# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_compound_1
_audit_block_doi                 10.5517/cc7b6c3
_database_code_depnum_ccdc_archive 'CCDC 218344'
_audit_update_record             
;
2003-08-27 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;

_audit_creation_method           'manually at CCDC'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_sum            C69
_chemical_formula_moiety         ?
_chemical_formula_weight         1970.13
_chemical_melting_point          ?

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P43
_symmetry_Int_Tables_number      ?

_cell_length_a                   13.214(2)
_cell_length_b                   13.214(2)
_cell_length_c                   43.809(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     ?
_cell_formula_units_Z            4

_exptl_crystal_density_diffrn    1.711
_exptl_crystal_description       'trapezoidal block'
_exptl_crystal_colour            gold
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203
_diffrn_radiation_probe          x-ray

_refine_ls_R_factor_gt           0.041
_refine_special_details          
;
?
;

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ru1 0.4248,1 -0.1955,1 -0.0540
Ru2 0.5507,1 0.2052,1 -0.0541
Ru3 0.28077,7 0.07077,8 0.05474,3
Ru4 0.68131,7 -0.05537,8 0.05744,2
S1 0.6937,3 0.3950,3 0.0584,1
S2 0.8728,3 -0.2057,3 -0.0548,1
S3 0.2693,3 -0.3835,3 0.0590,1
S4 0.0939,3 0.2193,3 -0.0590,1
F11 0.8730,8 0.3407,9 0.0415,3
F12 0.8172,7 0.4668,6 0.0171,3
F13 0.8680,8 0.4868,9 0.0620,3
F21 0.9630,8 -0.3799,8 -0.0592,3
F22 0.9455,7 -0.3266,7 -0.0137,3
F23 0.8180,9 -0.3856,7 -0.0374,3
F31 0.0919,7 -0.3200,9 0.0424,3
F32 0.1421,7 -0.4492,6 0.0175,3
F33 0.0914,9 -0.4682,12 0.0626,4
F41 0.0097,10 0.3952,8 -0.0640,3
F42 0.1571,8 0.3984,7 -0.0423,3
F43 0.0305,7 0.3450,7 -0.0182,3
O1W 0.4805,7 0.5041,6 0.0144,3
O2W 0.9833,6 0.0092,7 -0.0137,3
O3W 0.1084,8 -0.2021,10 0.1115,3
O4W 0.8811,9 0.2316,13 0.1113,3
O5W 0.6052,10 0.2797,15 0.1366,4
O6W 0.3780,9 -0.2836,9 0.1380,4
O11 0.6447,8 0.4909,7 0.0611,3
O12 0.6535,8 0.3265,7 0.0362,3
O13 0.7154,9 0.3490,9 0.0881,3
O21 0.8225,8 -0.2264,8 -0.0836,3
O22 0.8044,7 -0.1640,8 -0.0312,3
O23 0.9692,7 -0.1571,8 -0.0569,4
O31 0.3115,9 -0.3169,9 0.0375,3
O32 0.3145,8 -0.4822,7 0.0602,3
O33 0.2532,9 -0.3425,9 0.0886,3
O41 0.1614,8 0.1774,9 -0.0359,3
O42 0.1391,11 0.2359,10 -0.0876,3
O43 -0.0044,7 0.1744,8 -0.0591,3
C1 0.4848,5 0.0057,8 0.0008,4
C1S 0.8172,11 0.4233,12 0.0453,4
C2S 0.9026,12 -0.3298,11 -0.0393,4
C3S 0.1413,11 -0.4063,12 0.0463,4
C4S 0.0707,13 0.3451,12 -0.0440,5
C10 0.2777,9 -0.1445,10 -0.0723,3
C11 0.2637,8 -0.2341,9 -0.0552,4
C11' 0.5018,8 -0.0912,7 -0.0174,3
C12 0.3228,10 -0.3123,10 -0.0682,4
C12' 0.5546,8 -0.0897,9 -0.0459,3
C13 0.3698,9 -0.2730,11 -0.0938,4
C13' 0.5888,8 -0.1802,9 -0.0609,3
C14 0.3436,10 -0.1721,13 -0.0973,3
C14' 0.5700,10 -0.2728,10 -0.0464,4
C15 0.2150,11 -0.0477,11 -0.0700,4
C15' 0.5146,10 -0.2788,9 -0.0189,3
C16 0.1904,10 -0.2428,12 -0.0273,4
C16' 0.4775,10 -0.1907,9 -0.0063,3
C17 0.3226,13 -0.4188,12 -0.0568,7
C18 0.4360,12 -0.3303,19 -0.1163,5
C19 0.3740,12 -0.1017,15 -0.1221,4
C20 0.6981,8 0.1534,9 -0.0717,3
C21 0.6352,10 0.1892,13 -0.0966,4
C21' 0.4701,9 0.1017,8 -0.0179,3
C22 0.6128,10 0.2894,11 -0.0917,4
C22' 0.4932,9 0.2000,9 -0.0066,3
C23 0.6586,10 0.3209,9 -0.0653,3
C23' 0.4560,9 0.2883,10 -0.0210,4
C24 0.7145,9 0.2374,10 -0.0532,4
C24' 0.4032,9 0.2819,9 -0.0480,4
C25 0.7537,10 0.0552,11 -0.0716,4
C25' 0.3887,8 0.1871,9 -0.0620,3
C26 0.6049,11 0.1248,16 -0.1244,4
C26' 0.4197,9 0.0978,9 -0.0468,3
C27 0.5519,13 0.3586,15 -0.1127,5
C28 0.6585,13 0.4274,11 -0.0529,6
C29 0.7823,9 0.2397,10 -0.0245,4
C30 0.2457,8 0.2346,9 0.0530,4
C31 0.3298,10 0.2213,10 0.0751,4
C31' 0.3854,9 -0.0086,8 0.0206,3
C32 0.3006,12 0.1542,12 0.0976,4
C32' 0.3886,9 -0.0608,8 0.0490,3
C33 0.1919,10 0.1292,10 0.0919,4
C33' 0.2980,9 -0.0924,9 0.0625,4
C34 0.1621,10 0.1820,10 0.0651,4
C34' 0.2050,10 -0.0757,10 0.0492,4
C35 0.2430,11 0.2990,11 0.0274,4
C35' 0.2015,8 -0.0211,10 0.0218,4
C36 0.4273,11 0.2756,9 0.0715,4
C36' 0.2918,7 0.0124,8 0.0070,3
C37 0.3585,11 0.1208,12 0.1248,4
C38 0.1264,15 0.0703,12 0.1134,5
C39 0.0594,10 0.1777,11 0.0518,5
C40 0.7166,10 -0.2166,10 0.0584,4
C41 0.6331,9 -0.2053,10 0.0766,4
C41' 0.5817,9 0.0225,8 0.0216,3
C42 0.6526,10 -0.1353,10 0.1003,4
C42' 0.6755,8 -0.0022,9 0.0093,3
C43 0.7561,14 -0.1068,11 0.0985,4
C43' 0.7665,9 0.0320,10 0.0249,4
C44 0.7978,11 -0.1617,10 0.0714,4
C44' 0.7593,9 0.0889,10 0.0518,4
C45 0.7288,12 -0.2861,12 0.0328,4
C45' 0.6619,9 0.1096,9 0.0638,4
C46 0.5352,10 -0.2639,11 0.0725,4
C46' 0.5775,10 0.0745,9 0.0493,3
C47 0.5830,17 -0.1061,14 0.1259,5
C48 0.8188,19 -0.0469,12 0.1195,5
C49 0.9055,11 -0.1589,13 0.0606,6
H12' 0.5676 -0.0263 -0.0555
H13' 0.6232 -0.1769 -0.0798
H14' 0.5952 -0.3334 -0.0553
H15 0.2080 -0.0293 -0.0492
H15' 0.1501 -0.0587 -0.0787
H15'' 0.5030 -0.3424 -0.0095
H15''' 0.2484 0.0053 -0.0807
H16 0.2271 -0.2656 -0.0100
H16'' 0.1382 -0.2899 -0.0320
H16''' 0.4336 -0.1953 0.0108
H16'''' 0.1617 -0.1785 -0.0232
H17 0.3887 -0.4464 -0.0586
H17' 0.2768 -0.4581 -0.0686
H17'' 0.3022 -0.4198 -0.0360
H18 0.4339 -0.4002 -0.1119
H18' 0.5039 -0.3064 -0.1147
H18'' 0.4122 -0.3186 -0.1365
H19 0.4390 -0.1202 -0.1296
H19' 0.3762 -0.0344 -0.1146
H19'' 0.3262 -0.1057 -0.1384
H22' 0.5345 0.2065 0.0110
H23' 0.4679 0.3525 -0.0019
H24' 0.3762 0.3409 -0.0572
H25 0.7530 0.0278 -0.0515
H25' 0.8215 0.0658 -0.0779
H25'' 0.3582 0.1831 -0.0816
H25''' 0.7214 0.0092 -0.0852
H26 0.6624 0.1156 -0.1373
H26' 0.5534 0.1589 -0.1356
H26'' 0.4068 0.0338 -0.0560
H26''' 0.5808 0.0611 -0.1178
H27 0.5025 0.3934 -0.1009
H27' 0.5196 0.3193 -0.1279
H27'' 0.5962 0.4062 -0.1219
H28 0.6004 0.4623 -0.0602
H28' 0.7178 0.4615 -0.0594
H28'' 0.6567 0.4250 -0.0312
H29 0.7524 0.2823 -0.0096
H29' 0.8471 0.2654 -0.0298
H29'' 0.7889 0.1732 -0.0167
H32' 0.4516 -0.0738 0.0585
H33' 0.3011 -1.4262 0.0817
H34' 0.1446 -0.1007 0.0582
H35 0.1972 0.2727 0.0126
H35' 0.3088 0.3033 0.0186
H35'' 0.1379 -0.0058 0.0128
H35''' 0.2215 0.3646 0.0334
H36 0.4792 0.2390 0.0816
H36' 0.4218 0.3413 0.0802
H36'' 0.2881 0.0482 -0.0118
H36''' 0.4434 0.2814 0.0504
H37 0.4004 0.1748 0.1316
H37' 0.3998 0.0646 0.1194
H37'' 0.3132 0.1019 0.1405
H38 0.0696 0.1100 0.1193
H38' 0.1643 0.0532 0.1313
H38'' 0.1037 0.0100 0.1039
H39 0.0121 0.1592 0.0671
H39' 0.0580 0.1289 0.0358
H39'' 0.0420 0.2423 0.0437
H42' 0.6809 -0.0406 -0.0090
H43' 0.8308 0.0153 0.0166
H44' 0.8182 0.1131 0.0619
H45 0.7959 -0.3113 0.0325
H45' 0.7154 -0.2512 0.0142
H45'' 0.6560 0.1480 0.0821
H45''' 0.6825 -0.3408 0.0349
H46 0.5196 -0.2689 0.0514
H46' 0.4821 -0.2301 0.0828
H46'' 0.5130 0.0859 0.0582
H46''' 0.5434 -0.3301 0.0807
H47 0.6157 -0.0593 0.1389
H47' 0.5647 -0.1649 0.1371
H47'' 0.5234 -0.0760 0.1176
H48 0.8683 -0.0102 0.1083
H48' 0.8522 -0.0911 0.1335
H48'' 0.7774 -0.0010 0.1305
H49 0.9302 -0.0916 0.0616
H49' 0.9087 -0.1827 0.0402
H49'' 0.9457 -0.2012 0.0734


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 C10 2.207,13
Ru1 C11 2.189,11
Ru1 C11' 2.347,12
Ru1 C12 2.141,11
Ru1 C12' 2.242,11
Ru1 C13 2.149,14
Ru1 C13' 2.198,11
Ru1 C14 2.200,13
Ru1 C14' 2.199,11
Ru1 C15' 2.233,14
Ru1 C16' 2.205,13
Ru2 C20 2.204,11
Ru2 C21 2.181,15
Ru2 C21' 2.350,12
Ru2 C22 2.150,15
Ru2 C22' 2.216,14
Ru2 C23 2.147,12
Ru2 C23' 2.208,13
Ru2 C24 2.206,12
Ru2 C24' 2.213,11
Ru2 C25' 2.181,11
Ru2 C26' 2.262,12
Ru3 C30 2.215,11
Ru3 C31 2.274,13
Ru3 C31' 2.290,11
Ru3 C32 2.194,15
Ru3 C32' 2.262,11
Ru3 C33 2.152,14
Ru3 C33' 2.194,12
Ru3 C34 2.197,13
Ru3 C34' 2.193,13
Ru3 C35' 2.156,13
Ru3 C36' 2.235,12
Ru4 C40 2.181,12
Ru4 C41 2.244,12
Ru4 C41' 2.293,12
Ru4 C42 2.189,14
Ru4 C42' 2.226,13
Ru4 C43 2.161,16
Ru4 C43' 2.153,14
Ru4 C44 2.173,14
Ru4 C44' 2.181,13
Ru4 C45' 2.213,12
Ru4 C46' 2.226,12
S1 O11 1.429,9
S1 O12 1.429,11
S1 O13 1.465,13
S2 O21 1.451,13
S2 O22 1.479,11
S2 O23 1.430,10
S3 O31 1.405,12
S3 O32 1.436,10
S3 O33 1.421,12
S4 O41 1.456,13
S4 O42 1.407,14
S4 O43 1.429,9
S1 C1S 1.769,16
S2 C2S 1.818,15
S3 C3S 1.806,16
S4 C4S 1.813,16
F11 C1S 1.328,17
F12 C1S 1.365,21
F13 C1S 1.299,19
F21 C2S 1.355,19
F22 C2S 1.257,20
F23 C2S 1.343,17
F31 C3S 1.325,17
F32 C3S 1.383,20
F33 C3S 1.271,19
F41 C4S 1.361,21
F42 C4S 1.344,19
F43 C4S 1.250,21
C1 C11' 1.527,17
C1 C21' 1.523,18
C1 C31' 1.585,16
C1 C41' 1.585,19
C10 C11 1.413,20
C10 C14 1.446,20
C10 C15 1.528,19
C11 C12 1.414,9
C11 C16 1.562,21
C11' C12' 1.431,17
C11' C16' 1.440,16
C12 C13 1.386,21
C12 C17 1.492,21
C12' C13' 1.436,16
C13 C14 1.386,20
C13 C18 1.520,22
C13' C14' 1.401,20
C14 C19 1.488,22
C14' C15' 1.414,22
C15' C16' 1.377,17
C20 C21 1.453,20
C20 C24 1.391,20
C20 C25 1.491,19
C21 C22 1.373,21
C21 C26 1.537,23
C21' C22' 1.422,17
C21' C26' 1.432,19
C22 C23 1.370,21
C22 C27 1.527,24
C22' C23' 1.414,19
C23 C24 1.429,18
C23 C28 1.509,20
C23' C24' 1.375,21
C24 C29 1.545,22
C24' C25' 1.408,18
C25' C26' 1.417,16
C30 C31 1.486,19
C30 C34 1.410,18
C30 C35 1.409,22
C31 C32 1.381,22
C31 C36 1.483,19
C31' C32' 1.421,19
C31' C36' 1.402,16
C32 C33 1.495,20
C32 C37 1.483,23
C32' C33' 1.399,17
C33 C34 1.421,20
C33 C38 1.497,21
C33' C34' 1.378,19
C34 C39 1.479,21
C34' C35' 1.400,21
C35' C36' 1.429,16
C40 C41 1.368,20
C40 C44 1.415,20
C40 C45 1.461,25
C41 C42 1.417,21
C41 C46 1.518,18
C41' C42' 1.391,16
C41' C46' 1.397,18
C42 C43 1.422,21
C42 C47 1.499,23
C42' C43' 1.456,18
C43 C44 1.494,25
C43 C48 1.470,21
C43' C44' 1.403,22
C44 C49 1.500,22
C44' C45' 1.416,18
C45' C46' 1.365,17

####################################################################### 
# 
# 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_compound_2
_audit_block_doi                 10.5517/cc7b6d4
_database_code_depnum_ccdc_archive 'CCDC 218345'
_audit_update_record             
;
2003-08-27 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;

_audit_creation_method           'manually at CCDC'

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Fe(hexamethylbenzene)2 (PF6) thiourea'
_chemical_formula_sum            'Fe1 S1 P2 F12 N2 C26 H40'
_chemical_formula_moiety         ?
_chemical_formula_weight         758.48
_chemical_melting_point          ?

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Immm
_symmetry_Int_Tables_number      ?

_cell_length_a                   11.025(2)
_cell_length_b                   13.680(2)
_cell_length_c                   10.181(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1535.5
_cell_formula_units_Z            2

_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100C
_diffrn_radiation_probe          x-ray

_refine_ls_R_factor_gt           0.079
_refine_special_details          
;
?
;

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Fe1 0.0000 0.0000 0.0000
S1 0.5000 0.2617,8 0.0000
P1 0.5000 0.0000 0.5000
P2 0.5000 0.1863,8 0.0000
F1 0.4486,10 0.0708,9 0.3919,10
F2 0.3812,12 0.0590,10 0.5000
F3 0.3978,26 0.2714,13 0.0000
F4 0.4083,12 0.1112,11 0.0000
N1 0.5000 0.0850,14 0.1113,13
C1 0.1466,6 0.0000 0.1371,8
C2 0.1460,5 0.0878,5 0.0685,7
C11 0.1494,9 0.0000 0.2880,10
C12 0.1459,10 0.1874,8 0.1407,14


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 Fe1 2.135,6
C2 Fe1 2.126,5
N1 P2 1.790,19
F3 P2 1.620,20
F2 F2* 1.614,28
F1 P1 1.572,8
F4 N1 1.560,13
C12 C2 1.549,10
F2 P1 1.538,13
C1 C11 1.537,12
F4 P2 1.441,16
C2 C2* 1.396,14
C1 C2 1.389,8
F1 F2 1.338,13
F3 S1 1.134,27
P2 S1 1.032,11
F1 F1* 1.133,21


#END

####################################################################### 
# 
# 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_compound_1_CCDC1
_audit_block_doi                 10.5517/cc7b6f5
_database_code_depnum_ccdc_archive 'CCDC 218346'
_audit_update_record             
;
2003-08-27 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;

_audit_creation_method           'manually at CCDC'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_sum            'Mn1 P6 O1 N9 C114 H92'
_chemical_formula_moiety         ?
_chemical_formula_weight         1844.84
_chemical_melting_point          ?

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn
_symmetry_Int_Tables_number      60

_cell_length_a                   23.884(1)
_cell_length_b                   20.463(3)
_cell_length_c                   19.429(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9495.7
_cell_formula_units_Z            4

_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       'rectangular block'
_exptl_crystal_colour            'golden yellow'
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      203
_diffrn_radiation_probe          x-ray

_refine_ls_R_factor_gt           0.047
_refine_special_details          
;
?
;

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Mn1 0.00000 0.22892,3 0.25000
P1 0.78540,4 0.06749,4 0.48478,4
P2 0.77829,4 -0.03664,4 0.37934,5
P3 0.53476,3 0.20578,4 0.31441,4
O1 0.4079,5 0.0825,6 0.5607,6
N1 -0.1298,1 0.2268,2 0.2183,2
N2 -0.0185,1 0.1152,1 0.3572,1
N3 -0.0164,1 0.3383,1 0.3635,2
N12 0.7800,1 0.0342,1 0.4121,1
N34 0.5000 0.2288,2 0.2500
C1 -0.0825,1 0.2279,2 0.2294,2
C2 -0.0118,1 0.1575,2 0.3194,2
C3 -0.0109,1 0.2986,2 0.3218,2
C11 0.7171,1 0.0927,2 0.5148,2
C12 0.6697,1 0.0720,2 0.4808,2
C13 0.6171,1 0.0916,2 0.5034,2
C14 0.6123,2 0.1329,2 0.5583,2
C15 0.6592,2 0.1549,2 0.5919,2
C16 0.7119,2 0.1344,2 0.5710,2
C21 0.8176,2 0.0185,2 0.5503,2
C22 0.7872,2 -0.0110,2 0.6021,2
C23 0.8140,2 -0.0536,2 0.6473,2
C24 0.8699,2 -0.0654,2 0.6417,2
C25 0.9009,2 -0.0346,2 0.5915,2
C26 0.8754,2 0.0068,2 0.5456,2
C31 0.8279,1 0.1394,2 0.4765,2
C32 0.8375,1 0.1674,2 0.4125,2
C33 0.8691,2 0.2239,2 0.4071,2
C34 0.8913,2 0.2527,2 0.4649,2
C35 0.8826,1 0.2247,2 0.5284,2
C36 0.8513,1 0.1684,2 0.5345,2
C41 0.8382,1 -0.0481,2 0.3254,2
C42 0.8406,1 -0.1005,2 0.2794,2
C43 0.8846,2 -0.1065,2 0.2347,2
C44 0.9265,1 -0.0609,2 0.2353,2
C45 0.9258,1 -0.0097,2 0.2811,2
C46 0.8816,1 -0.0037,2 0.3261,2
C51 0.7189,1 -0.0432,2 0.3228,2
C52 0.6901,2 -0.1018,2 0.3124,2
C53 0.6477,2 -0.1046,2 0.2646,2
C54 0.6342,2 -0.0509,3 0.2261,2
C55 0.6625,2 0.0073,2 0.2357,2
C56 0.7045,2 0.0112,2 0.2843,2
C61 0.7750,1 -0.1017,2 0.4411,2
C62 0.7258,2 -0.1114,2 0.4778,2
C63 0.7243,2 -0.1563,2 0.5305,2
C64 0.7720,2 -0.1902,2 0.5482,2
C65 0.8204,2 -0.1808,2 0.5126,3
C66 0.8223,2 -0.1366,2 0.4590,2
C71 0.6089,1 0.2069,2 0.2958,2
C72 0.6475,2 0.2057,2 0.3489,2
C73 0.7039,2 0.2096,2 0.3348,2
C74 0.7226,2 0.2140,2 0.2690,3
C75 0.6847,2 0.2164,3 0.2165,2
C76 0.6281,2 0.2123,2 0.2302,2
C81 0.5246,1 0.2626,2 0.3829,2
C82 0.5134,1 0.3271,2 0.3663,2
C83 0.5077,2 0.3736,2 0.4174,2
C84 0.5123,2 0.3560,2 0.4854,2
C85 0.5246,2 0.2924,2 0.5025,2
C86 0.5309,1 0.2458,2 0.4520,2
C91 0.5174,1 0.1255,2 0.3455,2
C92 0.4713,2 0.1156,2 0.3879,2
C93 0.4573,2 0.0537,2 0.4095,2
C94 0.4881,2 0.0011,2 0.3887,2
C95 0.5324,2 0.0097,2 0.3464,3
C96 0.5477,2 0.0720,2 0.3248,2
H12 0.6726 0.0453 0.4404
H13 0.5837 0.0759 0.4817
H14 0.5768 0.1468 0.5734
H15 0.6549 0.1846 0.6290
H16 0.7443 0.1487 0.5959
H22 0.7477 -0.0030 0.6067
H23 0.7940 -0.0749 0.6840
H24 0.8893 -0.0951 0.6729
H25 0.9412 -0.0437 0.5878
H26 0.8969 0.0289 0.5123
H32 0.8220 0.1473 0.3722
H33 0.8742 0.2441 0.3633
H34 0.9146 0.2902 0.4609
H35 0.8968 0.2461 0.5686
H36 0.8462 0.1492 0.5782
H42 0.8104 -0.1308 0.2778
H43 0.8861 -0.1416 0.2039
H44 0.9573 -0.0654 0.2052
H45 0.9552 0.0218 0.2814
H46 0.8803 0.0323 0.3577
H52 0.6998 -0.1399 0.3378
H53 0.6266 -0.1431 0.2594
H54 0.6054 -0.0542 0.1930
H55 0.6520 0.0448 0.2085
H56 0.7227 0.0522 0.2919
H62 0.6929 -0.0873 0.4658
H63 0.6904 -0.1636 0.5550
H64 0.7710 -0.2200 0.5862
H65 0.8537 -0.2051 0.5249
H66 0.8562 -0.1295 0.4350
H72 0.6348 0.2044 0.3955
H73 0.7310 0.2101 0.3722
H74 0.7613 0.2152 0.2595
H75 0.6977 0.2197 0.1702
H76 0.6018 0.2153 0.1929
H82 0.5103 0.3395 0.3195
H83 0.4996 0.4179 0.4053
H84 0.5079 0.3882 0.5207
H85 0.5279 0.2798 0.5497
H86 0.5407 0.2016 0.4635
H92 0.4490 0.1541 0.4026
H93 0.4256 0.0485 0.4403
H94 0.4777 -0.0412 0.4040
H95 0.5554 -0.0268 0.3339
H96 0.5794 0.0783 0.2953

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn1 C1 2.011,3
C41 C42 1.398,4
Mn1 C2 2.008,4
C41 C46 1.379,4
Mn1 C3 2.013,4
C42 C43 1.370,5
P1 N12 1.573,3
C43 C44 1.368,5
P2 N12 1.583,3
C44 C45 1.374,5
P3 N34 1.574,1
C45 C46 1.375,4
P1 C11 1.807,3
C51 C52 1.395,5
P1 C21 1.793,3
C51 C56 1.386,5
P1 C31 1.795,3
C52 C53 1.374,5
P2 C41 1.789,3
C53 C54 1.369,6
P2 C51 1.800,4
C54 C55 1.383,6
P2 C61 1.794,4
C55 C56 1.379,5
P3 C71 1.808,3
C61 C62 1.389,5
P3 C81 1.784,3
C61 C66 1.381,5
P3 C91 1.800,3
C62 C63 1.375,5
N1 C1 1.151,4
C63 C64 1.379,6
N2 C2 1.147,4
C64 C65 1.360,6
N3 C3 1.154,4
C65 C66 1.380,5
C11 C12 1.378,5
C71 C72 1.383,5
C11 C16 1.390,5
C71 C76 1.359,5
C12 C13 1.391,5
C72 C73 1.378,5
C13 C14 1.365,5
C73 C74 1.356,6
C14 C15 1.373,5
C74 C75 1.364,6
C15 C16 1.386,5
C75 C76 1.380,5
C21 C22 1.381,5
C81 C82 1.384,4
C21 C26 1.403,5
C81 C86 1.395,4
C22 C23 1.393,5
C82 C83 1.382,5
C23 C24 1.361,7
C83 C84 1.373,5
C24 C25 1.377,6
C84 C85 1.376,5
C25 C26 1.374,5
C85 C86 1.376,5
C31 C32 1.388,4
C91 C92 1.390,4
C31 C36 1.391,4
C91 C96 1.371,5
C32 C33 1.386,5
C92 C93 1.375,5
C33 C34 1.375,5
C93 C94 1.366,5
C34 C35 1.377,5
C94 C95 1.350,6
C35 C36 1.378,5
C95 C96 1.391,5

####################################################################### 
# 
# 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_johben
_database_code_depnum_ccdc_archive 'CCDC 2176319'
loop_
_audit_author_name
_audit_author_address
'Nathan Schley' 'Vanderbilt University'
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_johben              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: We provide a new model for an old, published dataset. We are limited by the quality and completeness of the original data.
;
_vrf_PLAT183_johben              
;
PROBLEM: Missing _cell_measurement_reflns_used Value ....     Please Do !
RESPONSE: We provide a new model for an old, published dataset. We are limited by the quality and completeness of the original data.
;
_vrf_PLAT184_johben              
;
PROBLEM: Missing _cell_measurement_theta_min Value ......     Please Do !
RESPONSE: We provide a new model for an old, published dataset. We are limited by the quality and completeness of the original data.
;
_vrf_PLAT185_johben              
;
PROBLEM: Missing _cell_measurement_theta_max Value ......     Please Do !
RESPONSE: We provide a new model for an old, published dataset. We are limited by the quality and completeness of the original data.
;
_vrf_THETM01_johben              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: We provide a new model for an old, published dataset. We are limited by the quality and completeness of the original data.
;
# Added during the CSD deposition process: Tuesday 31 May 2022 05:00 PM
# end Validation Reply Form

_audit_creation_date             2021-09-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        {(TMEDA)2Li}{[Ti(N(TMS)2)2]2(μ-PhMe)}
_chemical_formula_moiety         'C31 H80 N4 Si8 Ti2, C12 H32 Li N4'
_chemical_formula_sum            'C43 H112 Li N8 Si8 Ti2'
_chemical_formula_weight         1068.86
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Li Li -0.0003 0.0001 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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      orthorhombic
_space_group_IT_number           23
_space_group_name_H-M_alt        'I 2 2 2'
_space_group_name_Hall           'I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   13.240(5)
_cell_length_b                   22.381(3)
_cell_length_c                   11.5750(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3430.0(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.924
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.8955
_diffrn_reflns_av_unetI/netI     0.2127
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1442
_diffrn_reflns_point_group_measured_fraction_full 0.564
_diffrn_reflns_point_group_measured_fraction_max 0.564
_diffrn_reflns_theta_full        23.543
_diffrn_reflns_theta_max         23.543
_diffrn_reflns_theta_min         1.820
_diffrn_ambient_temperature      295.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          
'Structure factors were obtained by extracting published values from 10.1021/ja00023a080 using the Tabula software package (https://tabula.technology/). The extracted tables were converted into an hklf 3 version hkl file using Microsoft Excel.'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                1071
_reflns_number_total             1435
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'ShelXS-1986 (Sheldrick, 2008)'
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -0.02(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1435
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1193P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1705
_refine_special_details          
'Disorder in a trimethylsilyl group was modeled over two orientations with similarity restraints placed on the atomic thermal parameters and Si-C bond distances. The toluene was disordered over 4 orientations related by symmetry, and was modeled without restraint.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C4 \\sim Si2-C4A \\sim Si2-C6 \\sim Si2-C5 \\sim Si2-C5A \\sim Si2-C6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5A \\sim C6 \\sim C4A \\sim C5 \\sim C6A: within 2.4A with sigma of
0.02 and sigma for terminal atoms of 0.02
4. Others
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
 Fixed Sof: H11(0.75) C12(0.25) H12A(0.25) H12B(0.25) H12C(0.25)
 Fixed X: Ti1(-0.5) C10(-0.5) Li1(-0.5)
 Fixed Y: C10(0) Li1(-0.5)
 Fixed Z: Ti1(-0.5) Li1(-0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
5.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C4A(H4AA,H4AB,H4AC),
 C5(H5A,H5B,H5C), C6A(H6AA,H6AB,H6AC)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C),
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Ti1 Ti -0.5000 -0.08220(7) -0.5000 0.0413(5) Uani 1 2 d S T P C .
Si1 Si -0.5626(2) -0.14255(13) -0.2468(2) 0.0684(8) Uani 1 1 d . . . . .
Si2 Si -0.6834(2) -0.17501(13) -0.4513(2) 0.0746(8) Uani 1 1 d D . . . .
N1 N -0.5823(5) -0.1370(3) -0.3926(5) 0.0485(16) Uani 1 1 d . . . . .
C1 C -0.4378(9) -0.1189(6) -0.1985(10) 0.125(5) Uani 1 1 d . . . . .
H1A H -0.3956 -0.1114 -0.2645 0.187 Uiso 1 1 calc GR . . . .
H1B H -0.4081 -0.1498 -0.1520 0.187 Uiso 1 1 calc GR . . . .
H1C H -0.4438 -0.0830 -0.1536 0.187 Uiso 1 1 calc GR . . . .
C2 C -0.6627(15) -0.1061(7) -0.1622(10) 0.160(7) Uani 1 1 d . . . . .
H2A H -0.6530 -0.0636 -0.1636 0.240 Uiso 1 1 calc GR . . . .
H2B H -0.6601 -0.1201 -0.0838 0.240 Uiso 1 1 calc GR . . . .
H2C H -0.7274 -0.1157 -0.1949 0.240 Uiso 1 1 calc GR . . . .
C3 C -0.5632(11) -0.2231(5) -0.1949(10) 0.122(5) Uani 1 1 d . . . . .
H3A H -0.6313 -0.2379 -0.1940 0.184 Uiso 1 1 calc GR . . . .
H3B H -0.5355 -0.2251 -0.1184 0.184 Uiso 1 1 calc GR . . . .
H3C H -0.5232 -0.2471 -0.2462 0.184 Uiso 1 1 calc GR . . . .
C10 C -0.5000 0.0000 -0.3799(9) 0.068(3) Uani 1 2 d S T P C .
H10 H -0.5000 0.0000 -0.2995 0.081 Uiso 1 2 calc RS T P . .
C11 C -0.4099(7) -0.0059(4) -0.4371(8) 0.073(3) Uani 1 1 d . . . . .
H11 H -0.3512 -0.0168 -0.3984 0.088 Uiso 0.75 1 calc R . . A -1
C4 C -0.6319(19) -0.2394(9) -0.542(2) 0.108(7) Uani 0.55(2) 1 d D U . B 1
H4A H -0.6871 -0.2612 -0.5751 0.162 Uiso 0.55(2) 1 calc R . . B 1
H4B H -0.5896 -0.2239 -0.6019 0.162 Uiso 0.55(2) 1 calc R . . B 1
H4C H -0.5930 -0.2656 -0.4932 0.162 Uiso 0.55(2) 1 calc R . . B 1
C5A C -0.719(2) -0.1630(13) -0.6055(16) 0.128(8) Uani 0.55(2) 1 d D U . B 1
H5AA H -0.7760 -0.1873 -0.6243 0.192 Uiso 0.55(2) 1 calc R . . B 1
H5AB H -0.7352 -0.1217 -0.6173 0.192 Uiso 0.55(2) 1 calc R . . B 1
H5AC H -0.6628 -0.1737 -0.6542 0.192 Uiso 0.55(2) 1 calc R . . B 1
C6 C -0.767(3) -0.2249(13) -0.360(3) 0.144(9) Uani 0.55(2) 1 d D U . B 1
H6A H -0.8186 -0.2420 -0.4082 0.216 Uiso 0.55(2) 1 calc R . . B 1
H6B H -0.7269 -0.2562 -0.3270 0.216 Uiso 0.55(2) 1 calc R . . B 1
H6C H -0.7974 -0.2017 -0.3001 0.216 Uiso 0.55(2) 1 calc R . . B 1
C4A C -0.660(3) -0.2579(7) -0.458(4) 0.137(8) Uani 0.45(2) 1 d D U . B 2
H4AA H -0.7172 -0.2776 -0.4905 0.206 Uiso 0.45(2) 1 calc R . . B 2
H4AB H -0.6011 -0.2656 -0.5043 0.206 Uiso 0.45(2) 1 calc R . . B 2
H4AC H -0.6482 -0.2728 -0.3808 0.206 Uiso 0.45(2) 1 calc R . . B 2
C5 C -0.7651(18) -0.1303(11) -0.552(2) 0.096(8) Uani 0.45(2) 1 d D U . B 2
H5A H -0.8190 -0.1550 -0.5798 0.144 Uiso 0.45(2) 1 calc R . . B 2
H5B H -0.7928 -0.0968 -0.5108 0.144 Uiso 0.45(2) 1 calc R . . B 2
H5C H -0.7253 -0.1164 -0.6154 0.144 Uiso 0.45(2) 1 calc R . . B 2
C6A C -0.800(2) -0.1896(17) -0.360(3) 0.128(10) Uani 0.45(2) 1 d D U . B 2
H6AA H -0.8486 -0.2111 -0.4055 0.191 Uiso 0.45(2) 1 calc R . . B 2
H6AB H -0.7814 -0.2129 -0.2940 0.191 Uiso 0.45(2) 1 calc R . . B 2
H6AC H -0.8281 -0.1523 -0.3358 0.191 Uiso 0.45(2) 1 calc R . . B 2
C12 C -0.289(2) 0.002(2) -0.399(4) 0.088(14) Uani 0.25 1 d . . . C -2
H12A H -0.2463 -0.0151 -0.4578 0.132 Uiso 0.25 1 calc GR . . C -2
H12B H -0.2771 -0.0184 -0.3271 0.132 Uiso 0.25 1 calc GR . . C -2
H12C H -0.2732 0.0435 -0.3903 0.132 Uiso 0.25 1 calc GR . . C -2
N2 N -0.5691(7) -0.4471(4) -0.3664(8) 0.089(3) Uani 1 1 d . . . . .
C7 C -0.5178(18) -0.3866(6) -0.3509(17) 0.183(8) Uani 1 1 d . . . . .
H7A H -0.4475 -0.3925 -0.3341 0.274 Uiso 1 1 calc GR . . . .
H7B H -0.5491 -0.3655 -0.2882 0.274 Uiso 1 1 calc GR . . . .
H7C H -0.5244 -0.3637 -0.4207 0.274 Uiso 1 1 calc GR . . . .
C8 C -0.6700(12) -0.4266(9) -0.3822(14) 0.194(10) Uani 1 1 d . . . . .
H8A H -0.6701 -0.3926 -0.4326 0.291 Uiso 1 1 calc GR . . . .
H8B H -0.6982 -0.4156 -0.3088 0.291 Uiso 1 1 calc GR . . . .
H8C H -0.7099 -0.4580 -0.4158 0.291 Uiso 1 1 calc GR . . . .
C9 C -0.5517(10) -0.4840(6) -0.2685(11) 0.127(5) Uani 1 1 d . . . . .
H9A H -0.6046 -0.5139 -0.2647 0.152 Uiso 1 1 calc R . . . .
H9B H -0.5565 -0.4596 -0.1994 0.152 Uiso 1 1 calc R . . . .
Li1 Li -0.5000 -0.5000 -0.5000 0.066(7) Uani 1 4 d S T P . .


_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
Ti1 N1 2.058(6) . ?
Ti1 N1 2.058(6) 4_454 ?
Ti1 C10 2.306(6) . ?
Ti1 C11 2.207(9) . ?
Si1 N1 1.712(6) . ?
Si1 C1 1.824(11) . ?
Si1 C2 1.839(15) . ?
Si1 C3 1.901(10) . ?
Si2 N1 1.725(7) . ?
Si2 C4 1.906(14) . ?
Si2 C5A 1.864(15) . ?
Si2 C6 1.890(15) . ?
Si2 C4A 1.883(16) . ?
Si2 C5 1.875(14) . ?
Si2 C6A 1.894(15) . ?
C10 C11 1.370(10) . ?
C10 C11 1.370(10) 2_455 ?
C11 C11 1.480(19) 3_554 ?
C11 C12 1.67(3) . ?
N2 C7 1.525(16) . ?
N2 C8 1.424(17) . ?
N2 C9 1.421(16) . ?
N2 Li1 2.153(8) . ?
C9 C9 1.54(2) 2_445 ?
C9 Li1 2.789(12) . ?
Li1 N2 2.153(8) 2_445 ?
Li1 N2 2.153(8) 3_544 ?
Li1 N2 2.153(8) 4_454 ?
Li1 C9 2.789(13) 3_544 ?
Li1 C9 2.789(13) 4_454 ?
Li1 C9 2.789(13) 2_445 ?

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
N1 Ti1 N1 106.9(3) . 4_454 ?
N1 Ti1 C10 147.08(18) 4_454 . ?
N1 Ti1 C10 96.4(2) . . ?
N1 Ti1 C11 123.2(3) . . ?
N1 Ti1 C11 112.0(3) 4_454 . ?
C11 Ti1 C10 35.3(3) . . ?
N1 Si1 C1 114.8(4) . . ?
N1 Si1 C2 112.5(6) . . ?
N1 Si1 C3 112.3(5) . . ?
C1 Si1 C2 111.2(7) . . ?
C1 Si1 C3 100.5(6) . . ?
C2 Si1 C3 104.4(7) . . ?
N1 Si2 C4 108.2(8) . . ?
N1 Si2 C5A 120.0(9) . . ?
N1 Si2 C6 121.7(13) . . ?
N1 Si2 C4A 111.8(11) . . ?
N1 Si2 C5 115.3(8) . . ?
N1 Si2 C6A 119.8(13) . . ?
C5A Si2 C4 71.0(15) . . ?
C5A Si2 C6 118.1(15) . . ?
C6 Si2 C4 93.9(12) . . ?
C4A Si2 C6A 89.3(16) . . ?
C5 Si2 C4A 126.8(15) . . ?
C5 Si2 C6A 88.1(17) . . ?
Si1 N1 Ti1 123.9(4) . . ?
Si1 N1 Si2 118.0(4) . . ?
Si2 N1 Ti1 117.8(3) . . ?
C11 C10 Ti1 77.6(5) 2_455 . ?
C11 C10 Ti1 68.4(4) . . ?
C11 C10 C11 122.2(10) 2_455 . ?
C10 C11 Ti1 76.3(5) . . ?
C10 C11 C11 117.3(5) . 3_554 ?
C10 C11 C12 134.2(17) . . ?
C11 C11 Ti1 79.2(6) 3_554 . ?
C11 C11 C12 103.9(18) 3_554 . ?
C12 C11 Ti1 133.3(15) . . ?
C7 N2 Li1 112.5(10) . . ?
C8 N2 C7 98.5(13) . . ?
C8 N2 Li1 118.9(9) . . ?
C9 N2 C7 110.5(12) . . ?
C9 N2 C8 116.2(12) . . ?
C9 N2 Li1 100.6(7) . . ?
N2 C9 C9 114.4(9) . 2_445 ?
N2 C9 Li1 49.3(5) . . ?
C9 C9 Li1 73.9(3) 2_445 . ?
N2 Li1 N2 88.1(5) 2_445 . ?
N2 Li1 N2 129.7(5) 2_445 4_454 ?
N2 Li1 N2 129.7(5) 3_544 . ?
N2 Li1 N2 88.1(5) 3_544 4_454 ?
N2 Li1 N2 113.2(5) 3_544 2_445 ?
N2 Li1 N2 113.2(5) 4_454 . ?
N2 Li1 C9 136.4(4) . 4_454 ?
N2 Li1 C9 131.1(4) 2_445 4_454 ?
N2 Li1 C9 59.0(4) . 2_445 ?
N2 Li1 C9 59.0(4) 2_445 . ?
N2 Li1 C9 131.1(4) 4_454 2_445 ?
N2 Li1 C9 30.1(4) . . ?
N2 Li1 C9 59.0(4) 3_544 4_454 ?
N2 Li1 C9 131.1(4) . 3_544 ?
N2 Li1 C9 30.1(4) 4_454 4_454 ?
N2 Li1 C9 136.4(4) 3_544 2_445 ?
N2 Li1 C9 131.1(4) 3_544 . ?
N2 Li1 C9 30.1(4) 3_544 3_544 ?
N2 Li1 C9 136.4(4) 4_454 . ?
N2 Li1 C9 136.4(4) 2_445 3_544 ?
N2 Li1 C9 59.0(4) 4_454 3_544 ?
N2 Li1 C9 30.1(4) 2_445 2_445 ?
C9 Li1 C9 165.2(6) 3_544 2_445 ?
C9 Li1 C9 32.1(5) 2_445 . ?
C9 Li1 C9 151.6(5) 3_544 . ?
C9 Li1 C9 32.1(5) 3_544 4_454 ?
C9 Li1 C9 165.2(6) 4_454 . ?
C9 Li1 C9 151.6(5) 2_445 4_454 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_21072_abs
_database_code_depnum_ccdc_archive 'CCDC 2183462'
loop_
_audit_author_name
_audit_author_address
'Daniel Huh'
;University of Minnesota
United States of America
;
_audit_update_record             
;
2022-07-02 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-08
_audit_creation_method           
; 
Olex2 1.3 
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) 
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H72 K2 N6 Si8 Ti2'
_chemical_formula_sum            'C24 H72 K2 N6 Si8 Ti2'
_chemical_formula_weight         843.59
_chemical_melting_point          ?
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'
K K 0.2009 0.2494 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.367(4)
_cell_length_b                   14.742(5)
_cell_length_c                   16.488(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.117(6)
_cell_angle_gamma                90
_cell_volume                     2276.7(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1862
_cell_measurement_temperature    396.15
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.824
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0556 before and 0.0486 after correction. 
The Ratio of minimum to maximum transmission is 0.8646. 
The λ/2 correction factor is 0.00150. 
;
_exptl_absorpt_special_details   
; 
 Reflections not merged 
   11423 Corrected reflections written to file 21072.hkl 
 Estimated minimum and maximum transmission:  0.6443  0.7452 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.075
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11137
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.483
_diffrn_reflns_theta_min         1.853
_diffrn_ambient_temperature      396.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.0
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3064
_reflns_number_total             4168
_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       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0439
_refine_ls_restrained_S_all      1.006
_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)+(0.0541P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          ?
_olex2_refinement_description    
; 
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
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
Ti1 Ti 1.02973(6) 0.43120(4) 0.45013(3) 0.01467(17) Uani 1 1 d . . . . .
K1 K 1.18524(9) 0.63517(5) 0.38869(5) 0.0302(2) Uani 1 1 d . . . . .
Si3 Si 1.24710(10) 0.42519(7) 0.29579(6) 0.0236(2) Uani 1 1 d . . . . .
Si4 Si 0.95349(10) 0.49014(7) 0.25929(6) 0.0212(2) Uani 1 1 d . . . . .
Si1 Si 1.11260(10) 0.76867(6) 0.56240(6) 0.0226(2) Uani 1 1 d . . . . .
Si2 Si 0.83969(10) 0.75968(6) 0.46825(6) 0.0204(2) Uani 1 1 d . . . . .
N3 N 1.0797(3) 0.45524(18) 0.32963(15) 0.0183(6) Uani 1 1 d . . . . .
N1 N 1.1302(3) 0.50992(18) 0.51500(16) 0.0188(6) Uani 1 1 d . . . . .
N2 N 0.9833(3) 0.70439(18) 0.51329(16) 0.0179(6) Uani 1 1 d . . . . .
C9 C 1.2520(5) 0.3146(3) 0.2382(3) 0.0386(11) Uani 1 1 d . . . . .
H9A H 1.222(5) 0.272(3) 0.268(3) 0.056(15) Uiso 1 1 d . . . . .
H9B H 1.348(6) 0.296(3) 0.237(3) 0.081(17) Uiso 1 1 d . . . . .
H9C H 1.206(5) 0.318(3) 0.183(3) 0.072(16) Uiso 1 1 d . . . . .
C7 C 1.3757(5) 0.4142(4) 0.3810(3) 0.0428(12) Uani 1 1 d . . . . .
H7A H 1.389(4) 0.470(3) 0.416(2) 0.038(12) Uiso 1 1 d . . . . .
H7B H 1.471(5) 0.409(3) 0.355(2) 0.049(12) Uiso 1 1 d . . . . .
H7C H 1.357(5) 0.364(3) 0.413(3) 0.060(15) Uiso 1 1 d . . . . .
C8 C 1.3286(5) 0.5125(3) 0.2270(3) 0.0312(9) Uani 1 1 d . . . . .
H8A H 1.272(4) 0.525(3) 0.182(3) 0.047(13) Uiso 1 1 d . . . . .
H8B H 1.416(5) 0.487(3) 0.209(2) 0.054(13) Uiso 1 1 d . . . . .
H8C H 1.349(4) 0.566(3) 0.252(2) 0.024(10) Uiso 1 1 d . . . . .
C12 C 0.7668(4) 0.4666(3) 0.2912(2) 0.0256(8) Uani 1 1 d . . . . .
H12A H 0.747(3) 0.406(2) 0.2882(19) 0.020(9) Uiso 1 1 d . . . . .
H12B H 0.699(4) 0.495(3) 0.256(2) 0.044(12) Uiso 1 1 d . . . . .
H12C H 0.748(4) 0.493(2) 0.345(2) 0.034(10) Uiso 1 1 d . . . . .
C10 C 0.9752(5) 0.4367(4) 0.1570(3) 0.0356(10) Uani 1 1 d . . . . .
H10A H 1.064(4) 0.446(2) 0.132(2) 0.035(11) Uiso 1 1 d . . . . .
H10B H 0.916(5) 0.460(3) 0.126(3) 0.046(14) Uiso 1 1 d . . . . .
H10C H 0.970(4) 0.368(3) 0.158(2) 0.041(12) Uiso 1 1 d . . . . .
C11 C 0.9662(5) 0.6151(3) 0.2401(3) 0.0349(10) Uani 1 1 d . . . . .
H11A H 0.939(4) 0.655(2) 0.290(2) 0.030(10) Uiso 1 1 d . . . . .
H11B H 0.900(5) 0.630(3) 0.202(3) 0.079(17) Uiso 1 1 d . . . . .
H11C H 1.054(5) 0.634(3) 0.223(2) 0.042(12) Uiso 1 1 d . . . . .
C1 C 1.0798(5) 0.7759(3) 0.6735(3) 0.0329(10) Uani 1 1 d . . . . .
H1A H 1.005(5) 0.813(3) 0.681(3) 0.069(16) Uiso 1 1 d . . . . .
H1B H 1.156(5) 0.801(3) 0.699(3) 0.071(16) Uiso 1 1 d . . . . .
H1C H 1.072(4) 0.711(3) 0.699(2) 0.052(13) Uiso 1 1 d . . . . .
C2 C 1.1312(5) 0.8893(3) 0.5280(3) 0.0410(11) Uani 1 1 d . . . . .
H2A H 1.153(4) 0.896(3) 0.475(3) 0.040(13) Uiso 1 1 d . . . . .
H2B H 1.207(4) 0.917(3) 0.565(2) 0.042(11) Uiso 1 1 d . . . . .
H2C H 1.048(5) 0.920(3) 0.542(2) 0.051(14) Uiso 1 1 d . . . . .
C3 C 1.2969(4) 0.7212(3) 0.5464(3) 0.0309(9) Uani 1 1 d . . . . .
H3A H 1.296(4) 0.661(2) 0.549(2) 0.021(10) Uiso 1 1 d . . . . .
H3B H 1.362(4) 0.746(3) 0.589(3) 0.050(12) Uiso 1 1 d . . . . .
H3C H 1.345(4) 0.741(3) 0.491(3) 0.048(12) Uiso 1 1 d . . . . .
C5 C 0.8960(5) 0.8358(3) 0.3837(3) 0.0318(10) Uani 1 1 d . . . . .
H5A H 0.931(5) 0.886(3) 0.400(3) 0.062(16) Uiso 1 1 d . . . . .
H5B H 0.820(6) 0.864(4) 0.363(3) 0.087(19) Uiso 1 1 d . . . . .
H5C H 0.916(5) 0.810(3) 0.343(3) 0.067(18) Uiso 1 1 d . . . . .
C4 C 0.7403(5) 0.8328(3) 0.5421(3) 0.0315(9) Uani 1 1 d . . . . .
H4A H 0.701(4) 0.803(3) 0.588(3) 0.051(13) Uiso 1 1 d . . . . .
H4B H 0.666(5) 0.860(3) 0.519(2) 0.048(13) Uiso 1 1 d . . . . .
H4C H 0.797(5) 0.882(3) 0.557(3) 0.065(16) Uiso 1 1 d . . . . .
C6 C 0.7074(4) 0.6810(3) 0.4207(3) 0.0286(9) Uani 1 1 d . . . . .
H6A H 0.735(7) 0.656(4) 0.367(4) 0.12(2) Uiso 1 1 d . . . . .
H6B H 0.622(6) 0.705(4) 0.411(4) 0.10(2) Uiso 1 1 d . . . . .
H6C H 0.674(5) 0.637(3) 0.450(3) 0.071(17) Uiso 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
Ti1 N3 2.073(3) . ?
Ti1 N1 1.825(3) 3_766 ?
Ti1 N1 1.836(3) . ?
Ti1 N2 2.091(3) 3_766 ?
K1 N3 2.993(3) . ?
K1 N1 2.831(3) . ?
K1 N2 2.976(3) . ?
K1 H8C 2.91(3) . ?
K1 H11A 2.83(3) . ?
K1 H11C 3.00(4) . ?
K1 H3A 2.86(3) . ?
K1 H3C 2.74(4) . ?
Si3 N3 1.723(3) . ?
Si3 C9 1.887(4) . ?
Si3 C7 1.856(5) . ?
Si3 C8 1.878(4) . ?
Si4 N3 1.732(3) . ?
Si4 C12 1.859(4) . ?
Si4 C10 1.873(4) . ?
Si4 C11 1.874(4) . ?
Si1 N2 1.737(3) . ?
Si1 C1 1.862(4) . ?
Si1 C2 1.875(4) . ?
Si1 C3 1.882(4) . ?
Si2 N2 1.738(3) . ?
Si2 C5 1.866(4) . ?
Si2 C4 1.875(4) . ?
Si2 C6 1.869(4) . ?
N1 Ti1 1.825(3) 3_766 ?
N2 Ti1 2.091(3) 3_766 ?
C9 K1 3.424(4) 2_745 ?
C9 H9A 0.85(5) . ?
C9 H9B 0.94(5) . ?
C9 H9C 1.01(5) . ?
C7 H7A 1.01(4) . ?
C7 H7B 0.99(4) . ?
C7 H7C 0.93(5) . ?
C8 H8A 0.93(4) . ?
C8 H8B 0.94(4) . ?
C8 H8C 0.91(4) . ?
C12 H12A 0.92(4) . ?
C12 H12B 0.95(4) . ?
C12 H12C 0.98(4) . ?
C10 H10A 0.94(4) . ?
C10 H10B 0.83(4) . ?
C10 H10C 1.01(4) . ?
C11 H11A 1.05(4) . ?
C11 H11B 0.90(5) . ?
C11 H11C 0.92(4) . ?
C1 H1A 0.90(5) . ?
C1 H1B 0.91(5) . ?
C1 H1C 1.05(4) . ?
C2 H2A 0.91(4) . ?
C2 H2B 1.02(4) . ?
C2 H2C 0.94(4) . ?
C3 H3A 0.89(3) . ?
C3 H3B 1.00(4) . ?
C3 H3C 1.06(4) . ?
C5 H5A 0.85(5) . ?
C5 H5B 0.89(6) . ?
C5 H5C 0.80(5) . ?
C4 H4A 0.95(4) . ?
C4 H4B 0.89(4) . ?
C4 H4C 0.94(5) . ?
C6 H6A 1.00(6) . ?
C6 H6B 0.88(6) . ?
C6 H6C 0.87(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
N3 Ti1 N2 116.95(11) . 3_766 ?
N1 Ti1 N3 114.06(11) 3_766 . ?
N1 Ti1 N3 109.50(11) . . ?
N1 Ti1 N1 86.33(12) 3_766 . ?
N1 Ti1 N2 117.77(11) . 3_766 ?
N1 Ti1 N2 108.38(11) 3_766 3_766 ?
N3 K1 H8C 67.2(7) . . ?
N3 K1 H11A 68.8(7) . . ?
N3 K1 H11C 64.2(8) . . ?
N3 K1 H3A 122.5(7) . . ?
N3 K1 H3C 152.0(8) . . ?
N1 K1 N3 66.48(8) . . ?
N1 K1 N2 66.35(8) . . ?
N1 K1 H8C 115.9(7) . . ?
N1 K1 H11A 109.8(7) . . ?
N1 K1 H11C 126.4(8) . . ?
N1 K1 H3A 58.3(7) . . ?
N1 K1 H3C 90.9(9) . . ?
N2 K1 N3 108.57(8) . . ?
N2 K1 H8C 172.2(7) . . ?
N2 K1 H11A 80.8(8) . . ?
N2 K1 H11C 111.8(8) . . ?
N2 K1 H3A 63.0(7) . . ?
N2 K1 H3C 74.2(9) . . ?
H8C K1 H11A 91.5(10) . . ?
H8C K1 H11C 60.6(10) . . ?
H8C K1 H3A 124.7(10) . . ?
H8C K1 H3C 112.7(11) . . ?
H11A K1 H11C 31.4(10) . . ?
H11A K1 H3A 143.8(10) . . ?
H11A K1 H3C 137.5(11) . . ?
H11C K1 H3A 172.1(10) . . ?
H11C K1 H3C 142.0(12) . . ?
H3A K1 H3C 32.6(10) . . ?
N3 Si3 K1 58.65(9) . . ?
N3 Si3 C9 114.10(18) . . ?
N3 Si3 C7 111.52(17) . . ?
N3 Si3 C8 112.99(17) . . ?
C9 Si3 K1 171.01(17) . . ?
C7 Si3 K1 81.59(18) . . ?
C7 Si3 C9 106.8(2) . . ?
C7 Si3 C8 104.6(2) . . ?
C8 Si3 K1 74.10(15) . . ?
C8 Si3 C9 106.1(2) . . ?
N3 Si4 K1 52.39(9) . . ?
N3 Si4 C12 113.32(16) . . ?
N3 Si4 C10 113.74(18) . . ?
N3 Si4 C11 111.18(17) . . ?
C12 Si4 K1 119.55(13) . . ?
C12 Si4 C10 106.3(2) . . ?
C12 Si4 C11 106.9(2) . . ?
C10 Si4 K1 133.99(15) . . ?
C10 Si4 C11 104.8(2) . . ?
C11 Si4 K1 59.58(15) . . ?
N2 Si1 K1 56.97(9) . . ?
N2 Si1 C1 111.96(17) . . ?
N2 Si1 C2 116.21(18) . . ?
N2 Si1 C3 111.76(16) . . ?
C1 Si1 K1 149.33(15) . . ?
C1 Si1 C2 105.0(2) . . ?
C1 Si1 C3 108.2(2) . . ?
C2 Si1 K1 105.33(19) . . ?
C2 Si1 C3 103.0(2) . . ?
C3 Si1 K1 60.15(13) . . ?
N2 Si2 C5 112.44(18) . . ?
N2 Si2 C4 112.13(18) . . ?
N2 Si2 C6 113.57(17) . . ?
C5 Si2 C4 106.3(2) . . ?
C5 Si2 C6 104.3(2) . . ?
C6 Si2 C4 107.5(2) . . ?
Ti1 N3 K1 85.11(9) . . ?
Si3 N3 Ti1 118.28(14) . . ?
Si3 N3 K1 91.89(11) . . ?
Si3 N3 Si4 118.66(15) . . ?
Si4 N3 Ti1 122.51(14) . . ?
Si4 N3 K1 100.32(11) . . ?
Ti1 N1 Ti1 93.67(12) 3_766 . ?
Ti1 N1 K1 94.44(10) . . ?
Ti1 N1 K1 94.15(10) 3_766 . ?
Ti1 N2 K1 84.77(9) 3_766 . ?
Si1 N2 Ti1 115.34(13) . 3_766 ?
Si1 N2 K1 93.74(11) . . ?
Si1 N2 Si2 118.79(15) . . ?
Si2 N2 Ti1 121.74(14) . 3_766 ?
Si2 N2 K1 110.99(12) . . ?
K1 C9 H9A 81(3) 2_745 . ?
K1 C9 H9B 66(3) 2_745 . ?
K1 C9 H9C 64(3) 2_745 . ?
Si3 C9 K1 168.3(2) . 2_745 ?
Si3 C9 H9A 110(3) . . ?
Si3 C9 H9B 107(3) . . ?
Si3 C9 H9C 114(3) . . ?
H9A C9 H9B 97(4) . . ?
H9A C9 H9C 115(4) . . ?
H9B C9 H9C 113(4) . . ?
Si3 C7 H7A 116(2) . . ?
Si3 C7 H7B 106(2) . . ?
Si3 C7 H7C 112(3) . . ?
H7A C7 H7B 102(3) . . ?
H7A C7 H7C 110(3) . . ?
H7B C7 H7C 110(4) . . ?
K1 C8 H8A 107(2) . . ?
K1 C8 H8B 141(3) . . ?
K1 C8 H8C 44(2) . . ?
Si3 C8 K1 74.74(14) . . ?
Si3 C8 H8A 113(2) . . ?
Si3 C8 H8B 105(3) . . ?
Si3 C8 H8C 114(2) . . ?
H8A C8 H8B 109(3) . . ?
H8A C8 H8C 108(3) . . ?
H8B C8 H8C 108(3) . . ?
Si4 C12 H12A 111(2) . . ?
Si4 C12 H12B 112(2) . . ?
Si4 C12 H12C 111(2) . . ?
H12A C12 H12B 105(3) . . ?
H12A C12 H12C 114(3) . . ?
H12B C12 H12C 104(3) . . ?
Si4 C10 H10A 116(2) . . ?
Si4 C10 H10B 108(3) . . ?
Si4 C10 H10C 114(2) . . ?
H10A C10 H10B 105(4) . . ?
H10A C10 H10C 101(3) . . ?
H10B C10 H10C 113(4) . . ?
K1 C11 H11A 60.2(19) . . ?
K1 C11 H11B 160(3) . . ?
K1 C11 H11C 69(2) . . ?
Si4 C11 K1 90.15(16) . . ?
Si4 C11 H11A 113.8(19) . . ?
Si4 C11 H11B 108(3) . . ?
Si4 C11 H11C 114(2) . . ?
H11A C11 H11B 104(4) . . ?
H11A C11 H11C 107(3) . . ?
H11B C11 H11C 109(4) . . ?
Si1 C1 H1A 108(3) . . ?
Si1 C1 H1B 111(3) . . ?
Si1 C1 H1C 111(2) . . ?
H1A C1 H1B 108(4) . . ?
H1A C1 H1C 116(4) . . ?
H1B C1 H1C 104(4) . . ?
Si1 C2 H2A 115(3) . . ?
Si1 C2 H2B 105(2) . . ?
Si1 C2 H2C 108(3) . . ?
H2A C2 H2B 112(3) . . ?
H2A C2 H2C 112(4) . . ?
H2B C2 H2C 104(3) . . ?
K1 C3 H3A 68(2) . . ?
K1 C3 H3B 163(2) . . ?
K1 C3 H3C 62(2) . . ?
Si1 C3 K1 87.79(15) . . ?
Si1 C3 H3A 111(2) . . ?
Si1 C3 H3B 109(2) . . ?
Si1 C3 H3C 114(2) . . ?
H3A C3 H3B 110(3) . . ?
H3A C3 H3C 108(3) . . ?
H3B C3 H3C 105(3) . . ?
Si2 C5 H5A 114(3) . . ?
Si2 C5 H5B 110(4) . . ?
Si2 C5 H5C 115(4) . . ?
H5A C5 H5B 91(4) . . ?
H5A C5 H5C 125(5) . . ?
H5B C5 H5C 95(4) . . ?
Si2 C4 H4A 116(3) . . ?
Si2 C4 H4B 112(3) . . ?
Si2 C4 H4C 110(3) . . ?
H4A C4 H4B 104(4) . . ?
H4A C4 H4C 112(4) . . ?
H4B C4 H4C 102(4) . . ?
Si2 C6 H6A 116(4) . . ?
Si2 C6 H6B 115(4) . . ?
Si2 C6 H6C 118(3) . . ?
H6A C6 H6B 103(5) . . ?
H6A C6 H6C 108(5) . . ?
H6B C6 H6C 94(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
K1 Si3 N3 Ti1 -85.46(14) . . . . ?
K1 Si3 N3 Si4 102.84(17) . . . . ?
K1 Si4 N3 Ti1 90.76(16) . . . . ?
K1 Si4 N3 Si3 -97.91(17) . . . . ?
K1 Si1 N2 Ti1 85.98(13) . . . 3_766 ?
K1 Si1 N2 Si2 -116.46(18) . . . . ?
N3 Ti1 N1 Ti1 114.25(11) . . . 3_766 ?
N3 Ti1 N1 K1 19.79(12) . . . . ?
N3 Si3 C9 K1 146.3(12) . . . 2_745 ?
N3 Si3 C8 K1 44.90(14) . . . . ?
N3 Si4 C11 K1 -9.41(18) . . . . ?
N1 Ti1 N1 Ti1 0.0 3_766 . . 3_766 ?
N1 Ti1 N1 K1 -94.46(11) 3_766 . . . ?
N2 Ti1 N1 Ti1 -108.87(12) 3_766 . . 3_766 ?
N2 Ti1 N1 K1 156.68(9) 3_766 . . . ?
N2 Si1 C3 K1 25.07(17) . . . . ?
C9 Si3 N3 Ti1 100.6(2) . . . . ?
C9 Si3 N3 K1 -173.98(18) . . . . ?
C9 Si3 N3 Si4 -71.1(2) . . . . ?
C9 Si3 C8 K1 170.65(17) . . . . ?
C7 Si3 N3 Ti1 -20.6(3) . . . . ?
C7 Si3 N3 K1 64.9(2) . . . . ?
C7 Si3 N3 Si4 167.7(2) . . . . ?
C7 Si3 C9 K1 -90.0(13) . . . 2_745 ?
C7 Si3 C8 K1 -76.61(18) . . . . ?
C8 Si3 N3 Ti1 -138.1(2) . . . . ?
C8 Si3 N3 K1 -52.64(19) . . . . ?
C8 Si3 N3 Si4 50.2(2) . . . . ?
C8 Si3 C9 K1 21.2(13) . . . 2_745 ?
C12 Si4 N3 Ti1 -19.5(2) . . . . ?
C12 Si4 N3 K1 -110.24(16) . . . . ?
C12 Si4 N3 Si3 151.85(19) . . . . ?
C12 Si4 C11 K1 114.77(16) . . . . ?
C10 Si4 N3 Ti1 -141.0(2) . . . . ?
C10 Si4 N3 K1 128.23(18) . . . . ?
C10 Si4 N3 Si3 30.3(3) . . . . ?
C10 Si4 C11 K1 -132.69(17) . . . . ?
C11 Si4 N3 Ti1 101.0(2) . . . . ?
C11 Si4 N3 K1 10.25(19) . . . . ?
C11 Si4 N3 Si3 -87.7(2) . . . . ?
C1 Si1 N2 Ti1 -61.6(2) . . . 3_766 ?
C1 Si1 N2 K1 -147.57(17) . . . . ?
C1 Si1 N2 Si2 96.0(2) . . . . ?
C1 Si1 C3 K1 148.78(16) . . . . ?
C2 Si1 N2 Ti1 177.8(2) . . . 3_766 ?
C2 Si1 N2 K1 91.8(2) . . . . ?
C2 Si1 N2 Si2 -24.7(3) . . . . ?
C2 Si1 C3 K1 -100.4(2) . . . . ?
C3 Si1 N2 Ti1 60.0(2) . . . 3_766 ?
C3 Si1 N2 K1 -26.00(19) . . . . ?
C3 Si1 N2 Si2 -142.5(2) . . . . ?
C5 Si2 N2 Ti1 -140.4(2) . . . 3_766 ?
C5 Si2 N2 K1 -43.4(2) . . . . ?
C5 Si2 N2 Si1 63.5(2) . . . . ?
C4 Si2 N2 Ti1 99.8(2) . . . 3_766 ?
C4 Si2 N2 K1 -163.12(18) . . . . ?
C4 Si2 N2 Si1 -56.2(2) . . . . ?
C6 Si2 N2 Ti1 -22.2(2) . . . 3_766 ?
C6 Si2 N2 K1 74.82(19) . . . . ?
C6 Si2 N2 Si1 -178.29(19) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_123vgya
_database_code_depnum_ccdc_archive 'CCDC 2183463'
loop_
_audit_author_name
_audit_author_address
'Daniel Huh'
;University of Minnesota
United States of America
;
_audit_update_record             
;
2022-07-02 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H109 Li N8 Si8 Ti2'
_chemical_formula_weight         1065.84

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'
Li Li 0.0008 0.0003 '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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_H-M_alt        'I 2 2 2'
_space_group_name_Hall           'I 2 2'

_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'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'

_cell_length_a                   11.4958(13)
_cell_length_b                   13.0602(15)
_cell_length_c                   22.084(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3315.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    126(2)
_cell_measurement_reflns_used    2915
_cell_measurement_theta_min      3.93
_cell_measurement_theta_max      74.17

_exptl_crystal_description       rectangular
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.673
_shelx_estimated_absorpt_T_min   0.710
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      126(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36985
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.932
_diffrn_reflns_theta_max         74.914
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3408
_reflns_number_gt                2787
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.998

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0660P)²+2.7723P] 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_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.042(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3408
_refine_ls_number_parameters     189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_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
Ti1 Ti 0.5000 0.5000 0.58272(6) 0.0343(3) Uani 1 2 d S T P B .
Si2 Si 0.54576(13) 0.68555(10) 0.67678(9) 0.0458(4) Uani 1 1 d . . . . .
Si1 Si 0.75483(12) 0.56527(11) 0.64260(9) 0.0475(4) Uani 1 1 d . . . . .
N1 N 0.6076(3) 0.5849(3) 0.6382(2) 0.0384(10) Uani 1 1 d . . . . .
N2 N 0.6344(4) 0.5667(3) 0.9468(3) 0.0485(12) Uani 1 1 d . . . . .
C1 C 0.6220(5) 0.5000 0.5000 0.054(2) Uani 1 2 d S T P B .
H1 H 0.7046 0.5000 0.5000 0.065 Uiso 1 2 calc R U P . .
C2 C 0.5622(5) 0.4051(4) 0.5052(3) 0.0537(15) Uani 1 1 d . . . . .
C12 C 0.7368(5) 0.5522(5) 0.9862(5) 0.078(3) Uani 1 1 d . . . . .
H12A H 0.7362 0.6044 1.0186 0.094 Uiso 1 1 calc R U . . .
H12B H 0.8086 0.5615 0.9621 0.094 Uiso 1 1 calc R U . . .
C11 C 0.6187(6) 0.6757(5) 0.9341(4) 0.070(2) Uani 1 1 d . . . . .
H11A H 0.6103 0.7131 0.9723 0.105 Uiso 1 1 calc R U . . .
H11B H 0.5488 0.6854 0.9094 0.105 Uiso 1 1 calc R U . . .
H11C H 0.6866 0.7016 0.9121 0.105 Uiso 1 1 calc R U . . .
C4 C 0.8064(6) 0.4357(6) 0.6171(4) 0.082(3) Uani 1 1 d . . . . .
H4A H 0.7818 0.3838 0.6465 0.124 Uiso 1 1 calc R U . . .
H4B H 0.8914 0.4358 0.6142 0.124 Uiso 1 1 calc R U . . .
H4C H 0.7728 0.4199 0.5774 0.124 Uiso 1 1 calc R U . . .
C10 C 0.6530(8) 0.5118(7) 0.8897(4) 0.091(3) Uani 1 1 d . . . . .
H10A H 0.7321 0.5248 0.8751 0.136 Uiso 1 1 calc R U . . .
H10B H 0.5968 0.5358 0.8595 0.136 Uiso 1 1 calc R U . . .
H10C H 0.6424 0.4382 0.8963 0.136 Uiso 1 1 calc R U . . .
C5 C 0.8382(6) 0.6609(7) 0.5971(6) 0.108(4) Uani 1 1 d . . . . .
H5A H 0.8215 0.6510 0.5540 0.162 Uiso 1 1 calc R U . . .
H5B H 0.9217 0.6517 0.6043 0.162 Uiso 1 1 calc R U . . .
H5C H 0.8152 0.7302 0.6092 0.162 Uiso 1 1 calc R U . . .
C6 C 0.8121(7) 0.5693(6) 0.7211(4) 0.091(3) Uani 1 1 d . . . . .
H6A H 0.7916 0.6349 0.7398 0.136 Uiso 1 1 calc R U . . .
H6B H 0.8969 0.5619 0.7203 0.136 Uiso 1 1 calc R U . . .
H6C H 0.7781 0.5132 0.7446 0.136 Uiso 1 1 calc R U . . .
C7A C 0.4607(13) 0.6383(10) 0.7434(7) 0.077(4) Uani 0.6667 1 d . . P A 1
H7AA H 0.4036 0.5875 0.7298 0.116 Uiso 0.6667 1 calc R U P A 1
H7AB H 0.4202 0.6959 0.7625 0.116 Uiso 0.6667 1 calc R U P A 1
H7AC H 0.5137 0.6067 0.7727 0.116 Uiso 0.6667 1 calc R U P A 1
C9A C 0.6409(13) 0.7872(12) 0.7063(9) 0.090(6) Uani 0.6667 1 d . . P A 1
H9AA H 0.6990 0.7571 0.7335 0.135 Uiso 0.6667 1 calc R U P A 1
H9AB H 0.5941 0.8373 0.7286 0.135 Uiso 0.6667 1 calc R U P A 1
H9AC H 0.6804 0.8213 0.6725 0.135 Uiso 0.6667 1 calc R U P A 1
C8A C 0.4423(13) 0.7622(8) 0.6277(7) 0.088(5) Uani 0.6667 1 d . . P A 1
H8AA H 0.4862 0.7968 0.5957 0.131 Uiso 0.6667 1 calc R U P A 1
H8AB H 0.4023 0.8133 0.6527 0.131 Uiso 0.6667 1 calc R U P A 1
H8AC H 0.3849 0.7161 0.6095 0.131 Uiso 0.6667 1 calc R U P A 1
Li1 Li 0.5000 0.5000 1.0000 0.038(4) Uani 1 4 d S T P . .
C9B C 0.3973(17) 0.7125(17) 0.6589(10) 0.057(5) Uani 0.3333 1 d . . P A 2
H9BA H 0.3764 0.6784 0.6209 0.086 Uiso 0.3333 1 calc R U P A 2
H9BB H 0.3868 0.7866 0.6545 0.086 Uiso 0.3333 1 calc R U P A 2
H9BC H 0.3471 0.6872 0.6915 0.086 Uiso 0.3333 1 calc R U P A 2
C8B C 0.635(3) 0.808(2) 0.6600(19) 0.104(14) Uani 0.3333 1 d . . P A 2
H8BA H 0.7183 0.7925 0.6631 0.157 Uiso 0.3333 1 calc R U P A 2
H8BB H 0.6148 0.8613 0.6895 0.157 Uiso 0.3333 1 calc R U P A 2
H8BC H 0.6174 0.8324 0.6191 0.157 Uiso 0.3333 1 calc R U P A 2
C7B C 0.552(4) 0.668(2) 0.7592(13) 0.103(11) Uani 0.3333 1 d . . P A 2
H7BA H 0.5488 0.5948 0.7688 0.154 Uiso 0.3333 1 calc R U P A 2
H7BB H 0.4852 0.7027 0.7780 0.154 Uiso 0.3333 1 calc R U P A 2
H7BC H 0.6242 0.6974 0.7749 0.154 Uiso 0.3333 1 calc R U P A 2
C3 C 0.6016(17) 0.2886(16) 0.4939(13) 0.046(5) Uani 0.25 1 d . . P B -1
H3A H 0.5412 0.2422 0.5089 0.069 Uiso 0.25 1 calc R U P B -1
H3B H 0.6746 0.2754 0.5155 0.069 Uiso 0.25 1 calc R U P B -1
H3C H 0.6131 0.2773 0.4505 0.069 Uiso 0.25 1 calc R U P B -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
Ti1 N1 2.063(4) 2_665 ?
Ti1 N1 2.063(4) . ?
Si2 N1 1.720(4) . ?
Si2 C9B 1.79(2) . ?
Si2 C7B 1.84(3) . ?
Si2 C9A 1.840(14) . ?
Si2 C7A 1.871(13) . ?
Si2 C8A 1.894(11) . ?
Si2 C8B 1.94(2) . ?
Si1 N1 1.715(4) . ?
Si1 C6 1.855(8) . ?
Si1 C5 1.868(8) . ?
Si1 C4 1.879(7) . ?
N2 C11 1.461(7) . ?
N2 C10 1.465(9) . ?
N2 C12 1.476(9) . ?
N2 Li1 2.128(5) . ?
C1 C2 1.421(6) . ?
C1 C2 1.421(6) 4_566 ?
C1 Ti1 2.303(4) 3_656 ?
C1 H1 0.9500 . ?
C2 C2 1.449(12) 3_656 ?
C2 C3 1.61(2) . ?
C2 Ti1 2.411(7) 3_656 ?
C12 C12 1.493(12) 4_567 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
Li1 N2 2.128(5) 2_665 ?
Li1 N2 2.128(5) 4_567 ?
Li1 N2 2.128(5) 3_657 ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C8B H8BA 0.9800 . ?
C8B H8BB 0.9800 . ?
C8B H8BC 0.9800 . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 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
N1 Ti1 N1 107.2(3) 2_665 . ?
N1 Si2 C9B 115.8(7) . . ?
N1 Si2 C7B 112.4(10) . . ?
C9B Si2 C7B 106.2(16) . . ?
N1 Si2 C9A 118.8(5) . . ?
N1 Si2 C7A 110.7(4) . . ?
C9A Si2 C7A 105.7(8) . . ?
N1 Si2 C8A 112.3(4) . . ?
C9A Si2 C8A 101.2(7) . . ?
C7A Si2 C8A 107.2(7) . . ?
N1 Si2 C8B 108.5(10) . . ?
C9B Si2 C8B 107.6(14) . . ?
C7B Si2 C8B 105.8(17) . . ?
N1 Si1 C6 113.5(3) . . ?
N1 Si1 C5 112.1(3) . . ?
C6 Si1 C5 107.5(5) . . ?
N1 Si1 C4 115.4(3) . . ?
C6 Si1 C4 101.1(4) . . ?
C5 Si1 C4 106.2(5) . . ?
Si1 N1 Si2 119.6(2) . . ?
Si1 N1 Ti1 123.0(2) . . ?
Si2 N1 Ti1 117.2(2) . . ?
C11 N2 C10 109.3(6) . . ?
C11 N2 C12 109.7(5) . . ?
C10 N2 C12 109.1(6) . . ?
C11 N2 Li1 114.5(4) . . ?
C10 N2 Li1 112.4(4) . . ?
C12 N2 Li1 101.6(4) . . ?
C2 C1 C2 122.2(6) . 4_566 ?
C2 C1 Ti1 76.7(3) . 3_656 ?
C2 C1 Ti1 69.0(3) 4_566 3_656 ?
C2 C1 Ti1 69.0(3) . . ?
C2 C1 Ti1 76.7(3) 4_566 . ?
Ti1 C1 Ti1 105.0(3) 3_656 . ?
C2 C1 H1 118.9 . . ?
C2 C1 H1 118.9 4_566 . ?
Ti1 C1 H1 127.5 3_656 . ?
Ti1 C1 H1 127.5 . . ?
C1 C2 C2 117.7(3) . 3_656 ?
C1 C2 C3 132.6(9) . . ?
C2 C2 C3 104.7(8) 3_656 . ?
C1 C2 Ti1 74.5(3) . . ?
C2 C2 Ti1 78.7(4) 3_656 . ?
C3 C2 Ti1 137.3(10) . . ?
C1 C2 Ti1 68.3(3) . 3_656 ?
C2 C2 Ti1 65.2(5) 3_656 3_656 ?
C3 C2 Ti1 116.4(11) . 3_656 ?
Ti1 C2 Ti1 103.74(19) . 3_656 ?
N2 C12 C12 111.0(5) . 4_567 ?
N2 C12 H12A 109.4 . . ?
C12 C12 H12A 109.4 4_567 . ?
N2 C12 H12B 109.4 . . ?
C12 C12 H12B 109.4 4_567 . ?
H12A C12 H12B 108.0 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7A H7AA 109.5 . . ?
Si2 C7A H7AB 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
Si2 C7A H7AC 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
Si2 C9A H9AA 109.5 . . ?
Si2 C9A H9AB 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
Si2 C9A H9AC 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
Si2 C8A H8AA 109.5 . . ?
Si2 C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
Si2 C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
N2 Li1 N2 112.9(3) . 2_665 ?
N2 Li1 N2 86.9(3) . 4_567 ?
N2 Li1 N2 131.6(3) 2_665 4_567 ?
N2 Li1 N2 131.6(3) . 3_657 ?
N2 Li1 N2 86.9(3) 2_665 3_657 ?
N2 Li1 N2 112.9(3) 4_567 3_657 ?
Si2 C9B H9BA 109.5 . . ?
Si2 C9B H9BB 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
Si2 C9B H9BC 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
Si2 C8B H8BA 109.5 . . ?
Si2 C8B H8BB 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
Si2 C8B H8BC 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
Si2 C7B H7BA 109.5 . . ?
Si2 C7B H7BB 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
Si2 C7B H7BC 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
C6 Si1 N1 Si2 47.8(4) . . . . ?
C5 Si1 N1 Si2 -74.3(5) . . . . ?
C4 Si1 N1 Si2 163.9(4) . . . . ?
C6 Si1 N1 Ti1 -137.3(4) . . . . ?
C5 Si1 N1 Ti1 100.6(5) . . . . ?
C4 Si1 N1 Ti1 -21.2(5) . . . . ?
C9B Si2 N1 Si1 169.6(9) . . . . ?
C7B Si2 N1 Si1 -68.1(15) . . . . ?
C9A Si2 N1 Si1 14.8(8) . . . . ?
C7A Si2 N1 Si1 -107.7(6) . . . . ?
C8A Si2 N1 Si1 132.5(6) . . . . ?
C8B Si2 N1 Si1 48.6(14) . . . . ?
C9B Si2 N1 Ti1 -5.6(9) . . . . ?
C7B Si2 N1 Ti1 116.7(15) . . . . ?
C9A Si2 N1 Ti1 -160.4(7) . . . . ?
C7A Si2 N1 Ti1 77.1(6) . . . . ?
C8A Si2 N1 Ti1 -42.7(6) . . . . ?
C8B Si2 N1 Ti1 -126.6(14) . . . . ?
C2 C1 C2 C2 10.2(6) 4_566 . . 3_656 ?
Ti1 C1 C2 C2 -44.0(8) 3_656 . . 3_656 ?
Ti1 C1 C2 C2 68.0(7) . . . 3_656 ?
C2 C1 C2 C3 160.9(15) 4_566 . . . ?
Ti1 C1 C2 C3 106.6(15) 3_656 . . . ?
Ti1 C1 C2 C3 -141.4(15) . . . . ?
C2 C1 C2 Ti1 -57.78(13) 4_566 . . . ?
Ti1 C1 C2 Ti1 -112.05(17) 3_656 . . . ?
C2 C1 C2 Ti1 54.27(16) 4_566 . . 3_656 ?
Ti1 C1 C2 Ti1 112.05(17) . . . 3_656 ?
C11 N2 C12 C12 164.2(8) . . . 4_567 ?
C10 N2 C12 C12 -76.1(10) . . . 4_567 ?
Li1 N2 C12 C12 42.7(10) . . . 4_567 ?

_refine_diff_density_max         0.378
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_20047z_a
_database_code_depnum_ccdc_archive 'CCDC 2183467'
loop_
_audit_author_name
_audit_author_address
'Daniel Huh'
;University of Minnesota
United States of America
;
_audit_update_record             
;
2022-07-02 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            'Ti complex'
_chemical_melting_point          ?
_chemical_formula_moiety         'C48.50 H100 K N4 Si8 Ti2'
_chemical_formula_sum            'C48.50 H100 K N4 Si8 Ti2'
_chemical_formula_weight         1098.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.4417(7)
_cell_length_b                   25.7154(9)
_cell_length_c                   14.5174(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.8550(10)
_cell_angle_gamma                90
_cell_volume                     6231.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    126(2)
_cell_measurement_reflns_used    9989
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.17

_exptl_crystal_description       Block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_F_000             2376
_exptl_transmission_factor_min   0.814
_exptl_transmission_factor_max   0.902
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.510
_shelx_estimated_absorpt_T_min   0.822
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      126(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   micro
_diffrn_measurement_device_type  'Bruker Photon-II CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            129122
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.999
_diffrn_reflns_theta_max         26.060
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12306
_reflns_number_gt                8721
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0294P)²+5.3162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12306
_refine_ls_number_parameters     683
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.002

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
Ti1 Ti 0.29602(3) 0.52340(2) 0.60952(3) 0.01726(11) Uani 1 1 d . . . . .
Ti2 Ti 0.39474(3) 0.61433(2) 0.79918(3) 0.01847(11) Uani 1 1 d . . . . .
K1 K 0.17346(4) 0.43798(2) 0.41544(4) 0.02724(15) Uani 1 1 d . . . . .
Si1 Si 0.26687(4) 0.55801(3) 0.37022(5) 0.02094(17) Uani 1 1 d . . . . .
Si2 Si 0.13489(4) 0.56679(3) 0.45814(5) 0.02031(16) Uani 1 1 d . . . . .
Si3 Si 0.35143(4) 0.40550(3) 0.59260(5) 0.02007(16) Uani 1 1 d . . . . .
Si4 Si 0.21494(4) 0.41044(3) 0.67325(5) 0.02002(16) Uani 1 1 d . . . . .
Si5 Si 0.30892(5) 0.62261(3) 0.97844(6) 0.02914(19) Uani 1 1 d . . . . .
Si6 Si 0.31482(6) 0.71510(3) 0.85890(6) 0.0358(2) Uani 1 1 d D . . . .
Si7 Si 0.55629(5) 0.66855(3) 0.75686(6) 0.02467(18) Uani 1 1 d . . . . .
Si8 Si 0.56763(5) 0.63060(3) 0.95149(5) 0.02366(17) Uani 1 1 d . . . . .
N1 N 0.22915(12) 0.54360(8) 0.46511(15) 0.0183(5) Uani 1 1 d . . . . .
N2 N 0.27646(12) 0.44199(8) 0.61714(14) 0.0183(5) Uani 1 1 d . . . . .
N3 N 0.34172(13) 0.65092(8) 0.88838(15) 0.0236(5) Uani 1 1 d . . . . .
N4 N 0.51043(13) 0.63839(8) 0.83348(15) 0.0194(5) Uani 1 1 d . . . . .
C10 C 0.25366(18) 0.50247(11) 0.2820(2) 0.0303(7) Uani 1 1 d . . . . .
H10A H 0.276978 0.511954 0.230504 0.045 Uiso 1 1 calc R U . . .
H10B H 0.196438 0.495148 0.254308 0.045 Uiso 1 1 calc R U . . .
H10C H 0.280688 0.471467 0.315405 0.045 Uiso 1 1 calc R U . . .
C9 C 0.21759(18) 0.61397(11) 0.2921(2) 0.0320(7) Uani 1 1 d . . . . .
H9A H 0.225067 0.645844 0.330663 0.048 Uiso 1 1 calc R U . . .
H9B H 0.160208 0.606905 0.265255 0.048 Uiso 1 1 calc R U . . .
H9C H 0.241810 0.618356 0.239488 0.048 Uiso 1 1 calc R U . . .
C8 C 0.37525(17) 0.57589(11) 0.4063(2) 0.0287(7) Uani 1 1 d . . . . .
H8A H 0.383221 0.608146 0.443843 0.043 Uiso 1 1 calc R U . . .
H8B H 0.392712 0.580974 0.348579 0.043 Uiso 1 1 calc R U . . .
H8C H 0.406718 0.547926 0.445467 0.043 Uiso 1 1 calc R U . . .
C12 C 0.05733(16) 0.54554(12) 0.3438(2) 0.0298(7) Uani 1 1 d . . . . .
H12A H 0.009280 0.567143 0.333432 0.045 Uiso 1 1 calc R U . . .
H12B H 0.043356 0.509027 0.349658 0.045 Uiso 1 1 calc R U . . .
H12C H 0.079193 0.549457 0.289170 0.045 Uiso 1 1 calc R U . . .
C11 C 0.12556(17) 0.63936(10) 0.4665(2) 0.0282(7) Uani 1 1 d . . . . .
H11A H 0.076909 0.647743 0.484349 0.042 Uiso 1 1 calc R U . . .
H11B H 0.122480 0.655135 0.404126 0.042 Uiso 1 1 calc R U . . .
H11C H 0.172418 0.653026 0.515548 0.042 Uiso 1 1 calc R U . . .
C13 C 0.09623(16) 0.53897(11) 0.5556(2) 0.0257(6) Uani 1 1 d . . . . .
H13A H 0.040198 0.549283 0.544638 0.039 Uiso 1 1 calc R U . . .
H13B H 0.128405 0.552158 0.618256 0.039 Uiso 1 1 calc R U . . .
H13C H 0.099903 0.500955 0.554926 0.039 Uiso 1 1 calc R U . . .
C14 C 0.31100(17) 0.34663(10) 0.5160(2) 0.0277(6) Uani 1 1 d . . . . .
H14A H 0.355707 0.325752 0.508181 0.042 Uiso 1 1 calc R U . . .
H14B H 0.277439 0.357963 0.452674 0.042 Uiso 1 1 calc R U . . .
H14C H 0.278890 0.325653 0.547380 0.042 Uiso 1 1 calc R U . . .
C15 C 0.40234(16) 0.44502(10) 0.51934(19) 0.0239(6) Uani 1 1 d . . . . .
H15A H 0.443693 0.423939 0.503732 0.036 Uiso 1 1 calc R U . . .
H15B H 0.427143 0.475667 0.556225 0.036 Uiso 1 1 calc R U . . .
H15C H 0.362852 0.456171 0.459702 0.036 Uiso 1 1 calc R U . . .
C16 C 0.43159(17) 0.38053(11) 0.6991(2) 0.0286(7) Uani 1 1 d . . . . .
H16A H 0.480993 0.375060 0.681168 0.043 Uiso 1 1 calc R U . . .
H16B H 0.414336 0.347516 0.720374 0.043 Uiso 1 1 calc R U . . .
H16C H 0.441397 0.405941 0.751557 0.043 Uiso 1 1 calc R U . . .
C17 C 0.26102(18) 0.35177(11) 0.7450(2) 0.0297(7) Uani 1 1 d . . . . .
H17A H 0.223387 0.337069 0.776693 0.044 Uiso 1 1 calc R U . . .
H17B H 0.310537 0.361900 0.793795 0.044 Uiso 1 1 calc R U . . .
H17C H 0.273213 0.325713 0.702044 0.044 Uiso 1 1 calc R U . . .
C19 C 0.12192(17) 0.38377(11) 0.5834(2) 0.0284(6) Uani 1 1 d . . . . .
H19A H 0.089914 0.364643 0.617557 0.043 Uiso 1 1 calc R U . . .
H19B H 0.137461 0.360292 0.538708 0.043 Uiso 1 1 calc R U . . .
H19C H 0.090190 0.412553 0.547300 0.043 Uiso 1 1 calc R U . . .
C18 C 0.17966(17) 0.44934(10) 0.76147(19) 0.0249(6) Uani 1 1 d . . . . .
H18A H 0.225807 0.460040 0.814724 0.037 Uiso 1 1 calc R U . . .
H18B H 0.143464 0.428168 0.786526 0.037 Uiso 1 1 calc R U . . .
H18C H 0.151162 0.480253 0.729531 0.037 Uiso 1 1 calc R U . . .
C20 C 0.3179(2) 0.55021(12) 0.9905(2) 0.0397(8) Uani 1 1 d . . . . .
H20A H 0.310607 0.539571 1.052188 0.059 Uiso 1 1 calc R U . . .
H20B H 0.371112 0.539397 0.987755 0.059 Uiso 1 1 calc R U . . .
H20C H 0.276801 0.533780 0.937767 0.059 Uiso 1 1 calc R U . . .
C21 C 0.1994(2) 0.63430(17) 0.9605(4) 0.0718(13) Uani 1 1 d . . . . .
H21A H 0.183944 0.619715 1.014866 0.108 Uiso 1 1 calc R U . . .
H21B H 0.168244 0.617524 0.900719 0.108 Uiso 1 1 calc R U . . .
H21C H 0.188761 0.671783 0.956423 0.108 Uiso 1 1 calc R U . . .
C22 C 0.3652(2) 0.64745(14) 1.1008(2) 0.0485(9) Uani 1 1 d . . . . .
H22A H 0.352605 0.625859 1.150159 0.073 Uiso 1 1 calc R U . . .
H22B H 0.349410 0.683498 1.107644 0.073 Uiso 1 1 calc R U . . .
H22C H 0.422829 0.645975 1.108573 0.073 Uiso 1 1 calc R U . . .
C23A C 0.3108(9) 0.7573(7) 0.9614(10) 0.039(3) Uani 0.60(2) 1 d D . P A 1
H23A H 0.295607 0.792629 0.938027 0.059 Uiso 0.60(2) 1 calc R U P A 1
H23B H 0.363529 0.757923 1.009365 0.059 Uiso 0.60(2) 1 calc R U P A 1
H23C H 0.271050 0.743443 0.990821 0.059 Uiso 0.60(2) 1 calc R U P A 1
C24A C 0.2072(7) 0.7168(4) 0.7746(9) 0.063(3) Uani 0.60(2) 1 d D . P A 1
H24A H 0.185717 0.752068 0.772794 0.094 Uiso 0.60(2) 1 calc R U P A 1
H24B H 0.173771 0.692644 0.798359 0.094 Uiso 0.60(2) 1 calc R U P A 1
H24C H 0.207298 0.706390 0.709675 0.094 Uiso 0.60(2) 1 calc R U P A 1
C25B C 0.3788(9) 0.7468(4) 0.7976(13) 0.079(4) Uani 0.60(2) 1 d D . P A 1
H25A H 0.360288 0.782508 0.781370 0.119 Uiso 0.60(2) 1 calc R U P A 1
H25B H 0.376649 0.727671 0.738463 0.119 Uiso 0.60(2) 1 calc R U P A 1
H25C H 0.433999 0.747240 0.839693 0.119 Uiso 0.60(2) 1 calc R U P A 1
C23B C 0.2860(13) 0.7518(11) 0.9536(16) 0.042(5) Uani 0.40(2) 1 d D . P A 2
H23D H 0.283462 0.789035 0.938309 0.062 Uiso 0.40(2) 1 calc R U P A 2
H23E H 0.325833 0.745939 1.015924 0.062 Uiso 0.40(2) 1 calc R U P A 2
H23F H 0.233360 0.739966 0.956610 0.062 Uiso 0.40(2) 1 calc R U P A 2
C24B C 0.2402(11) 0.7270(5) 0.7411(9) 0.046(4) Uani 0.40(2) 1 d D . P A 2
H24D H 0.226419 0.764079 0.734996 0.069 Uiso 0.40(2) 1 calc R U P A 2
H24E H 0.191819 0.706563 0.736700 0.069 Uiso 0.40(2) 1 calc R U P A 2
H24F H 0.262654 0.716784 0.689332 0.069 Uiso 0.40(2) 1 calc R U P A 2
C25A C 0.4051(7) 0.7565(5) 0.8503(13) 0.048(4) Uani 0.40(2) 1 d D . P A 2
H25D H 0.386600 0.791281 0.826526 0.072 Uiso 0.40(2) 1 calc R U P A 2
H25E H 0.430473 0.739807 0.805842 0.072 Uiso 0.40(2) 1 calc R U P A 2
H25F H 0.444084 0.759258 0.914120 0.072 Uiso 0.40(2) 1 calc R U P A 2
C28 C 0.4888(2) 0.69580(13) 0.6429(2) 0.0415(8) Uani 1 1 d . . . . .
H28A H 0.519872 0.717826 0.611889 0.062 Uiso 1 1 calc R U . . .
H28B H 0.446669 0.716605 0.657539 0.062 Uiso 1 1 calc R U . . .
H28C H 0.464298 0.667274 0.599607 0.062 Uiso 1 1 calc R U . . .
C27 C 0.62491(19) 0.62331(12) 0.7170(2) 0.0367(8) Uani 1 1 d . . . . .
H27A H 0.647630 0.641336 0.671472 0.055 Uiso 1 1 calc R U . . .
H27B H 0.594658 0.592840 0.685619 0.055 Uiso 1 1 calc R U . . .
H27C H 0.668280 0.612126 0.773063 0.055 Uiso 1 1 calc R U . . .
C26 C 0.61831(19) 0.72624(11) 0.8138(2) 0.0347(7) Uani 1 1 d . . . . .
H26A H 0.643876 0.741411 0.768234 0.052 Uiso 1 1 calc R U . . .
H26B H 0.659599 0.715092 0.871954 0.052 Uiso 1 1 calc R U . . .
H26C H 0.583775 0.752281 0.830997 0.052 Uiso 1 1 calc R U . . .
C31 C 0.53035(18) 0.57621(11) 1.0117(2) 0.0331(7) Uani 1 1 d . . . . .
H31A H 0.566376 0.571452 1.076890 0.050 Uiso 1 1 calc R U . . .
H31B H 0.528662 0.544141 0.974696 0.050 Uiso 1 1 calc R U . . .
H31C H 0.476399 0.584427 1.015213 0.050 Uiso 1 1 calc R U . . .
C29 C 0.5671(2) 0.69049(12) 1.0248(2) 0.0381(8) Uani 1 1 d . . . . .
H29A H 0.594781 0.683313 1.092584 0.057 Uiso 1 1 calc R U . . .
H29B H 0.511645 0.700747 1.018231 0.057 Uiso 1 1 calc R U . . .
H29C H 0.594562 0.718749 1.001888 0.057 Uiso 1 1 calc R U . . .
C30 C 0.67467(17) 0.61192(12) 0.9656(2) 0.0358(7) Uani 1 1 d . . . . .
H30A H 0.702915 0.607186 1.033978 0.054 Uiso 1 1 calc R U . . .
H30B H 0.700835 0.639482 0.939055 0.054 Uiso 1 1 calc R U . . .
H30C H 0.676034 0.579368 0.930973 0.054 Uiso 1 1 calc R U . . .
C7 C 0.50110(16) 0.51101(11) 0.7546(2) 0.0286(7) Uani 1 1 d . . . . .
H7A H 0.541801 0.536520 0.786826 0.043 Uiso 1 1 calc R U . . .
H7B H 0.513480 0.497571 0.697389 0.043 Uiso 1 1 calc R U . . .
H7C H 0.500782 0.482262 0.798811 0.043 Uiso 1 1 calc R U . . .
C1 C 0.41990(16) 0.53669(10) 0.72510(18) 0.0203(6) Uani 1 1 d . . . . .
C6 C 0.36551(16) 0.53082(10) 0.78206(19) 0.0208(6) Uani 1 1 d . . . . .
C5 C 0.28801(17) 0.55478(10) 0.74940(19) 0.0214(6) Uani 1 1 d . . . . .
C4 C 0.27515(17) 0.59704(10) 0.68172(19) 0.0207(6) Uani 1 1 d . . . . .
C3 C 0.33902(16) 0.61347(10) 0.64327(19) 0.0207(6) Uani 1 1 d . . . . .
C2 C 0.40343(16) 0.57656(10) 0.65173(19) 0.0200(6) Uani 1 1 d . . . . .
C38 C 0.1902(2) 0.29183(14) 0.2789(3) 0.0530(10) Uani 1 1 d . . . . .
H38A H 0.165282 0.261559 0.240916 0.080 Uiso 1 1 calc R U . . .
H38B H 0.215131 0.281211 0.345773 0.080 Uiso 1 1 calc R U . . .
H38C H 0.231081 0.306338 0.252160 0.080 Uiso 1 1 calc R U . . .
C32 C 0.12785(19) 0.33197(12) 0.2759(2) 0.0362(8) Uani 1 1 d . . . . .
C33 C 0.1193(2) 0.37478(13) 0.2144(2) 0.0420(8) Uani 1 1 d . . . . .
H33 H 0.153016 0.376988 0.169305 0.050 Uiso 1 1 calc R U . . .
C34 C 0.0569(2) 0.40994(13) 0.2047(2) 0.0425(9) Uani 1 1 d . . . . .
H34 H 0.045997 0.436654 0.152448 0.051 Uiso 1 1 calc R U . . .
C35 C 0.0034(2) 0.40311(13) 0.2568(2) 0.0423(8) Uani 1 1 d . . . . .
H35 H -0.044762 0.426041 0.244755 0.051 Uiso 1 1 calc R U . . .
C36 C 0.0121(2) 0.36106(13) 0.3189(2) 0.0396(8) Uani 1 1 d . . . . .
H36 H -0.024710 0.356177 0.355244 0.048 Uiso 1 1 calc R U . . .
C37 C 0.0741(2) 0.32641(12) 0.3279(2) 0.0357(8) Uani 1 1 d . . . . .
H37 H 0.079811 0.297997 0.371222 0.043 Uiso 1 1 calc R U . . .
H6 H 0.3737(16) 0.5044(11) 0.824(2) 0.025(8) Uiso 1 1 d . . . . .
H5 H 0.2497(16) 0.5511(10) 0.7846(19) 0.025(7) Uiso 1 1 d . . . . .
H4 H 0.2304(16) 0.6157(10) 0.6723(18) 0.018(7) Uiso 1 1 d . . . . .
H3 H 0.3270(16) 0.6383(11) 0.590(2) 0.026(7) Uiso 1 1 d . . . . .
H2 H 0.4428(16) 0.5850(10) 0.6237(18) 0.020(7) Uiso 1 1 d . . . . .
C45 C -0.0103(2) 0.26853(14) 0.0757(2) 0.0518(10) Uani 1 1 d D . . . .
H45A H 0.029836 0.244393 0.114204 0.078 Uiso 1 1 calc R U . . .
H45B H -0.062493 0.251176 0.054890 0.078 Uiso 1 1 calc R U . . .
H45C H -0.013870 0.299080 0.114557 0.078 Uiso 1 1 calc R U . . .
C39 C 0.0139(2) 0.28533(12) -0.0114(2) 0.0363(8) Uani 1 1 d D . . . .
C44 C 0.0930(2) 0.29684(14) -0.0048(2) 0.0461(9) Uani 1 1 d D . . . .
H44 H 0.132898 0.293173 0.055314 0.055 Uiso 1 1 calc R U . . .
C43 C 0.1148(2) 0.31360(15) -0.0844(3) 0.0568(11) Uani 1 1 d D . . . .
H43 H 0.169223 0.321558 -0.078345 0.068 Uiso 1 1 calc R U . . .
C42 C 0.0584(3) 0.31868(14) -0.1713(3) 0.0531(10) Uani 1 1 d D . . . .
H42 H 0.073131 0.330457 -0.225779 0.064 Uiso 1 1 calc R U . . .
C41 C -0.0196(2) 0.30669(16) -0.1793(3) 0.0575(11) Uani 1 1 d D . . . .
H41 H -0.059105 0.309594 -0.239862 0.069 Uiso 1 1 calc R U . . .
C40 C -0.0414(2) 0.29036(14) -0.0997(3) 0.0498(9) Uani 1 1 d D . . . .
H40 H -0.095941 0.282451 -0.106466 0.060 Uiso 1 1 calc R U . . .
C52 C 0.1250(8) 0.4701(7) -0.0082(15) 0.067(4) Uani 0.5 1 d D . P B -1
H52A H 0.118912 0.435056 -0.035965 0.101 Uiso 0.5 1 calc R U P B -1
H52B H 0.162779 0.469072 0.056629 0.101 Uiso 0.5 1 calc R U P B -1
H52C H 0.145391 0.493560 -0.048780 0.101 Uiso 0.5 1 calc R U P B -1
C46 C 0.0459(5) 0.4891(3) -0.0027(5) 0.0409(17) Uani 0.5 1 d D . P B -1
C51 C 0.0395(11) 0.5333(8) 0.046(2) 0.036(4) Uani 0.5 1 d D . P B -1
H51 H 0.087234 0.551435 0.078004 0.043 Uiso 0.5 1 calc R U P B -1
C50 C -0.0333(11) 0.5536(4) 0.0514(7) 0.072(4) Uani 0.5 1 d D . P B -1
H50 H -0.037062 0.585478 0.083002 0.086 Uiso 0.5 1 calc R U P B -1
C49 C -0.0976(10) 0.5245(9) 0.0083(17) 0.114(8) Uani 0.5 1 d D . P B -1
H49 H -0.149076 0.535917 0.009475 0.136 Uiso 0.5 1 calc R U P B -1
C48 C -0.0911(9) 0.4780(6) -0.0381(8) 0.078(4) Uani 0.5 1 d D . P B -1
H48 H -0.138464 0.458958 -0.067733 0.094 Uiso 0.5 1 calc R U P B -1
C47 C -0.0201(11) 0.4591(10) -0.042(2) 0.063(6) Uani 0.5 1 d D . P B -1
H47 H -0.016138 0.426536 -0.071746 0.075 Uiso 0.5 1 calc R U P B -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
Ti1 N2 2.129(2) . ?
Ti1 N1 2.147(2) . ?
Ti1 C5 2.227(3) . ?
Ti1 C4 2.245(3) . ?
Ti1 C2 2.256(3) . ?
Ti1 C1 2.345(3) . ?
Ti1 C3 2.440(3) . ?
Ti1 C6 2.453(3) . ?
Ti1 K1 3.7203(7) . ?
Ti2 N3 2.028(2) . ?
Ti2 N4 2.030(2) . ?
Ti2 C3 2.189(3) . ?
Ti2 C6 2.205(3) . ?
Ti2 C4 2.322(3) . ?
Ti2 C5 2.356(3) . ?
Ti2 C1 2.368(3) . ?
Ti2 C2 2.395(3) . ?
K1 N1 2.904(2) . ?
K1 N2 2.960(2) . ?
K1 C34 3.226(3) . ?
K1 C33 3.234(3) . ?
K1 C35 3.308(3) . ?
K1 C32 3.352(3) . ?
K1 C14 3.372(3) . ?
K1 C36 3.392(3) . ?
K1 C37 3.402(3) . ?
K1 C12 3.408(3) . ?
K1 Si2 3.4715(10) . ?
K1 Si3 3.5097(9) . ?
Si1 N1 1.730(2) . ?
Si1 C8 1.867(3) . ?
Si1 C9 1.879(3) . ?
Si1 C10 1.887(3) . ?
Si2 N1 1.724(2) . ?
Si2 C13 1.877(3) . ?
Si2 C11 1.880(3) . ?
Si2 C12 1.892(3) . ?
Si3 N2 1.728(2) . ?
Si3 C15 1.871(3) . ?
Si3 C16 1.872(3) . ?
Si3 C14 1.890(3) . ?
Si4 N2 1.726(2) . ?
Si4 C18 1.865(3) . ?
Si4 C17 1.877(3) . ?
Si4 C19 1.891(3) . ?
Si5 N3 1.732(2) . ?
Si5 C20 1.872(3) . ?
Si5 C22 1.875(3) . ?
Si5 C21 1.876(4) . ?
Si6 N3 1.735(2) . ?
Si6 C25B 1.810(8) . ?
Si6 C24B 1.850(8) . ?
Si6 C23A 1.859(8) . ?
Si6 C23B 1.854(12) . ?
Si6 C24A 1.921(8) . ?
Si6 C25A 1.935(10) . ?
Si7 N4 1.730(2) . ?
Si7 C28 1.866(3) . ?
Si7 C27 1.877(3) . ?
Si7 C26 1.880(3) . ?
Si8 N4 1.726(2) . ?
Si8 C31 1.864(3) . ?
Si8 C29 1.874(3) . ?
Si8 C30 1.881(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25B H25A 0.9800 . ?
C25B H25B 0.9800 . ?
C25B H25C 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C7 C1 1.508(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C1 C6 1.436(4) . ?
C1 C2 1.446(4) . ?
C6 C5 1.435(4) . ?
C6 H6 0.89(3) . ?
C5 C4 1.438(4) . ?
C5 H5 0.96(3) . ?
C4 C3 1.446(4) . ?
C4 H4 0.89(3) . ?
C3 C2 1.449(4) . ?
C3 H3 0.98(3) . ?
C2 H2 0.92(3) . ?
C38 C32 1.490(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C32 C37 1.371(4) . ?
C32 C33 1.398(4) . ?
C33 C34 1.390(5) . ?
C33 H33 1.0000 . ?
C34 C35 1.372(5) . ?
C34 H34 1.0000 . ?
C35 C36 1.388(5) . ?
C35 H35 1.0000 . ?
C36 C37 1.378(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C45 C39 1.507(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C39 C40 1.369(4) . ?
C39 C44 1.387(4) . ?
C44 C43 1.386(5) . ?
C44 H44 0.9500 . ?
C43 C42 1.363(5) . ?
C43 H43 0.9500 . ?
C42 C41 1.367(5) . ?
C42 H42 0.9500 . ?
C41 C40 1.381(5) . ?
C41 H41 0.9500 . ?
C40 H40 0.9500 . ?
C52 C46 1.487(11) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C46 C51 1.360(14) . ?
C46 C47 1.367(15) . ?
C51 C50 1.396(14) . ?
C51 H51 0.9500 . ?
C50 C49 1.343(16) . ?
C50 H50 0.9500 . ?
C49 C48 1.391(15) . ?
C49 H49 0.9500 . ?
C48 C47 1.350(14) . ?
C48 H48 0.9500 . ?
C47 H47 0.9500 . ?

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
N2 Ti1 N1 103.82(8) . . ?
N2 Ti1 C5 104.81(9) . . ?
N1 Ti1 C5 130.01(9) . . ?
N2 Ti1 C4 139.04(9) . . ?
N1 Ti1 C4 97.82(9) . . ?
C5 Ti1 C4 37.52(9) . . ?
N2 Ti1 C2 135.63(9) . . ?
N1 Ti1 C2 106.97(9) . . ?
C5 Ti1 C2 78.43(10) . . ?
C4 Ti1 C2 66.18(10) . . ?
N2 Ti1 C1 103.56(8) . . ?
N1 Ti1 C1 142.24(9) . . ?
C5 Ti1 C1 65.36(10) . . ?
C4 Ti1 C1 77.49(10) . . ?
C2 Ti1 C1 36.58(9) . . ?
N2 Ti1 C3 165.34(9) . . ?
N1 Ti1 C3 90.84(8) . . ?
C5 Ti1 C3 64.52(9) . . ?
C4 Ti1 C3 35.65(9) . . ?
C2 Ti1 C3 35.66(9) . . ?
C1 Ti1 C3 63.40(9) . . ?
N2 Ti1 C6 93.59(8) . . ?
N1 Ti1 C6 161.09(9) . . ?
C5 Ti1 C6 35.30(9) . . ?
C4 Ti1 C6 63.68(9) . . ?
C2 Ti1 C6 63.26(9) . . ?
C1 Ti1 C6 34.73(9) . . ?
C3 Ti1 C6 71.89(9) . . ?
N2 Ti1 K1 52.64(6) . . ?
N1 Ti1 K1 51.18(6) . . ?
C5 Ti1 K1 136.92(7) . . ?
C4 Ti1 K1 135.76(7) . . ?
C2 Ti1 K1 144.40(7) . . ?
C1 Ti1 K1 146.71(6) . . ?
C3 Ti1 K1 142.01(6) . . ?
C6 Ti1 K1 145.53(7) . . ?
N3 Ti2 N4 107.88(9) . . ?
N3 Ti2 C3 121.14(10) . . ?
N4 Ti2 C3 111.62(9) . . ?
N3 Ti2 C6 112.99(10) . . ?
N4 Ti2 C6 120.36(9) . . ?
C3 Ti2 C6 81.65(10) . . ?
N3 Ti2 C4 94.53(9) . . ?
N4 Ti2 C4 148.85(9) . . ?
C3 Ti2 C4 37.25(10) . . ?
C6 Ti2 C4 66.53(10) . . ?
N3 Ti2 C5 91.80(10) . . ?
N4 Ti2 C5 156.07(9) . . ?
C3 Ti2 C5 66.55(10) . . ?
C6 Ti2 C5 36.49(9) . . ?
C4 Ti2 C5 35.80(9) . . ?
N3 Ti2 C1 149.31(9) . . ?
N4 Ti2 C1 93.81(9) . . ?
C3 Ti2 C1 66.87(9) . . ?
C6 Ti2 C1 36.37(9) . . ?
C4 Ti2 C1 75.55(9) . . ?
C5 Ti2 C1 63.05(9) . . ?
N3 Ti2 C2 156.59(9) . . ?
N4 Ti2 C2 91.53(9) . . ?
C3 Ti2 C2 36.49(9) . . ?
C6 Ti2 C2 64.96(10) . . ?
C4 Ti2 C2 62.76(9) . . ?
C5 Ti2 C2 73.23(10) . . ?
C1 Ti2 C2 35.34(9) . . ?
N1 K1 N2 70.03(6) . . ?
N1 K1 C34 121.19(7) . . ?
N2 K1 C34 168.76(7) . . ?
N1 K1 C33 133.10(7) . . ?
N2 K1 C33 147.70(8) . . ?
C34 K1 C33 24.85(9) . . ?
N1 K1 C35 126.45(8) . . ?
N2 K1 C35 149.62(8) . . ?
C34 K1 C35 24.20(8) . . ?
C33 K1 C35 42.85(9) . . ?
N1 K1 C32 156.12(7) . . ?
N2 K1 C32 126.58(7) . . ?
C34 K1 C32 43.20(8) . . ?
C33 K1 C32 24.43(8) . . ?
C35 K1 C32 49.53(8) . . ?
N1 K1 C14 113.53(6) . . ?
N2 K1 C14 56.26(6) . . ?
C34 K1 C14 115.36(8) . . ?
C33 K1 C14 91.47(8) . . ?
C35 K1 C14 119.61(8) . . ?
C32 K1 C14 73.11(7) . . ?
N1 K1 C36 145.64(7) . . ?
N2 K1 C36 128.44(7) . . ?
C34 K1 C36 42.17(8) . . ?
C33 K1 C36 48.99(8) . . ?
C35 K1 C36 23.87(8) . . ?
C32 K1 C36 41.67(8) . . ?
C14 K1 C36 99.99(8) . . ?
N1 K1 C37 168.24(7) . . ?
N2 K1 C37 119.74(7) . . ?
C34 K1 C37 49.05(8) . . ?
C33 K1 C37 41.85(8) . . ?
C35 K1 C37 41.81(8) . . ?
C32 K1 C37 23.41(7) . . ?
C14 K1 C37 78.20(7) . . ?
C36 K1 C37 23.41(7) . . ?
N1 K1 C12 56.16(6) . . ?
N2 K1 C12 114.21(6) . . ?
C34 K1 C12 74.74(8) . . ?
C33 K1 C12 98.06(8) . . ?
C35 K1 C12 70.98(8) . . ?
C32 K1 C12 117.38(8) . . ?
C14 K1 C12 169.33(7) . . ?
C36 K1 C12 89.93(8) . . ?
C37 K1 C12 112.17(8) . . ?
N1 K1 Si2 29.71(4) . . ?
N2 K1 Si2 83.31(4) . . ?
C34 K1 Si2 106.33(6) . . ?
C33 K1 Si2 128.30(7) . . ?
C35 K1 Si2 101.65(6) . . ?
C32 K1 Si2 149.28(6) . . ?
C14 K1 Si2 137.54(5) . . ?
C36 K1 Si2 116.71(6) . . ?
C37 K1 Si2 140.13(6) . . ?
C12 K1 Si2 31.91(5) . . ?
N1 K1 Si3 83.08(4) . . ?
N2 K1 Si3 29.45(4) . . ?
C34 K1 Si3 145.28(7) . . ?
C33 K1 Si3 120.45(7) . . ?
C35 K1 Si3 150.41(6) . . ?
C32 K1 Si3 104.71(6) . . ?
C14 K1 Si3 31.80(5) . . ?
C36 K1 Si3 127.98(6) . . ?
C37 K1 Si3 108.63(6) . . ?
C12 K1 Si3 137.55(5) . . ?
Si2 K1 Si3 105.80(2) . . ?
N1 Si1 C8 114.66(12) . . ?
N1 Si1 C9 115.58(12) . . ?
C8 Si1 C9 103.27(13) . . ?
N1 Si1 C10 112.23(12) . . ?
C8 Si1 C10 106.94(13) . . ?
C9 Si1 C10 103.02(13) . . ?
N1 Si1 K1 51.76(7) . . ?
C8 Si1 K1 128.93(9) . . ?
C9 Si1 K1 127.47(10) . . ?
C10 Si1 K1 60.48(9) . . ?
N1 Si2 C13 111.65(11) . . ?
N1 Si2 C11 116.01(12) . . ?
C13 Si2 C11 105.81(13) . . ?
N1 Si2 C12 112.25(12) . . ?
C13 Si2 C12 103.27(13) . . ?
C11 Si2 C12 106.87(13) . . ?
N1 Si2 K1 56.60(7) . . ?
C13 Si2 K1 84.35(9) . . ?
C11 Si2 K1 169.59(10) . . ?
C12 Si2 K1 72.19(9) . . ?
N2 Si3 C15 109.53(11) . . ?
N2 Si3 C16 116.39(12) . . ?
C15 Si3 C16 106.98(13) . . ?
N2 Si3 C14 112.38(12) . . ?
C15 Si3 C14 104.97(13) . . ?
C16 Si3 C14 105.86(13) . . ?
N2 Si3 K1 57.36(7) . . ?
C15 Si3 K1 85.34(9) . . ?
C16 Si3 K1 167.68(10) . . ?
C14 Si3 K1 70.09(9) . . ?
N2 Si4 C18 116.49(11) . . ?
N2 Si4 C17 114.52(12) . . ?
C18 Si4 C17 102.91(13) . . ?
N2 Si4 C19 111.78(12) . . ?
C18 Si4 C19 106.28(13) . . ?
C17 Si4 C19 103.60(13) . . ?
N2 Si4 K1 52.67(7) . . ?
C18 Si4 K1 126.18(9) . . ?
C17 Si4 K1 130.35(10) . . ?
C19 Si4 K1 59.36(9) . . ?
N3 Si5 C20 116.82(13) . . ?
N3 Si5 C22 112.05(14) . . ?
C20 Si5 C22 104.11(15) . . ?
N3 Si5 C21 111.93(16) . . ?
C20 Si5 C21 103.12(18) . . ?
C22 Si5 C21 108.0(2) . . ?
N3 Si6 C25B 112.8(3) . . ?
N3 Si6 C24B 117.0(4) . . ?
N3 Si6 C23A 115.3(6) . . ?
C25B Si6 C23A 107.7(6) . . ?
N3 Si6 C23B 114.5(10) . . ?
C24B Si6 C23B 109.3(9) . . ?
N3 Si6 C24A 108.8(3) . . ?
C25B Si6 C24A 107.7(4) . . ?
C23A Si6 C24A 103.9(5) . . ?
N3 Si6 C25A 111.8(4) . . ?
C24B Si6 C25A 102.6(5) . . ?
C23B Si6 C25A 99.7(7) . . ?
N4 Si7 C28 116.57(13) . . ?
N4 Si7 C27 112.04(12) . . ?
C28 Si7 C27 104.74(15) . . ?
N4 Si7 C26 112.65(12) . . ?
C28 Si7 C26 103.20(14) . . ?
C27 Si7 C26 106.72(14) . . ?
N4 Si8 C31 111.89(12) . . ?
N4 Si8 C29 111.82(12) . . ?
C31 Si8 C29 106.89(14) . . ?
N4 Si8 C30 114.04(13) . . ?
C31 Si8 C30 103.17(14) . . ?
C29 Si8 C30 108.45(15) . . ?
Si2 N1 Si1 117.10(12) . . ?
Si2 N1 Ti1 112.33(11) . . ?
Si1 N1 Ti1 127.24(11) . . ?
Si2 N1 K1 93.69(9) . . ?
Si1 N1 K1 100.35(9) . . ?
Ti1 N1 K1 93.67(7) . . ?
Si4 N2 Si3 116.94(12) . . ?
Si4 N2 Ti1 128.14(11) . . ?
Si3 N2 Ti1 112.39(11) . . ?
Si4 N2 K1 99.70(9) . . ?
Si3 N2 K1 93.19(8) . . ?
Ti1 N2 K1 92.48(7) . . ?
Si5 N3 Si6 117.45(13) . . ?
Si5 N3 Ti2 126.77(12) . . ?
Si6 N3 Ti2 115.13(12) . . ?
Si8 N4 Si7 116.62(13) . . ?
Si8 N4 Ti2 117.10(11) . . ?
Si7 N4 Ti2 126.22(12) . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C12 K1 75.89(9) . . ?
Si2 C12 H12A 109.5 . . ?
K1 C12 H12A 155.9 . . ?
Si2 C12 H12B 109.5 . . ?
K1 C12 H12B 48.4 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
K1 C12 H12C 89.7 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si3 C14 K1 78.11(9) . . ?
Si3 C14 H14A 109.5 . . ?
K1 C14 H14A 145.2 . . ?
Si3 C14 H14B 109.5 . . ?
K1 C14 H14B 39.7 . . ?
H14A C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
K1 C14 H14C 98.9 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si3 C16 H16A 109.5 . . ?
Si3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C19 H19A 109.5 . . ?
Si4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si5 C20 H20A 109.5 . . ?
Si5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si5 C21 H21A 109.5 . . ?
Si5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si5 C22 H22A 109.5 . . ?
Si5 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si5 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si6 C23A H23A 109.5 . . ?
Si6 C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
Si6 C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
Si6 C24A H24A 109.5 . . ?
Si6 C24A H24B 109.4 . . ?
H24A C24A H24B 109.5 . . ?
Si6 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
Si6 C25B H25A 109.5 . . ?
Si6 C25B H25B 109.4 . . ?
H25A C25B H25B 109.5 . . ?
Si6 C25B H25C 109.5 . . ?
H25A C25B H25C 109.5 . . ?
H25B C25B H25C 109.5 . . ?
Si6 C23B H23D 109.5 . . ?
Si6 C23B H23E 109.4 . . ?
H23D C23B H23E 109.5 . . ?
Si6 C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
Si6 C24B H24D 109.5 . . ?
Si6 C24B H24E 109.4 . . ?
H24D C24B H24E 109.5 . . ?
Si6 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
Si6 C25A H25D 109.5 . . ?
Si6 C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
Si6 C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
Si7 C28 H28A 109.5 . . ?
Si7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si7 C27 H27A 109.5 . . ?
Si7 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si7 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si7 C26 H26A 109.5 . . ?
Si7 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si7 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si8 C31 H31A 109.5 . . ?
Si8 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si8 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si8 C29 H29A 109.5 . . ?
Si8 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si8 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si8 C30 H30A 109.5 . . ?
Si8 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si8 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C1 C2 118.4(2) . . ?
C6 C1 C7 120.9(2) . . ?
C2 C1 C7 119.3(2) . . ?
C6 C1 Ti1 76.78(15) . . ?
C2 C1 Ti1 68.36(14) . . ?
C7 C1 Ti1 137.24(18) . . ?
C6 C1 Ti2 65.59(14) . . ?
C2 C1 Ti2 73.34(15) . . ?
C7 C1 Ti2 121.51(17) . . ?
Ti1 C1 Ti2 101.20(10) . . ?
C5 C6 C1 118.7(2) . . ?
C5 C6 Ti2 77.51(15) . . ?
C1 C6 Ti2 78.03(15) . . ?
C5 C6 Ti1 63.70(14) . . ?
C1 C6 Ti1 68.50(14) . . ?
Ti2 C6 Ti1 102.73(11) . . ?
C5 C6 H6 120.1(18) . . ?
C1 C6 H6 117.8(18) . . ?
Ti2 C6 H6 132.8(18) . . ?
Ti1 C6 H6 124.5(18) . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 Ti1 81.00(16) . . ?
C4 C5 Ti1 71.91(15) . . ?
C6 C5 Ti2 65.99(14) . . ?
C4 C5 Ti2 70.81(15) . . ?
Ti1 C5 Ti2 105.21(11) . . ?
C6 C5 H5 121.2(16) . . ?
C4 C5 H5 116.4(16) . . ?
Ti1 C5 H5 133.6(16) . . ?
Ti2 C5 H5 120.9(16) . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 Ti1 70.56(15) . . ?
C3 C4 Ti1 79.57(16) . . ?
C5 C4 Ti2 73.39(15) . . ?
C3 C4 Ti2 66.37(15) . . ?
Ti1 C4 Ti2 105.76(11) . . ?
C5 C4 H4 117.8(17) . . ?
C3 C4 H4 121.5(17) . . ?
Ti1 C4 H4 129.4(17) . . ?
Ti2 C4 H4 124.7(17) . . ?
C4 C3 C2 116.2(2) . . ?
C4 C3 Ti2 76.38(15) . . ?
C2 C3 Ti2 79.52(15) . . ?
C4 C3 Ti1 64.78(14) . . ?
C2 C3 Ti1 65.20(14) . . ?
Ti2 C3 Ti1 103.63(10) . . ?
C4 C3 H3 118.9(16) . . ?
C2 C3 H3 118.6(16) . . ?
Ti2 C3 H3 137.8(16) . . ?
Ti1 C3 H3 118.5(16) . . ?
C1 C2 C3 120.7(2) . . ?
C1 C2 Ti1 75.07(15) . . ?
C3 C2 Ti1 79.14(16) . . ?
C1 C2 Ti2 71.32(14) . . ?
C3 C2 Ti2 63.99(14) . . ?
Ti1 C2 Ti2 103.04(11) . . ?
C1 C2 H2 118.6(17) . . ?
C3 C2 H2 117.9(16) . . ?
Ti1 C2 H2 133.7(16) . . ?
Ti2 C2 H2 123.3(16) . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C32 C33 118.1(3) . . ?
C37 C32 C38 121.4(3) . . ?
C33 C32 C38 120.4(3) . . ?
C37 C32 K1 80.34(17) . . ?
C33 C32 K1 73.05(17) . . ?
C38 C32 K1 120.1(2) . . ?
C34 C33 C32 120.8(3) . . ?
C34 C33 K1 77.25(18) . . ?
C32 C33 K1 82.52(18) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
K1 C33 H33 119.2 . . ?
C35 C34 C33 119.9(3) . . ?
C35 C34 K1 81.27(18) . . ?
C33 C34 K1 77.90(18) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
K1 C34 H34 119.7 . . ?
C34 C35 C36 119.6(3) . . ?
C34 C35 K1 74.53(18) . . ?
C36 C35 K1 81.48(19) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
K1 C35 H35 120.0 . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 K1 78.66(18) . . ?
C35 C36 K1 74.65(18) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
K1 C36 H36 117.5 . . ?
C32 C37 C36 121.6(3) . . ?
C32 C37 K1 76.25(17) . . ?
C36 C37 K1 77.93(18) . . ?
C32 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
K1 C37 H37 117.2 . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C40 C39 C44 117.4(3) . . ?
C40 C39 C45 121.4(3) . . ?
C44 C39 C45 121.2(3) . . ?
C43 C44 C39 121.1(3) . . ?
C43 C44 H44 119.4 . . ?
C39 C44 H44 119.4 . . ?
C42 C43 C44 120.2(4) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C42 C41 119.4(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C39 C40 C41 121.5(4) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 H40 119.3 . . ?
C46 C52 H52A 109.5 . . ?
C46 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C46 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C46 C47 120.4(11) . . ?
C51 C46 C52 121.4(11) . . ?
C47 C46 C52 118.1(12) . . ?
C46 C51 C50 123.8(12) . . ?
C46 C51 H51 118.1 . . ?
C50 C51 H51 118.1 . . ?
C49 C50 C51 114.5(13) . . ?
C49 C50 H50 122.8 . . ?
C51 C50 H50 122.8 . . ?
C50 C49 C48 122.1(12) . . ?
C50 C49 H49 119.0 . . ?
C48 C49 H49 119.0 . . ?
C47 C48 C49 122.5(15) . . ?
C47 C48 H48 118.7 . . ?
C49 C48 H48 118.7 . . ?
C48 C47 C46 116.6(16) . . ?
C48 C47 H47 121.7 . . ?
C46 C47 H47 121.7 . . ?

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
C13 Si2 N1 Si1 170.74(13) . . . . ?
C11 Si2 N1 Si1 -67.94(17) . . . . ?
C12 Si2 N1 Si1 55.32(17) . . . . ?
K1 Si2 N1 Si1 103.60(13) . . . . ?
C13 Si2 N1 Ti1 -28.35(15) . . . . ?
C11 Si2 N1 Ti1 92.96(14) . . . . ?
C12 Si2 N1 Ti1 -143.77(12) . . . . ?
K1 Si2 N1 Ti1 -95.50(10) . . . . ?
C13 Si2 N1 K1 67.14(11) . . . . ?
C11 Si2 N1 K1 -171.54(11) . . . . ?
C12 Si2 N1 K1 -48.28(12) . . . . ?
C8 Si1 N1 Si2 139.16(14) . . . . ?
C9 Si1 N1 Si2 19.18(18) . . . . ?
C10 Si1 N1 Si2 -98.57(15) . . . . ?
K1 Si1 N1 Si2 -99.60(13) . . . . ?
C8 Si1 N1 Ti1 -18.50(19) . . . . ?
C9 Si1 N1 Ti1 -138.48(15) . . . . ?
C10 Si1 N1 Ti1 103.77(16) . . . . ?
K1 Si1 N1 Ti1 102.74(14) . . . . ?
C8 Si1 N1 K1 -121.24(12) . . . . ?
C9 Si1 N1 K1 118.78(12) . . . . ?
C10 Si1 N1 K1 1.04(13) . . . . ?
C18 Si4 N2 Si3 144.65(13) . . . . ?
C17 Si4 N2 Si3 24.53(18) . . . . ?
C19 Si4 N2 Si3 -92.89(15) . . . . ?
K1 Si4 N2 Si3 -98.64(13) . . . . ?
C18 Si4 N2 Ti1 -15.75(19) . . . . ?
C17 Si4 N2 Ti1 -135.87(15) . . . . ?
C19 Si4 N2 Ti1 106.70(16) . . . . ?
K1 Si4 N2 Ti1 100.96(15) . . . . ?
C18 Si4 N2 K1 -116.71(11) . . . . ?
C17 Si4 N2 K1 123.17(12) . . . . ?
C19 Si4 N2 K1 5.74(13) . . . . ?
C15 Si3 N2 Si4 173.33(13) . . . . ?
C16 Si3 N2 Si4 -65.21(17) . . . . ?
C14 Si3 N2 Si4 57.07(16) . . . . ?
K1 Si3 N2 Si4 102.57(13) . . . . ?
C15 Si3 N2 Ti1 -23.25(15) . . . . ?
C16 Si3 N2 Ti1 98.21(14) . . . . ?
C14 Si3 N2 Ti1 -139.50(12) . . . . ?
K1 Si3 N2 Ti1 -94.01(10) . . . . ?
C15 Si3 N2 K1 70.76(11) . . . . ?
C16 Si3 N2 K1 -167.78(11) . . . . ?
C14 Si3 N2 K1 -45.49(12) . . . . ?
C20 Si5 N3 Si6 166.55(15) . . . . ?
C22 Si5 N3 Si6 -73.49(19) . . . . ?
C21 Si5 N3 Si6 48.0(2) . . . . ?
C20 Si5 N3 Ti2 -3.7(2) . . . . ?
C22 Si5 N3 Ti2 116.24(18) . . . . ?
C21 Si5 N3 Ti2 -122.3(2) . . . . ?
C25B Si6 N3 Si5 159.7(7) . . . . ?
C24B Si6 N3 Si5 -109.2(8) . . . . ?
C23A Si6 N3 Si5 35.4(5) . . . . ?
C23B Si6 N3 Si5 20.5(7) . . . . ?
C24A Si6 N3 Si5 -80.8(6) . . . . ?
C25A Si6 N3 Si5 133.0(6) . . . . ?
C25B Si6 N3 Ti2 -28.9(7) . . . . ?
C24B Si6 N3 Ti2 62.2(8) . . . . ?
C23A Si6 N3 Ti2 -153.2(5) . . . . ?
C23B Si6 N3 Ti2 -168.1(7) . . . . ?
C24A Si6 N3 Ti2 90.6(6) . . . . ?
C25A Si6 N3 Ti2 -55.6(6) . . . . ?
C31 Si8 N4 Si7 -156.38(14) . . . . ?
C29 Si8 N4 Si7 83.73(17) . . . . ?
C30 Si8 N4 Si7 -39.77(18) . . . . ?
C31 Si8 N4 Ti2 26.26(17) . . . . ?
C29 Si8 N4 Ti2 -93.62(16) . . . . ?
C30 Si8 N4 Ti2 142.88(14) . . . . ?
C28 Si7 N4 Si8 -161.27(15) . . . . ?
C27 Si7 N4 Si8 78.11(16) . . . . ?
C26 Si7 N4 Si8 -42.24(18) . . . . ?
C28 Si7 N4 Ti2 15.8(2) . . . . ?
C27 Si7 N4 Ti2 -104.81(16) . . . . ?
C26 Si7 N4 Ti2 134.84(15) . . . . ?
N1 Si2 C12 K1 40.88(10) . . . . ?
C13 Si2 C12 K1 -79.52(10) . . . . ?
C11 Si2 C12 K1 169.14(10) . . . . ?
N2 Si3 C14 K1 39.70(10) . . . . ?
C15 Si3 C14 K1 -79.27(10) . . . . ?
C16 Si3 C14 K1 167.76(10) . . . . ?
C2 C1 C6 C5 15.5(4) . . . . ?
C7 C1 C6 C5 -178.2(2) . . . . ?
Ti1 C1 C6 C5 -40.6(2) . . . . ?
Ti2 C1 C6 C5 68.4(2) . . . . ?
C2 C1 C6 Ti2 -52.9(2) . . . . ?
C7 C1 C6 Ti2 113.4(2) . . . . ?
Ti1 C1 C6 Ti2 -109.01(8) . . . . ?
C2 C1 C6 Ti1 56.1(2) . . . . ?
C7 C1 C6 Ti1 -137.6(2) . . . . ?
Ti2 C1 C6 Ti1 109.01(8) . . . . ?
C1 C6 C5 C4 -20.6(4) . . . . ?
Ti2 C6 C5 C4 48.1(2) . . . . ?
Ti1 C6 C5 C4 -63.1(2) . . . . ?
C1 C6 C5 Ti1 42.5(2) . . . . ?
Ti2 C6 C5 Ti1 111.18(9) . . . . ?
C1 C6 C5 Ti2 -68.7(2) . . . . ?
Ti1 C6 C5 Ti2 -111.18(9) . . . . ?
C6 C5 C4 C3 3.1(4) . . . . ?
Ti1 C5 C4 C3 -64.8(2) . . . . ?
Ti2 C5 C4 C3 49.1(2) . . . . ?
C6 C5 C4 Ti1 67.9(2) . . . . ?
Ti2 C5 C4 Ti1 113.94(9) . . . . ?
C6 C5 C4 Ti2 -46.0(2) . . . . ?
Ti1 C5 C4 Ti2 -113.94(9) . . . . ?
C5 C4 C3 C2 18.6(4) . . . . ?
Ti1 C4 C3 C2 -41.6(2) . . . . ?
Ti2 C4 C3 C2 70.9(2) . . . . ?
C5 C4 C3 Ti2 -52.2(2) . . . . ?
Ti1 C4 C3 Ti2 -112.46(9) . . . . ?
C5 C4 C3 Ti1 60.2(2) . . . . ?
Ti2 C4 C3 Ti1 112.46(9) . . . . ?
C6 C1 C2 C3 7.0(4) . . . . ?
C7 C1 C2 C3 -159.6(2) . . . . ?
Ti1 C1 C2 C3 67.3(2) . . . . ?
Ti2 C1 C2 C3 -42.3(2) . . . . ?
C6 C1 C2 Ti1 -60.4(2) . . . . ?
C7 C1 C2 Ti1 133.1(2) . . . . ?
Ti2 C1 C2 Ti1 -109.68(8) . . . . ?
C6 C1 C2 Ti2 49.3(2) . . . . ?
C7 C1 C2 Ti2 -117.2(2) . . . . ?
Ti1 C1 C2 Ti2 109.68(8) . . . . ?
C4 C3 C2 C1 -23.8(4) . . . . ?
Ti2 C3 C2 C1 45.2(2) . . . . ?
Ti1 C3 C2 C1 -65.2(2) . . . . ?
C4 C3 C2 Ti1 41.4(2) . . . . ?
Ti2 C3 C2 Ti1 110.45(9) . . . . ?
C4 C3 C2 Ti2 -69.0(2) . . . . ?
Ti1 C3 C2 Ti2 -110.45(9) . . . . ?
C37 C32 C33 C34 -1.5(4) . . . . ?
C38 C32 C33 C34 174.3(3) . . . . ?
K1 C32 C33 C34 -70.3(3) . . . . ?
C37 C32 C33 K1 68.8(3) . . . . ?
C38 C32 C33 K1 -115.5(3) . . . . ?
C32 C33 C34 C35 0.7(5) . . . . ?
K1 C33 C34 C35 -72.4(3) . . . . ?
C32 C33 C34 K1 73.1(3) . . . . ?
C33 C34 C35 C36 0.1(5) . . . . ?
K1 C34 C35 C36 -70.5(3) . . . . ?
C33 C34 C35 K1 70.6(3) . . . . ?
C34 C35 C36 C37 -0.1(5) . . . . ?
K1 C35 C36 C37 -66.8(3) . . . . ?
C34 C35 C36 K1 66.7(3) . . . . ?
C33 C32 C37 C36 1.5(4) . . . . ?
C38 C32 C37 C36 -174.2(3) . . . . ?
K1 C32 C37 C36 66.2(3) . . . . ?
C33 C32 C37 K1 -64.8(2) . . . . ?
C38 C32 C37 K1 119.5(3) . . . . ?
C35 C36 C37 C32 -0.7(5) . . . . ?
K1 C36 C37 C32 -65.4(3) . . . . ?
C35 C36 C37 K1 64.7(3) . . . . ?
C40 C39 C44 C43 1.0(5) . . . . ?
C45 C39 C44 C43 -178.3(3) . . . . ?
C39 C44 C43 C42 -0.5(6) . . . . ?
C44 C43 C42 C41 -0.6(6) . . . . ?
C43 C42 C41 C40 1.0(6) . . . . ?
C44 C39 C40 C41 -0.5(5) . . . . ?
C45 C39 C40 C41 178.8(3) . . . . ?
C42 C41 C40 C39 -0.5(6) . . . . ?
C47 C46 C51 C50 -6(5) . . . . ?
C52 C46 C51 C50 178(2) . . . . ?
C46 C51 C50 C49 3(4) . . . . ?
C51 C50 C49 C48 0(3) . . . . ?
C50 C49 C48 C47 0(3) . . . . ?
C49 C48 C47 C46 -3(4) . . . . ?
C51 C46 C47 C48 6(5) . . . . ?
C52 C46 C47 C48 -179(2) . . . . ?

_refine_diff_density_max         0.364
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.066

