60 C59 SI4 122.3(4) . . ?
C61 C60 C59 121.0(5) . . ?
C61 C60 H60 119.5 . . ?
C59 C60 H60 119.5 . . ?
C62 C61 C60 120.1(5) . . ?
C62 C61 H61 119.9 . . ?
C60 C61 H61 119.9 . . ?
C63 C62 C61 120.1(5) . . ?
C63 C62 C65 117.8(5) . . ?
C61 C62 C65 122.0(5) . . ?
C62 C63 C64 119.7(5) . . ?
C62 C63 H63 120.2 . . ?
C64 C63 H63 120.2 . . ?
C63 C64 C59 121.4(5) . . ?
C63 C64 H64 119.3 . . ?
C59 C64 H64 119.3 . . ?
O22 C65 O21 123.0(5) . . ?
O22 C65 C62 120.4(5) . . ?
O21 C65 C62 116.6(5) . . ?
C71 C66 C67 118.0(4) . . ?
C71 C66 SI6 120.4(4) . . ?
C67 C66 SI6 121.5(4) . . ?
C68 C67 C66 121.1(5) . . ?
C68 C67 H67 119.5 . . ?
C66 C67 H67 119.5 . . ?
C67 C68 C69 120.2(5) . . ?
C67 C68 H68 119.9 . . ?
C69 C68 H68 119.9 . . ?
C68 C69 C70 119.3(4) . . ?
C68 C69 C72 121.3(5) . . ?
C70 C69 C72 119.3(5) . . ?
C71 C70 C69 119.6(5) . . ?
C71 C70 H70 120.2 . . ?
C69 C70 H70 120.2 . . ?
C70 C71 C66 121.7(5) . . ?
C70 C71 H71 119.1 . . ?
C66 C71 H71 119.1 . . ?
O23 C72 O24 122.5(5) . . ?
O23 C72 C69 122.8(5) . . ?
O24 C72 C69 114.7(5) . . ?
C78 C73 C74 118.0(5) . . ?
C78 C73 SI6 121.3(4) . . ?
C74 C73 SI6 120.6(4) . . ?
C75 C74 C73 121.0(5) . . ?
C75 C74 H74 119.5 . . ?
C73 C74 H74 119.5 . . ?
C74 C75 C76 120.4(5) . . ?
C74 C75 H75 119.8 . . ?
C76 C75 H75 119.8 . . ?
C75 C76 C77 119.7(5) . . ?
C75 C76 C79 120.5(5) . . ?
C77 C76 C79 119.8(5) . . ?
C78 C77 C76 119.3(5) . . ?
C78 C77 H77 120.3 . . ?
C76 C77 H77 120.3 . . ?
C77 C78 C73 121.6(5) . . ?
C77 C78 H78 119.2 . . ?
C73 C78 H78 119.2 . . ?
O26 C79 O25 124.0(5) . . ?
O26 C79 C76 119.5(5) . . ?
O25 C79 C76 116.5(5) . . ?
C81 C80 C85 116.3(5) . . ?
C81 C80 SI6 121.3(4) . . ?
C85 C80 SI6 122.4(4) . . ?
C80 C81 C82 122.1(6) . . ?
C80 C81 H81 118.9 . . ?
C82 C81 H81 118.9 . . ?
C83 C82 C81 119.8(6) . . ?
C83 C82 H82 120.1 . . ?
C81 C82 H82 120.1 . . ?
C84 C83 C82 120.0(6) . . ?
C84 C83 C86 120.5(5) . . ?
C82 C83 C86 119.3(5) . . ?
C83 C84 C85 119.3(6) . . ?
C83 C84 H84 120.3 . . ?
C85 C84 H84 120.3 . . ?
C80 C85 C84 122.3(6) . . ?
C80 C85 H85 118.8 . . ?
C84 C85 H85 118.8 . . ?
O27 C86 O28 123.0(5) . . ?
O27 C86 C83 120.6(5) . . ?
O28 C86 C83 116.3(5) . . ?
SI5 C87 H87A 109.5 . . ?
SI5 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
SI5 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
SI5 C88 H88A 109.5 . . ?
SI5 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
SI5 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C90 C89 H89A 109.5 . . ?
C90 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C90 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
O30 C90 O29 122.8(6) . . ?
O30 C90 C89 114.6(6) . . ?
O29 C90 C89 122.5(6) . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
O32 C92 O31 124.0(6) . . ?
O32 C92 C91 118.2(6) . . ?
O31 C92 C91 117.7(6) . . ?
SI3 O1 SI2 139.8(2) . . ?
SI2 O2 SI1 152.9(3) . . ?
C7 O3 H3A 109.5 . . ?
C14 O6 H6A 109.5 . . ?
C21 O8 H8 109.5 . . ?
C28 O9 H9A 109.5 . . ?
C35 O12 H12A 109.5 . . ?
C42 O13 H13A 109.5 . . ?
SI4 O15 SI5 156.1(2) . . ?
SI5 O16 SI6 151.8(2) . . ?
C51 O18 H18 109.5 . . ?
C58 O20 H20A 109.5 . . ?
C65 O21 H21 109.5 . . ?
C72 O24 H24A 109.5 . . ?
C79 O25 H25 109.5 . . ?
C86 O28 H28 109.5 . . ?
C90 O30 H30A 109.5 . . ?
C92 O31 H31A 109.5 . . ?
O2 SI1 C29 109.1(2) . . ?
O2 SI1 C22 106.0(2) . . ?
C29 SI1 C22 113.3(2) . . ?
O2 SI1 C36 110.9(2) . . ?
C29 SI1 C36 111.5(2) . . ?
C22 SI1 C36 105.9(2) . . ?
O2 SI2 O1 109.69(19) . . ?
O2 SI2 C43 109.5(3) . . ?
O1 SI2 C43 106.7(3) . . ?
O2 SI2 C44 107.7(3) . . ?
O1 SI2 C44 110.2(2) . . ?
C43 SI2 C44 113.0(4) . . ?
O1 SI3 C1 108.6(2) . . ?
O1 SI3 C8 108.7(2) . . ?
C1 SI3 C8 110.0(2) . . ?
O1 SI3 C15 111.9(2) . . ?
C1 SI3 C15 110.1(2) . . ?
C8 SI3 C15 107.5(2) . . ?
O15 SI4 C45 110.3(2) . . ?
O15 SI4 C59 109.3(2) . . ?
C45 SI4 C59 108.9(2) . . ?
O15 SI4 C52 111.8(2) . . ?
C45 SI4 C52 106.6(2) . . ?
C59 SI4 C52 109.9(2) . . ?
O15 SI5 O16 110.9(2) . . ?
O15 SI5 C87 110.0(3) . . ?
O16 SI5 C87 106.3(3) . . ?
O15 SI5 C88 107.5(3) . . ?
O16 SI5 C88 109.0(3) . . ?
C87 SI5 C88 113.3(3) . . ?
O16 SI6 C66 110.9(2) . . ?
O16 SI6 C73 107.9(2) . . ?
C66 SI6 C73 108.4(2) . . ?
O16 SI6 C80 107.8(2) . . ?
C66 SI6 C80 109.3(2) . . ?
C73 SI6 C80 112.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.2(8) . . . . ?
SI3 C1 C2 C3 177.4(4) . . . . ?
C1 C2 C3 C4 0.3(8) . . . . ?
C2 C3 C4 C5 -0.5(8) . . . . ?
C2 C3 C4 C7 179.2(5) . . . . ?
C3 C4 C5 C6 0.2(8) . . . . ?
C7 C4 C5 C6 -179.4(5) . . . . ?
C4 C5 C6 C1 0.3(8) . . . . ?
C2 C1 C6 C5 -0.4(8) . . . . ?
SI3 C1 C6 C5 -177.7(4) . . . . ?
C5 C4 C7 O4 12.5(8) . . . . ?
C3 C4 C7 O4 -167.1(6) . . . . ?
C5 C4 C7 O3 -167.4(5) . . . . ?
C3 C4 C7 O3 13.0(8) . . . . ?
C13 C8 C9 C10 0.7(8) . . . . ?
SI3 C8 C9 C10 -177.3(4) . . . . ?
C8 C9 C10 C11 0.1(9) . . . . ?
C9 C10 C11 C12 -1.0(8) . . . . ?
C9 C10 C11 C14 178.2(5) . . . . ?
C10 C11 C12 C13 1.3(8) . . . . ?
C14 C11 C12 C13 -178.0(5) . . . . ?
C11 C12 C13 C8 -0.5(9) . . . . ?
C9 C8 C13 C12 -0.5(8) . . . . ?
SI3 C8 C13 C12 177.5(4) . . . . ?
C10 C11 C14 O5 -2.2(8) . . . . ?
C12 C11 C14 O5 177.0(6) . . . . ?
C10 C11 C14 O6 179.5(5) . . . . ?
C12 C11 C14 O6 -1.2(8) . . . . ?
C20 C15 C16 C17 0.2(8) . . . . ?
SI3 C15 C16 C17 -178.3(4) . . . . ?
C15 C16 C17 C18 -2.2(8) . . . . ?
C16 C17 C18 C19 2.0(8) . . . . ?
C16 C17 C18 C21 -174.5(5) . . . . ?
C17 C18 C19 C20 0.1(9) . . . . ?
C21 C18 C19 C20 176.7(5) . . . . ?
C18 C19 C20 C15 -2.1(9) . . . . ?
C16 C15 C20 C19 1.9(9) . . . . ?
SI3 C15 C20 C19 -179.5(5) . . . . ?
C19 C18 C21 O7 -4.7(9) . . . . ?
C17 C18 C21 O7 171.8(5) . . . . ?
C19 C18 C21 O8 175.7(5) . . . . ?
C17 C18 C21 O8 -7.8(8) . . . . ?
C27 C22 C23 C24 0.2(8) . . . . ?
SI1 C22 C23 C24 -172.9(4) . . . . ?
C22 C23 C24 C25 0.9(9) . . . . ?
C23 C24 C25 C26 -1.5(8) . . . . ?
C23 C24 C25 C28 -179.2(5) . . . . ?
C24 C25 C26 C27 0.9(8) . . . . ?
C28 C25 C26 C27 178.6(5) . . . . ?
C25 C26 C27 C22 0.2(8) . . . . ?
C23 C22 C27 C26 -0.8(7) . . . . ?
SI1 C22 C27 C26 172.1(4) . . . . ?
C26 C25 C28 O10 7.5(7) . . . . ?
C24 C25 C28 O10 -174.8(5) . . . . ?
C26 C25 C28 O9 -172.9(5) . . . . ?
C24 C25 C28 O9 4.8(7) . . . . ?
C34 C29 C30 C31 -0.7(8) . . . . ?
SI1 C29 C30 C31 178.0(4) . . . . ?
C29 C30 C31 C32 -2.0(8) . . . . ?
C30 C31 C32 C33 2.7(8) . . . . ?
C30 C31 C32 C35 -176.0(5) . . . . ?
C31 C32 C33 C34 -0.7(8) . . . . ?
C35 C32 C33 C34 178.0(5) . . . . ?
C32 C33 C34 C29 -2.1(9) . . . . ?
C30 C29 C34 C33 2.7(8) . . . . ?
SI1 C29 C34 C33 -176.0(4) . . . . ?
C33 C32 C35 O11 -15.8(8) . . . . ?
C31 C32 C35 O11 162.9(5) . . . . ?
C33 C32 C35 O12 165.3(5) . . . . ?
C31 C32 C35 O12 -16.0(8) . . . . ?
C41 C36 C37 C38 0.8(9) . . . . ?
SI1 C36 C37 C38 -177.3(5) . . . . ?
C36 C37 C38 C39 -0.8(9) . . . . ?
C37 C38 C39 C40 -0.9(9) . . . . ?
C37 C38 C39 C42 -179.7(6) . . . . ?
C38 C39 C40 C41 2.6(9) . . . . ?
C42 C39 C40 C41 -178.6(6) . . . . ?
C39 C40 C41 C36 -2.6(10) . . . . ?
C37 C36 C41 C40 0.8(9) . . . . ?
SI1 C36 C41 C40 179.0(5) . . . . ?
C40 C39 C42 O14 -9.8(11) . . . . ?
C38 C39 C42 O14 168.9(7) . . . . ?
C40 C39 C42 O13 168.5(6) . . . . ?
C38 C39 C42 O13 -12.7(9) . . . . ?
C50 C45 C46 C47 -2.1(8) . . . . ?
SI4 C45 C46 C47 174.9(4) . . . . ?
C45 C46 C47 C48 -0.4(9) . . . . ?
C46 C47 C48 C49 2.5(9) . . . . ?
C46 C47 C48 C51 -177.4(5) . . . . ?
C47 C48 C49 C50 -1.8(8) . . . . ?
C51 C48 C49 C50 178.0(5) . . . . ?
C48 C49 C50 C45 -0.9(9) . . . . ?
C46 C45 C50 C49 2.8(8) . . . . ?
SI4 C45 C50 C49 -174.4(4) . . . . ?
C47 C48 C51 O17 -9.4(8) . . . . ?
C49 C48 C51 O17 170.7(5) . . . . ?
C47 C48 C51 O18 171.3(5) . . . . ?
C49 C48 C51 O18 -8.6(8) . . . . ?
C57 C52 C53 C54 -3.4(9) . . . . ?
SI4 C52 C53 C54 174.5(5) . . . . ?
C52 C53 C54 C55 4.5(10) . . . . ?
C53 C54 C55 C56 -2.4(10) . . . . ?
C53 C54 C55 C58 177.8(6) . . . . ?
C54 C55 C56 C57 -0.5(9) . . . . ?
C58 C55 C56 C57 179.2(5) . . . . ?
C55 C56 C57 C52 1.6(9) . . . . ?
C53 C52 C57 C56 0.4(9) . . . . ?
SI4 C52 C57 C56 -177.7(4) . . . . ?
C54 C55 C58 O19 -162.7(6) . . . . ?
C56 C55 C58 O19 17.5(9) . . . . ?
C54 C55 C58 O20 17.9(9) . . . . ?
C56 C55 C58 O20 -161.8(6) . . . . ?
C64 C59 C60 C61 0.9(9) . . . . ?
SI4 C59 C60 C61 178.6(4) . . . . ?
C59 C60 C61 C62 0.9(9) . . . . ?
C60 C61 C62 C63 -1.6(9) . . . . ?
C60 C61 C62 C65 176.1(5) . . . . ?
C61 C62 C63 C64 0.6(10) . . . . ?
C65 C62 C63 C64 -177.3(6) . . . . ?
C62 C63 C64 C59 1.2(11) . . . . ?
C60 C59 C64 C63 -1.9(9) . . . . ?
SI4 C59 C64 C63 -179.7(5) . . . . ?
C63 C62 C65 O22 3.7(10) . . . . ?
C61 C62 C65 O22 -174.1(7) . . . . ?
C63 C62 C65 O21 -174.3(6) . . . . ?
C61 C62 C65 O21 7.9(9) . . . . ?
C71 C66 C67 C68 -0.8(8) . . . . ?
SI6 C66 C67 C68 175.8(4) . . . . ?
C66 C67 C68 C69 1.5(8) . . . . ?
C67 C68 C69 C70 -1.4(8) . . . . ?
C67 C68 C69 C72 -179.7(5) . . . . ?
C68 C69 C70 C71 0.7(9) . . . . ?
C72 C69 C70 C71 179.1(5) . . . . ?
C69 C70 C71 C66 0.0(9) . . . . ?
C67 C66 C71 C70 0.1(9) . . . . ?
SI6 C66 C71 C70 -176.6(5) . . . . ?
C68 C69 C72 O23 -167.3(6) . . . . ?
C70 C69 C72 O23 14.3(9) . . . . ?
C68 C69 C72 O24 13.0(8) . . . . ?
C70 C69 C72 O24 -165.4(5) . . . . ?
C78 C73 C74 C75 1.0(8) . . . . ?
SI6 C73 C74 C75 177.3(4) . . . . ?
C73 C74 C75 C76 -0.8(9) . . . . ?
C74 C75 C76 C77 0.8(8) . . . . ?
C74 C75 C76 C79 179.0(5) . . . . ?
C75 C76 C77 C78 -0.9(8) . . . . ?
C79 C76 C77 C78 -179.1(5) . . . . ?
C76 C77 C78 C73 1.1(9) . . . . ?
C74 C73 C78 C77 -1.1(8) . . . . ?
SI6 C73 C78 C77 -177.4(4) . . . . ?
C75 C76 C79 O26 2.4(8) . . . . ?
C77 C76 C79 O26 -179.4(5) . . . . ?
C75 C76 C79 O25 -176.3(5) . . . . ?
C77 C76 C79 O25 1.9(8) . . . . ?
C85 C80 C81 C82 -0.1(11) . . . . ?
SI6 C80 C81 C82 -179.7(6) . . . . ?
C80 C81 C82 C83 2.1(13) . . . . ?
C81 C82 C83 C84 -2.9(12) . . . . ?
C81 C82 C83 C86 173.6(7) . . . . ?
C82 C83 C84 C85 1.7(10) . . . . ?
C86 C83 C84 C85 -174.7(6) . . . . ?
C81 C80 C85 C84 -1.2(10) . . . . ?
SI6 C80 C85 C84 178.4(5) . . . . ?
C83 C84 C85 C80 0.4(11) . . . . ?
C84 C83 C86 O27 -3.0(9) . . . . ?
C82 C83 C86 O27 -179.4(7) . . . . ?
C84 C83 C86 O28 175.7(6) . . . . ?
C82 C83 C86 O28 -0.8(9) . . . . ?
SI2 O2 SI1 C29 -117.5(5) . . . . ?
SI2 O2 SI1 C22 120.1(5) . . . . ?
SI2 O2 SI1 C36 5.6(6) . . . . ?
C34 C29 SI1 O2 164.4(4) . . . . ?
C30 C29 SI1 O2 -14.2(5) . . . . ?
C34 C29 SI1 C22 -77.8(5) . . . . ?
C30 C29 SI1 C22 103.5(4) . . . . ?
C34 C29 SI1 C36 41.6(5) . . . . ?
C30 C29 SI1 C36 -137.0(4) . . . . ?
C27 C22 SI1 O2 159.7(4) . . . . ?
C23 C22 SI1 O2 -27.6(5) . . . . ?
C27 C22 SI1 C29 40.0(5) . . . . ?
C23 C22 SI1 C29 -147.2(4) . . . . ?
C27 C22 SI1 C36 -82.5(5) . . . . ?
C23 C22 SI1 C36 90.3(4) . . . . ?
C37 C36 SI1 O2 -109.4(5) . . . . ?
C41 C36 SI1 O2 72.5(5) . . . . ?
C37 C36 SI1 C29 12.3(5) . . . . ?
C41 C36 SI1 C29 -165.8(4) . . . . ?
C37 C36 SI1 C22 136.1(5) . . . . ?
C41 C36 SI1 C22 -42.0(5) . . . . ?
SI1 O2 SI2 O1 27.1(6) . . . . ?
SI1 O2 SI2 C43 -89.7(6) . . . . ?
SI1 O2 SI2 C44 147.0(6) . . . . ?
SI3 O1 SI2 O2 93.0(4) . . . . ?
SI3 O1 SI2 C43 -148.5(4) . . . . ?
SI3 O1 SI2 C44 -25.5(5) . . . . ?
SI2 O1 SI3 C1 78.1(4) . . . . ?
SI2 O1 SI3 C8 -162.2(3) . . . . ?
SI2 O1 SI3 C15 -43.6(4) . . . . ?
C2 C1 SI3 O1 20.4(5) . . . . ?
C6 C1 SI3 O1 -162.5(4) . . . . ?
C2 C1 SI3 C8 -98.5(5) . . . . ?
C6 C1 SI3 C8 78.7(5) . . . . ?
C2 C1 SI3 C15 143.2(4) . . . . ?
C6 C1 SI3 C15 -39.7(5) . . . . ?
C13 C8 SI3 O1 -2.9(5) . . . . ?
C9 C8 SI3 O1 175.0(4) . . . . ?
C13 C8 SI3 C1 115.9(5) . . . . ?
C9 C8 SI3 C1 -66.1(5) . . . . ?
C13 C8 SI3 C15 -124.2(5) . . . . ?
C9 C8 SI3 C15 53.7(5) . . . . ?
C16 C15 SI3 O1 86.7(5) . . . . ?
C20 C15 SI3 O1 -91.8(5) . . . . ?
C16 C15 SI3 C1 -34.2(5) . . . . ?
C20 C15 SI3 C1 147.3(4) . . . . ?
C16 C15 SI3 C8 -154.0(4) . . . . ?
C20 C15 SI3 C8 27.4(5) . . . . ?
SI5 O15 SI4 C45 -94.6(7) . . . . ?
SI5 O15 SI4 C59 145.7(6) . . . . ?
SI5 O15 SI4 C52 23.7(7) . . . . ?
C46 C45 SI4 O15 19.4(5) . . . . ?
C50 C45 SI4 O15 -163.6(4) . . . . ?
C46 C45 SI4 C59 139.4(4) . . . . ?
C50 C45 SI4 C59 -43.7(5) . . . . ?
C46 C45 SI4 C52 -102.1(5) . . . . ?
C50 C45 SI4 C52 74.9(4) . . . . ?
C64 C59 SI4 O15 -159.0(5) . . . . ?
C60 C59 SI4 O15 23.4(5) . . . . ?
C64 C59 SI4 C45 80.5(5) . . . . ?
C60 C59 SI4 C45 -97.1(5) . . . . ?
C64 C59 SI4 C52 -35.9(5) . . . . ?
C60 C59 SI4 C52 146.5(5) . . . . ?
C57 C52 SI4 O15 -83.8(5) . . . . ?
C53 C52 SI4 O15 98.3(5) . . . . ?
C57 C52 SI4 C45 36.7(5) . . . . ?
C53 C52 SI4 C45 -141.2(5) . . . . ?
C57 C52 SI4 C59 154.6(4) . . . . ?
C53 C52 SI4 C59 -23.3(6) . . . . ?
SI4 O15 SI5 O16 -73.3(7) . . . . ?
SI4 O15 SI5 C87 43.9(7) . . . . ?
SI4 O15 SI5 C88 167.6(7) . . . . ?
SI6 O16 SI5 O15 -58.6(6) . . . . ?
SI6 O16 SI5 C87 -178.1(5) . . . . ?
SI6 O16 SI5 C88 59.5(6) . . . . ?
SI5 O16 SI6 C66 8.4(6) . . . . ?
SI5 O16 SI6 C73 127.0(5) . . . . ?
SI5 O16 SI6 C80 -111.3(5) . . . . ?
C71 C66 SI6 O16 89.4(5) . . . . ?
C67 C66 SI6 O16 -87.2(5) . . . . ?
C71 C66 SI6 C73 -29.0(5) . . . . ?
C67 C66 SI6 C73 154.5(4) . . . . ?
C71 C66 SI6 C80 -151.8(4) . . . . ?
C67 C66 SI6 C80 31.6(5) . . . . ?
C78 C73 SI6 O16 8.4(5) . . . . ?
C74 C73 SI6 O16 -167.8(4) . . . . ?
C78 C73 SI6 C66 128.6(4) . . . . ?
C74 C73 SI6 C66 -47.6(5) . . . . ?
C78 C73 SI6 C80 -110.4(5) . . . . ?
C74 C73 SI6 C80 73.4(5) . . . . ?
C81 C80 SI6 O16 7.4(6) . . . . ?
C85 C80 SI6 O16 -172.2(5) . . . . ?
C81 C80 SI6 C66 -113.3(5) . . . . ?
C85 C80 SI6 C66 67.1(5) . . . . ?
C81 C80 SI6 C73 126.2(5) . . . . ?
C85 C80 SI6 C73 -53.4(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O29_$1 0.84 1.83 2.647(6) 165.0 1_565
O6 H6A O26_$2 0.84 1.78 2.619(5) 171.9 2_565
O8 H8 O7_$3 0.84 1.92 2.750(5) 167.4 2_655
O9 H9A O27_$4 0.84 1.84 2.672(6) 168.6 3_655
O12 H12A O11_$3 0.84 1.86 2.699(5) 175.3 2_655
O13 H13A O7_$5 0.84 1.96 2.790(6) 171.8 2
O18 H18 O32_$1 0.84 1.76 2.579(7) 166.4 1_565
O20 H20A O33Aa 0.84 1.79 2.607(17) 162.2 .
O20 H20A O33Bb 0.84 1.74 2.571(14) 170.6 .
O21 H21 O22_$6 0.84 1.76 2.603(5) 175.7 2_755
O24 H24A O19_$7 0.84 1.81 2.617(5) 160.2 1_655
O25 H25 O5_$8 0.84 1.77 2.600(6) 172.0 2_545
O28 H28 O10_$4 0.84 1.81 2.608(6) 157.0 3_655
O30 H30A O4_$9 0.84 1.75 2.582(7) 173.4 1_545
O31 H31A O17_$9 0.84 1.81 2.640(7) 168.3 1_545

_refine_diff_density_max         1.012
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.188

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_IMP20
_database_code_depnum_ccdc_archive 'CCDC 1836631'
_audit_update_record             
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;

#2017ncs0062
_audit_creation_date             2017-08-11
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.07.04 svn.r3437 for OlexSys, GUI svn.r5361)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44H30 O14 Si3 Mn3 (C3H7NO)8'
_chemical_oxdiff_usercomment     LD_TS_Mn_AcOH(cone)
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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'

_cell_length_a                   18.9725(6)
_cell_length_b                   19.7061(5)
_cell_length_c                   25.3721(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.476(2)
_cell_angle_gamma                90
_cell_volume                     9382.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3360
_cell_measurement_theta_min      2.1480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_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
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7396
_reflns_number_total             10752
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       .
_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_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0833
_refine_ls_restrained_S_all      1.068
_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
_refine_special_details          
'There is disorder of multiple DMF molecules (both bound and free). As such various geometrical (SAME, FREE, BUMP) and displacement (DELU, SIMU, RIGU) restraints were employed.'
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 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_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 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) . . . . ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_IMP-21
_database_code_depnum_ccdc_archive 'CCDC 1836632'
_audit_update_record             
;
2018-04-12 deposited with the CCDC.
2018-06-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_CHEMW03_IMP-21              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The disordered solvent and dimethylammonium cation were removed using SQUEEZE. The atoms have been added to the formula moiety and sum lines in the CIF in order to obtain a charge-balanced compound.
;
# Added during the CSD deposition process: Thursday 12 April 2018 11:30 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H33 O16 Si3 Zn3, C2 H8 N, 3.75(C3 H7 N O)'
_chemical_formula_sum            'C59.25 H67.25 N4.75 O19.75 Si3 Zn3'
_chemical_formula_weight         1442.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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. 
;

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'

_cell_length_a                   32.1888(9)
_cell_length_b                   13.9804(3)
_cell_length_c                   30.8839(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.684(3)
_cell_angle_gamma                90
_cell_volume                     13829.8(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18718
_cell_measurement_theta_min      2.7970
_cell_measurement_theta_max      70.0160

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             5968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.312
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.30d (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63730
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.759
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12625
_reflns_number_gt                10298
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30d (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0835P)²+12.5203P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12625
_refine_ls_number_parameters     633
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.000000 0.17296(3) 0.250000 0.03536(13) Uani 1 2 d S T P . .
Zn2 Zn 0.05989(2) 0.17587(2) 0.34205(2) 0.03957(11) Uani 1 1 d . . . . .
Zn3 Zn 0.16537(2) 0.25250(2) 0.43454(2) 0.03731(11) Uani 1 1 d . . . . .
Zn4 Zn 0.250000 1.250000 0.500000 0.03416(13) Uani 1 2 d S . P . .
Si1 Si 0.25879(3) 0.68564(10) 0.24322(3) 0.0390(3) Uani 0.856(4) 1 d D U P A 1
Si1' Si 0.2543(2) 0.7350(7) 0.2370(2) 0.0484(19) Uiso 0.144(4) 1 d D U P A 2
O2 O 0.20871(6) 0.67392(13) 0.23779(7) 0.0454(5) Uani 1 1 d D . . . .
Si3 Si 0.16107(2) 0.67426(5) 0.21513(2) 0.03731(17) Uani 1 1 d . . . . .
O4 O 0.27028(7) 0.75266(12) 0.28619(6) 0.0441(5) Uani 1 1 d D . . . .
Si5 Si 0.29065(2) 0.75001(5) 0.33677(2) 0.03727(17) Uani 1 1 d . . . . .
C6 C 0.27598(13) 0.7441(3) 0.19496(13) 0.0631(11) Uani 0.856(4) 1 d D U P A 1
H6A H 0.264680 0.709565 0.168796 0.095 Uiso 0.856(4) 1 calc R U P A 1
H6B H 0.306545 0.743781 0.196781 0.095 Uiso 0.856(4) 1 calc R U P A 1
H6C H 0.265894 0.810301 0.193499 0.095 Uiso 0.856(4) 1 calc R U P A 1
C7 C 0.28144(13) 0.5649(3) 0.25177(13) 0.0627(11) Uani 0.856(4) 1 d D U P A 1
H7A H 0.278776 0.544306 0.281701 0.094 Uiso 0.856(4) 1 calc R U P A 1
H7B H 0.311011 0.566419 0.246726 0.094 Uiso 0.856(4) 1 calc R U P A 1
H7C H 0.266536 0.519941 0.231425 0.094 Uiso 0.856(4) 1 calc R U P A 1
C6' C 0.3015(7) 0.6742(17) 0.2217(9) 0.074(6) Uiso 0.144(4) 1 d D U P A 2
H6'A H 0.302513 0.609017 0.233407 0.111 Uiso 0.144(4) 1 calc R U P A 2
H6'B H 0.326309 0.709552 0.233664 0.111 Uiso 0.144(4) 1 calc R U P A 2
H6'C H 0.300741 0.671764 0.189924 0.111 Uiso 0.144(4) 1 calc R U P A 2
C7' C 0.2485(10) 0.8561(14) 0.2143(11) 0.091(7) Uiso 0.144(4) 1 d D U P A 2
H7'A H 0.248244 0.853163 0.182546 0.137 Uiso 0.144(4) 1 calc R U P A 2
H7'B H 0.271911 0.895900 0.226321 0.137 Uiso 0.144(4) 1 calc R U P A 2
H7'C H 0.222221 0.884030 0.221829 0.137 Uiso 0.144(4) 1 calc R U P A 2
C11 C 0.13489(8) 0.56481(18) 0.23364(9) 0.0375(6) Uani 1 1 d . . . . .
C12 C 0.15526(9) 0.5019(2) 0.26286(10) 0.0481(7) Uani 1 1 d . . . . .
H12 H 0.183701 0.513353 0.272794 0.058 Uiso 1 1 calc R U . . .
C13 C 0.13540(9) 0.4219(2) 0.27832(10) 0.0486(7) Uani 1 1 d . . . . .
H13 H 0.149913 0.381577 0.299485 0.058 Uiso 1 1 calc R U . . .
C14 C 0.09478(8) 0.40139(19) 0.26287(9) 0.0383(6) Uani 1 1 d . . . . .
C15 C 0.07371(9) 0.4623(2) 0.23283(10) 0.0470(7) Uani 1 1 d . . . . .
H15 H 0.045791 0.448346 0.221704 0.056 Uiso 1 1 calc R U . . .
C16 C 0.09329(9) 0.5437(2) 0.21895(10) 0.0483(7) Uani 1 1 d . . . . .
H16 H 0.078178 0.585917 0.199083 0.058 Uiso 1 1 calc R U . . .
C17 C 0.07319(8) 0.31430(19) 0.27841(9) 0.0387(6) Uani 1 1 d . . . . .
O18 O 0.08784(6) 0.27993(15) 0.31459(6) 0.0459(5) Uani 1 1 d . . . . .
O19 O 0.04283(6) 0.28295(14) 0.25433(6) 0.0434(4) Uani 1 1 d . . . . .
C21 C 0.15908(9) 0.67655(18) 0.15446(9) 0.0396(6) Uani 1 1 d . . . . .
C22 C 0.14322(11) 0.6018(2) 0.12850(10) 0.0566(8) Uani 1 1 d . . . . .
H22 H 0.132306 0.547167 0.141760 0.068 Uiso 1 1 calc R U . . .
C23 C 0.14289(11) 0.6047(2) 0.08325(10) 0.0572(8) Uani 1 1 d . . . . .
H23 H 0.131704 0.552557 0.066126 0.069 Uiso 1 1 calc R U . . .
C24 C 0.15885(9) 0.6834(2) 0.06336(9) 0.0425(6) Uani 1 1 d . . . . .
C25 C 0.17472(10) 0.75851(19) 0.08872(9) 0.0450(7) Uani 1 1 d . . . . .
H25 H 0.186067 0.812427 0.075329 0.054 Uiso 1 1 calc R U . . .
C26 C 0.17432(10) 0.7563(2) 0.13379(10) 0.0474(7) Uani 1 1 d . . . . .
H26 H 0.184540 0.809667 0.150668 0.057 Uiso 1 1 calc R U . . .
C27 C 0.15831(9) 0.6868(2) 0.01535(9) 0.0453(7) Uani 1 1 d . . . . .
O28 O 0.13590(8) 0.63293(19) -0.00828(7) 0.0700(7) Uani 1 1 d . . . . .
O29 O 0.18101(6) 0.75158(12) -0.00140(6) 0.0388(4) Uani 1 1 d . . . . .
C31 C 0.13503(9) 0.78380(19) 0.23411(9) 0.0389(6) Uani 1 1 d . . . . .
C32 C 0.10204(11) 0.8274(2) 0.20900(10) 0.0552(8) Uani 1 1 d . . . . .
H32 H 0.092949 0.801958 0.181156 0.066 Uiso 1 1 calc R U . . .
C33 C 0.08224(11) 0.9071(2) 0.22375(10) 0.0554(8) Uani 1 1 d . . . . .
H33 H 0.059965 0.935964 0.205900 0.067 Uiso 1 1 calc R U . . .
C34 C 0.09467(9) 0.94498(19) 0.26432(9) 0.0413(6) Uani 1 1 d . . . . .
C35 C 0.12740(10) 0.9033(2) 0.28957(10) 0.0568(8) Uani 1 1 d . . . . .
H35 H 0.136440 0.928954 0.317400 0.068 Uiso 1 1 calc R U . . .
C36 C 0.14727(10) 0.8232(2) 0.27412(10) 0.0541(8) Uani 1 1 d . . . . .
H36 H 0.169892 0.795150 0.291778 0.065 Uiso 1 1 calc R U . . .
C37 C 0.07211(9) 1.03056(19) 0.28020(9) 0.0428(6) Uani 1 1 d . . . . .
O38 O 0.04367(6) 1.06617(14) 0.25507(6) 0.0470(5) Uani 1 1 d . . . . .
O39 O 0.08378(7) 1.05975(14) 0.31842(7) 0.0535(5) Uani 1 1 d . . . . .
C41 C 0.27206(8) 0.85746(18) 0.36456(8) 0.0376(6) Uani 1 1 d . . . . .
C42 C 0.24097(10) 0.9155(2) 0.34456(10) 0.0494(7) Uani 1 1 d . . . . .
H42 H 0.229684 0.901340 0.315686 0.059 Uiso 1 1 calc R U . . .
C43 C 0.22598(10) 0.9937(2) 0.36568(9) 0.0497(7) Uani 1 1 d . . . . .
H43 H 0.204070 1.031191 0.351492 0.060 Uiso 1 1 calc R U . . .
C44 C 0.24263(9) 1.01779(18) 0.40731(9) 0.0390(6) Uani 1 1 d . . . . .
C45 C 0.27351(10) 0.9598(2) 0.42822(10) 0.0481(7) Uani 1 1 d . . . . .
H45 H 0.284911 0.974772 0.456973 0.058 Uiso 1 1 calc R U . . .
C46 C 0.28771(10) 0.8804(2) 0.40730(10) 0.0489(7) Uani 1 1 d . . . . .
H46 H 0.308434 0.840793 0.422172 0.059 Uiso 1 1 calc R U . . .
C47 C 0.22744(9) 1.10423(19) 0.42955(9) 0.0388(6) Uani 1 1 d . . . . .
O48 O 0.19402(6) 1.14108(14) 0.41305(6) 0.0468(5) Uani 1 1 d . . . . .
O49 O 0.24953(6) 1.13297(13) 0.46278(6) 0.0423(4) Uani 1 1 d . . . . .
C51 C 0.34889(9) 0.74833(18) 0.34005(10) 0.0413(6) Uani 1 1 d . . . . .
C52 C 0.37333(11) 0.8246(2) 0.35579(13) 0.0637(10) Uani 1 1 d . . . . .
H52 H 0.360234 0.879660 0.366337 0.076 Uiso 1 1 calc R U . . .
C53 C 0.41625(11) 0.8227(2) 0.35652(13) 0.0653(10) Uani 1 1 d . . . . .
H53 H 0.432277 0.875597 0.367944 0.078 Uiso 1 1 calc R U . . .
C54 C 0.43613(10) 0.7440(2) 0.34072(10) 0.0459(7) Uani 1 1 d . . . . .
C55 C 0.41247(9) 0.6671(2) 0.32473(10) 0.0448(7) Uani 1 1 d . . . . .
H55 H 0.425702 0.612914 0.313598 0.054 Uiso 1 1 calc R U . . .
C56 C 0.36943(9) 0.6689(2) 0.32492(10) 0.0453(7) Uani 1 1 d . . . . .
H56 H 0.353551 0.614825 0.314523 0.054 Uiso 1 1 calc R U . . .
C57 C 0.48228(10) 0.7419(2) 0.34146(11) 0.0528(8) Uani 1 1 d . . . . .
O58 O 0.50447(8) 0.7998(2) 0.36345(10) 0.0823(9) Uani 1 1 d . . . . .
O59 O 0.49876(6) 0.67474(13) 0.31993(6) 0.0417(4) Uani 1 1 d . . . . .
C61 C 0.27073(8) 0.64121(18) 0.36296(8) 0.0369(6) Uani 1 1 d . . . . .
C62 C 0.29425(9) 0.5912(2) 0.39602(10) 0.0460(7) Uani 1 1 d . . . . .
H62 H 0.321636 0.612387 0.405721 0.055 Uiso 1 1 calc R U . . .
C63 C 0.27819(9) 0.5108(2) 0.41491(10) 0.0463(7) Uani 1 1 d . . . . .
H63 H 0.294625 0.477894 0.437429 0.056 Uiso 1 1 calc R U . . .
C64 C 0.23849(8) 0.47839(18) 0.40122(8) 0.0372(6) Uani 1 1 d . . . . .
C65 C 0.21447(9) 0.5287(2) 0.36920(10) 0.0492(7) Uani 1 1 d . . . . .
H65 H 0.186868 0.508155 0.360007 0.059 Uiso 1 1 calc R U . . .
C66 C 0.23059(9) 0.6089(2) 0.35059(10) 0.0504(7) Uani 1 1 d . . . . .
H66 H 0.213678 0.642691 0.328740 0.060 Uiso 1 1 calc R U . . .
C67 C 0.22144(9) 0.39056(18) 0.42058(8) 0.0382(6) Uani 1 1 d . . . . .
O68 O 0.24486(6) 0.34540(14) 0.44777(6) 0.0440(4) Uani 1 1 d . . . . .
O69 O 0.18430(6) 0.36701(13) 0.40718(6) 0.0447(4) Uani 1 1 d . . . . .
C70 C 0.08372(11) 0.1623(3) 0.42681(10) 0.0608(9) Uani 1 1 d . . . . .
O71 O 0.05421(8) 0.1272(2) 0.40241(7) 0.0784(8) Uani 1 1 d . . . . .
O72 O 0.10878(6) 0.21808(16) 0.41190(6) 0.0480(5) Uani 1 1 d . . . . .
C73 C 0.08800(16) 0.1352(4) 0.47415(12) 0.1076(19) Uani 1 1 d . . . . .
H73A H 0.080927 0.190320 0.491611 0.161 Uiso 1 1 calc R U . . .
H73B H 0.116822 0.115538 0.482938 0.161 Uiso 1 1 calc R U . . .
H73C H 0.069037 0.082151 0.478747 0.161 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O38 2.0459(19) 2_545 ?
Zn1 O38 2.0459(19) 1_545 ?
Zn1 O19 2.0608(18) 2 ?
Zn1 O19 2.0608(19) . ?
Zn1 O59 2.1642(18) 4_545 ?
Zn1 O59 2.1642(18) 3_445 ?
Zn2 O18 1.9483(19) . ?
Zn2 O39 1.967(2) 1_545 ?
Zn2 O71 2.009(2) . ?
Zn2 O59 2.018(2) 3_445 ?
Zn3 O69 1.9365(19) . ?
Zn3 O72 1.946(2) . ?
Zn3 O48 1.9592(19) 1_545 ?
Zn3 O29 1.9935(19) 6_566 ?
Zn4 O49 1.9988(17) . ?
Zn4 O49 1.9988(17) 7_576 ?
Zn4 O68 2.0871(18) 7_566 ?
Zn4 O68 2.0871(18) 1_565 ?
Zn4 O29 2.2168(19) 6_576 ?
Zn4 O29 2.2168(19) 4 ?
Si1 O2 1.613(2) . ?
Si1 O4 1.637(2) . ?
Si1 C6 1.833(4) . ?
Si1 C7 1.847(4) . ?
Si1' O4 1.575(6) . ?
Si1' O2 1.700(7) . ?
Si1' C7' 1.835(15) . ?
Si1' C6' 1.843(14) . ?
O2 Si3 1.621(2) . ?
Si3 C11 1.864(3) . ?
Si3 C31 1.868(3) . ?
Si3 C21 1.869(3) . ?
O4 Si5 1.634(2) . ?
Si5 C41 1.858(3) . ?
Si5 C61 1.866(3) . ?
Si5 C51 1.867(3) . ?
C11 C12 1.379(4) . ?
C11 C16 1.402(4) . ?
C12 C13 1.396(4) . ?
C13 C14 1.377(4) . ?
C14 C15 1.386(4) . ?
C14 C17 1.504(4) . ?
C15 C16 1.389(4) . ?
C17 O19 1.248(3) . ?
C17 O18 1.264(3) . ?
C21 C22 1.384(4) . ?
C21 C26 1.398(4) . ?
C22 C23 1.397(4) . ?
C23 C24 1.384(4) . ?
C24 C25 1.378(4) . ?
C24 C27 1.482(4) . ?
C25 C26 1.394(4) . ?
C27 O28 1.231(4) . ?
C27 O29 1.303(3) . ?
C31 C36 1.375(4) . ?
C31 C32 1.392(4) . ?
C32 C33 1.383(4) . ?
C33 C34 1.383(4) . ?
C34 C35 1.376(4) . ?
C34 C37 1.507(4) . ?
C35 C36 1.397(4) . ?
C37 O38 1.244(3) . ?
C37 O39 1.270(3) . ?
C41 C42 1.385(4) . ?
C41 C46 1.403(4) . ?
C42 C43 1.384(4) . ?
C43 C44 1.385(4) . ?
C44 C45 1.391(4) . ?
C44 C47 1.496(3) . ?
C45 C46 1.384(4) . ?
C47 O48 1.255(3) . ?
C47 O49 1.255(3) . ?
C51 C52 1.385(4) . ?
C51 C56 1.397(4) . ?
C52 C53 1.380(5) . ?
C53 C54 1.385(4) . ?
C54 C55 1.381(4) . ?
C54 C57 1.484(4) . ?
C55 C56 1.386(4) . ?
C57 O58 1.237(4) . ?
C57 O59 1.294(4) . ?
C61 C66 1.386(4) . ?
C61 C62 1.397(4) . ?
C62 C63 1.389(4) . ?
C63 C64 1.382(4) . ?
C64 C65 1.385(4) . ?
C64 C67 1.494(4) . ?
C65 C66 1.384(4) . ?
C67 O68 1.243(3) . ?
C67 O69 1.269(3) . ?
C70 O72 1.243(4) . ?
C70 O71 1.252(4) . ?
C70 C73 1.503(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O38 Zn1 O38 86.27(12) 2_545 1_545 ?
O38 Zn1 O19 95.13(8) 2_545 2 ?
O38 Zn1 O19 178.49(8) 1_545 2 ?
O38 Zn1 O19 178.49(8) 2_545 . ?
O38 Zn1 O19 95.13(8) 1_545 . ?
O19 Zn1 O19 83.48(11) 2 . ?
O38 Zn1 O59 90.71(7) 2_545 4_545 ?
O38 Zn1 O59 90.25(7) 1_545 4_545 ?
O19 Zn1 O59 90.28(7) 2 4_545 ?
O19 Zn1 O59 88.73(7) . 4_545 ?
O38 Zn1 O59 90.25(7) 2_545 3_445 ?
O38 Zn1 O59 90.71(7) 1_545 3_445 ?
O19 Zn1 O59 88.73(7) 2 3_445 ?
O19 Zn1 O59 90.29(7) . 3_445 ?
O59 Zn1 O59 178.68(10) 4_545 3_445 ?
O18 Zn2 O39 103.91(9) . 1_545 ?
O18 Zn2 O71 138.14(10) . . ?
O39 Zn2 O71 98.04(11) 1_545 . ?
O18 Zn2 O59 109.58(8) . 3_445 ?
O39 Zn2 O59 105.77(8) 1_545 3_445 ?
O71 Zn2 O59 97.82(9) . 3_445 ?
O69 Zn3 O72 111.80(8) . . ?
O69 Zn3 O48 109.30(9) . 1_545 ?
O72 Zn3 O48 97.86(9) . 1_545 ?
O69 Zn3 O29 113.41(8) . 6_566 ?
O72 Zn3 O29 119.01(8) . 6_566 ?
O48 Zn3 O29 103.44(8) 1_545 6_566 ?
O49 Zn4 O49 180.0 . 7_576 ?
O49 Zn4 O68 85.24(8) . 7_566 ?
O49 Zn4 O68 94.76(8) 7_576 7_566 ?
O49 Zn4 O68 94.76(8) . 1_565 ?
O49 Zn4 O68 85.24(8) 7_576 1_565 ?
O68 Zn4 O68 180.00(7) 7_566 1_565 ?
O49 Zn4 O29 91.73(7) . 6_576 ?
O49 Zn4 O29 88.27(7) 7_576 6_576 ?
O68 Zn4 O29 90.65(7) 7_566 6_576 ?
O68 Zn4 O29 89.35(7) 1_565 6_576 ?
O49 Zn4 O29 88.27(7) . 4 ?
O49 Zn4 O29 91.73(7) 7_576 4 ?
O68 Zn4 O29 89.35(7) 7_566 4 ?
O68 Zn4 O29 90.65(7) 1_565 4 ?
O29 Zn4 O29 180.00(10) 6_576 4 ?
O2 Si1 O4 106.60(12) . . ?
O2 Si1 C6 109.88(17) . . ?
O4 Si1 C6 109.99(16) . . ?
O2 Si1 C7 107.35(17) . . ?
O4 Si1 C7 110.66(15) . . ?
C6 Si1 C7 112.2(2) . . ?
O4 Si1' O2 105.3(4) . . ?
O4 Si1' C7' 103.6(12) . . ?
O2 Si1' C7' 114.5(11) . . ?
O4 Si1' C6' 96.9(10) . . ?
O2 Si1' C6' 120.4(10) . . ?
C7' Si1' C6' 112.5(11) . . ?
Si1 O2 Si3 159.65(14) . . ?
Si3 O2 Si1' 140.6(3) . . ?
O2 Si3 C11 107.60(11) . . ?
O2 Si3 C31 107.56(12) . . ?
C11 Si3 C31 110.26(12) . . ?
O2 Si3 C21 111.72(12) . . ?
C11 Si3 C21 110.48(12) . . ?
C31 Si3 C21 109.18(12) . . ?
Si1' O4 Si5 168.9(4) . . ?
Si5 O4 Si1 143.08(13) . . ?
O4 Si5 C41 107.83(11) . . ?
O4 Si5 C61 108.08(11) . . ?
C41 Si5 C61 108.58(12) . . ?
O4 Si5 C51 110.96(12) . . ?
C41 Si5 C51 110.65(12) . . ?
C61 Si5 C51 110.63(12) . . ?
C12 C11 C16 117.0(2) . . ?
C12 C11 Si3 121.6(2) . . ?
C16 C11 Si3 121.3(2) . . ?
C11 C12 C13 122.1(3) . . ?
C14 C13 C12 120.0(3) . . ?
C13 C14 C15 119.3(2) . . ?
C13 C14 C17 120.7(2) . . ?
C15 C14 C17 120.0(2) . . ?
C14 C15 C16 120.2(3) . . ?
C15 C16 C11 121.4(3) . . ?
O19 C17 O18 126.5(2) . . ?
O19 C17 C14 117.0(2) . . ?
O18 C17 C14 116.5(2) . . ?
C17 O18 Zn2 121.40(18) . . ?
C17 O19 Zn1 141.30(18) . . ?
C22 C21 C26 117.6(3) . . ?
C22 C21 Si3 122.8(2) . . ?
C26 C21 Si3 119.5(2) . . ?
C21 C22 C23 121.6(3) . . ?
C24 C23 C22 120.1(3) . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 C27 120.8(2) . . ?
C23 C24 C27 120.1(3) . . ?
C24 C25 C26 120.8(3) . . ?
C25 C26 C21 120.8(3) . . ?
O28 C27 O29 120.6(3) . . ?
O28 C27 C24 121.4(3) . . ?
O29 C27 C24 117.9(3) . . ?
C27 O29 Zn3 106.13(17) . 6_565 ?
C27 O29 Zn4 125.85(17) . 4_545 ?
Zn3 O29 Zn4 99.96(8) 6_565 4_545 ?
C36 C31 C32 117.4(3) . . ?
C36 C31 Si3 120.9(2) . . ?
C32 C31 Si3 121.7(2) . . ?
C33 C32 C31 121.4(3) . . ?
C34 C33 C32 120.4(3) . . ?
C35 C34 C33 119.2(3) . . ?
C35 C34 C37 121.2(3) . . ?
C33 C34 C37 119.6(3) . . ?
C34 C35 C36 119.8(3) . . ?
C31 C36 C35 121.9(3) . . ?
O38 C37 O39 125.6(3) . . ?
O38 C37 C34 117.6(3) . . ?
O39 C37 C34 116.7(2) . . ?
C37 O38 Zn1 142.89(19) . 1_565 ?
C37 O39 Zn2 121.29(18) . 1_565 ?
C42 C41 C46 117.5(2) . . ?
C42 C41 Si5 121.3(2) . . ?
C46 C41 Si5 121.2(2) . . ?
C43 C42 C41 121.5(3) . . ?
C42 C43 C44 120.6(3) . . ?
C43 C44 C45 118.9(2) . . ?
C43 C44 C47 120.6(3) . . ?
C45 C44 C47 120.6(2) . . ?
C46 C45 C44 120.3(3) . . ?
C45 C46 C41 121.2(3) . . ?
O48 C47 O49 126.5(2) . . ?
O48 C47 C44 116.8(2) . . ?
O49 C47 C44 116.7(2) . . ?
C47 O48 Zn3 127.03(17) . 1_565 ?
C47 O49 Zn4 134.72(18) . . ?
C52 C51 C56 117.3(3) . . ?
C52 C51 Si5 122.8(2) . . ?
C56 C51 Si5 119.9(2) . . ?
C53 C52 C51 121.6(3) . . ?
C52 C53 C54 120.5(3) . . ?
C55 C54 C53 119.1(3) . . ?
C55 C54 C57 120.4(3) . . ?
C53 C54 C57 120.5(3) . . ?
C54 C55 C56 120.0(3) . . ?
C55 C56 C51 121.5(3) . . ?
O58 C57 O59 120.9(3) . . ?
O58 C57 C54 121.2(3) . . ?
O59 C57 C54 117.9(3) . . ?
C57 O59 Zn2 104.83(18) . 3 ?
C57 O59 Zn1 124.8(2) . 3 ?
Zn2 O59 Zn1 102.95(8) 3 3 ?
C66 C61 C62 117.4(3) . . ?
C66 C61 Si5 119.8(2) . . ?
C62 C61 Si5 122.7(2) . . ?
C63 C62 C61 121.0(3) . . ?
C64 C63 C62 120.5(3) . . ?
C63 C64 C65 119.1(3) . . ?
C63 C64 C67 120.8(2) . . ?
C65 C64 C67 120.1(2) . . ?
C66 C65 C64 120.1(3) . . ?
C65 C66 C61 121.8(3) . . ?
O68 C67 O69 125.2(2) . . ?
O68 C67 C64 117.7(2) . . ?
O69 C67 C64 117.0(2) . . ?
C67 O68 Zn4 147.43(19) . 1_545 ?
C67 O69 Zn3 113.51(17) . . ?
O72 C70 O71 120.3(3) . . ?
O72 C70 C73 121.2(3) . . ?
O71 C70 C73 118.5(3) . . ?
C70 O71 Zn2 107.0(2) . . ?
C70 O72 Zn3 129.9(2) . . ?

_refine_diff_density_max         0.767
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.071



#===END

