# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_TiOPcPentyl4N
_database_code_depnum_ccdc_archive 'CCDC 1581401'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-02-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of titanyl phthalocyanine with tetrapentylammonium cations'
_chemical_formula_moiety         '2(C32 H16 N8 O Ti), 2(C20 H44 N)'
_chemical_formula_sum            'C104 H120 N18 O2 Ti2'
_chemical_formula_weight         1749.97
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
_chemical_oxdiff_formula         'C52 H60 N9 Ti1 O1'
_chemical_oxdiff_usercomment     TiOPc_TPA
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   11.8378(3)
_cell_length_b                   13.0103(3)
_cell_length_c                   16.5916(3)
_cell_angle_alpha                67.7290(19)
_cell_angle_beta                 71.634(2)
_cell_angle_gamma                78.1997(19)
_cell_volume                     2233.71(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    25883
_cell_measurement_temperature    116.95(10)
_cell_measurement_theta_max      32.6910
_cell_measurement_theta_min      1.8130
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             930
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0902
-4 2 5 0.0655
5 3 -4 0.1796
5 0 1 0.0851
0 -1 -1 0.1014
0 1 0 0.1153
0 -1 0 0.0824
-1 0 -1 0.1098

_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.198
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9989 0.0002 0.9988 -0.0531 -0.0430 -0.0061
-3.9937 1.9975 4.9924 -0.0572 0.2122 0.3246
4.9932 2.9956 -3.9932 0.2089 -0.3792 -0.1573
4.9939 0.0004 0.9995 -0.1093 -0.2550 -0.1330
-0.0003 -0.9987 -0.9987 -0.0019 0.0148 -0.0604
0.0001 0.9986 0.0001 0.0410 -0.0248 0.0347
-0.0001 -0.9986 -0.0001 -0.0410 0.0248 -0.0347
-0.9989 -0.0002 -0.9988 0.0531 0.0430 0.0061

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46042
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.821
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      116.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  97.00   1.00   40.00    --   20.14  77.00-150.00  111
  2  ω     -9.00  94.00   1.00   40.00    --   20.14  57.00  90.00  103
  3  ω     -1.00  95.00   1.00   40.00    --   20.14  37.00   0.00   96
  4  ω    -56.00  45.00   1.00   40.00    --   20.14 -37.00 -60.00  101
  5  ω    -25.00  62.00   1.00   40.00    --   20.14 -99.00  90.00   87
  6  ω     48.00 110.00   1.00   40.00    --   20.14 178.00-120.00   62
  7  ω    -52.00  50.00   1.00   40.00    --   20.14 -57.00-150.00  102
  8  ω    -80.00 -44.00   1.00   40.00    --  -20.45 128.00-131.95   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140689000
_diffrn_orient_matrix_UB_12      0.0410148000
_diffrn_orient_matrix_UB_13      -0.0391256000
_diffrn_orient_matrix_UB_21      -0.0530665000
_diffrn_orient_matrix_UB_22      -0.0248115000
_diffrn_orient_matrix_UB_23      0.0099832000
_diffrn_orient_matrix_UB_31      -0.0317750000
_diffrn_orient_matrix_UB_32      0.0347251000
_diffrn_orient_matrix_UB_33      0.0257157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                24196
_reflns_number_total             26916
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.391(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         26916
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.041
_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)+(0.0518P)²+0.2776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0963
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.609(14) 0.391(14)
2. 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
3. Shared sites
{C425, C411}
4. Others
 Sof(C422)=Sof(H42D)=Sof(H42E)=Sof(C423)=Sof(H42F)=Sof(H42G)=Sof(C421)=
 Sof(H42H)=Sof(H42I)=Sof(C424)=Sof(H42J)=Sof(H42K)=Sof(H42L)=Sof(C425)=1-FVAR(1)
 Sof(C411)=Sof(C412)=Sof(H41F)=Sof(H41G)=Sof(C413)=Sof(H41H)=Sof(H41I)=
 Sof(C414)=Sof(H41J)=Sof(H41K)=Sof(C415)=Sof(H41L)=Sof(H41M)=Sof(H41N)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C401(H40A,H40B), C402(H40C,H40D), C403(H40E,H40F), C404(H40G,H40H), C406(H40L,
 H40M), C407(H40N,H40O), C408(H40P,H40Q), C409(H40R,H40S), C411(H41D,H41E),
 C412(H41F,H41G), C413(H41H,H41I), C414(H41J,H41K), C416(H41O,H41P), C417(H41Q,
 H41R), C418(H41S,H41T), C419(H41U,H41V), C301(H30A,H30B), C302(H30C,H30D),
 C303(H30E,H30F), C304(H30G,H30H), C306(H30L,H30M), C307(H30N,H30O), C308(H30P,
 H30Q), C309(H30R,H30S), C311(H31D,H31E), C312(H31F,H31G), C313(H31H,H31I),
 C314(H31J,H31K), C316(H31O,H31P), C317(H31Q,H31R), C318(H31S,H31T), C319(H31U,
 H31V), C422(H42D,H42E), C423(H42F,H42G), C421(H42H,H42I)
5.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C217(H217), C218(H218),
 C219(H219), C220(H220), C221(H221), C222(H222), C223(H223), C224(H224),
 C225(H225), C226(H226), C227(H227), C228(H228), C229(H229), C230(H230),
 C231(H231), C232(H232)
5.c Idealised Me refined as rotating group:
 C405(H40I,H40J,H40K), C410(H41A,H41B,H41C), C415(H41L,H41M,H41N), C420(H42A,
 H42B,H42C), C305(H30I,H30J,H30K), C310(H31A,H31B,H31C), C315(H31L,H31M,H31N),
 C320(H32A,H32B,H32C), C424(H42J,H42K,H42L)
;
_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 0.99588(3) 0.18842(3) 0.74643(2) 0.01135(8) Uani 1 1 d . . . . .
O1 O 1.14096(16) 0.15097(16) 0.72174(13) 0.0189(4) Uani 1 1 d . . . . .
N101 N 0.96506(18) 0.30359(17) 0.81040(14) 0.0134(4) Uani 1 1 d . . . . .
N102 N 0.92412(18) 0.08019(17) 0.87355(14) 0.0123(4) Uani 1 1 d . . . . .
N103 N 0.91791(18) 0.09828(17) 0.70230(14) 0.0133(4) Uani 1 1 d . . . . .
N104 N 0.95937(18) 0.32309(18) 0.63765(14) 0.0140(4) Uani 1 1 d . . . . .
N105 N 0.92316(18) 0.18617(18) 0.96856(14) 0.0132(4) Uani 1 1 d . . . . .
N106 N 0.89433(18) -0.07264(17) 0.83266(14) 0.0132(4) Uani 1 1 d . . . . .
N107 N 0.91634(19) 0.22613(18) 0.55116(14) 0.0145(4) Uani 1 1 d . . . . .
N108 N 0.98377(19) 0.47582(18) 0.68130(15) 0.0156(4) Uani 1 1 d . . . . .
C101 C 0.9770(2) 0.4171(2) 0.76641(17) 0.0143(5) Uani 1 1 d . . . . .
C102 C 0.9682(2) 0.4685(2) 0.83264(17) 0.0146(5) Uani 1 1 d . . . . .
C103 C 0.9428(2) 0.3852(2) 0.91754(17) 0.0138(5) Uani 1 1 d . . . . .
C104 C 0.9431(2) 0.2822(2) 0.90266(16) 0.0126(4) Uani 1 1 d . . . . .
C105 C 0.9152(2) 0.0922(2) 0.95484(16) 0.0126(4) Uani 1 1 d . . . . .
C106 C 0.8935(2) -0.0120(2) 1.02603(16) 0.0119(4) Uani 1 1 d . . . . .
C107 C 0.8895(2) -0.0897(2) 0.98623(16) 0.0124(4) Uani 1 1 d . . . . .
C108 C 0.9054(2) -0.0286(2) 0.89112(16) 0.0120(4) Uani 1 1 d . . . . .
C109 C 0.8966(2) -0.0125(2) 0.74798(17) 0.0132(5) Uani 1 1 d . . . . .
C110 C 0.8727(2) -0.0571(2) 0.68696(16) 0.0141(5) Uani 1 1 d . . . . .
C111 C 0.8815(2) 0.0294(2) 0.60397(17) 0.0139(5) Uani 1 1 d . . . . .
C112 C 0.9080(2) 0.1279(2) 0.61469(16) 0.0134(5) Uani 1 1 d . . . . .
C113 C 0.9359(2) 0.3176(2) 0.56294(16) 0.0140(5) Uani 1 1 d . . . . .
C114 C 0.9340(2) 0.4277(2) 0.49722(17) 0.0150(5) Uani 1 1 d . . . . .
C115 C 0.9559(2) 0.5001(2) 0.53490(17) 0.0150(5) Uani 1 1 d . . . . .
C116 C 0.9701(2) 0.4324(2) 0.62288(17) 0.0145(5) Uani 1 1 d . . . . .
C117 C 0.9740(2) 0.5783(2) 0.82275(19) 0.0182(5) Uani 1 1 d . . . . .
H117 H 0.992571 0.632702 0.765958 0.022 Uiso 1 1 calc R . . . .
C118 C 0.9510(3) 0.6039(2) 0.90115(19) 0.0202(5) Uani 1 1 d . . . . .
H118 H 0.954628 0.676712 0.896651 0.024 Uiso 1 1 calc R . . . .
C119 C 0.9225(2) 0.5214(2) 0.98693(19) 0.0195(5) Uani 1 1 d . . . . .
H119 H 0.906617 0.540791 1.038182 0.023 Uiso 1 1 calc R . . . .
C120 C 0.9176(2) 0.4111(2) 0.99659(18) 0.0162(5) Uani 1 1 d . . . . .
H120 H 0.898452 0.356695 1.053316 0.019 Uiso 1 1 calc R . . . .
C121 C 0.8746(2) -0.0437(2) 1.11967(16) 0.0145(5) Uani 1 1 d . . . . .
H121 H 0.874435 0.007703 1.146249 0.017 Uiso 1 1 calc R . . . .
C122 C 0.8561(2) -0.1543(2) 1.17148(17) 0.0157(5) Uani 1 1 d . . . . .
H122 H 0.844833 -0.177660 1.233598 0.019 Uiso 1 1 calc R . . . .
C123 C 0.8542(2) -0.2316(2) 1.13113(17) 0.0155(5) Uani 1 1 d . . . . .
H123 H 0.842518 -0.305388 1.167187 0.019 Uiso 1 1 calc R . . . .
C124 C 0.8692(2) -0.2002(2) 1.03901(17) 0.0142(5) Uani 1 1 d . . . . .
H124 H 0.865830 -0.251235 1.013133 0.017 Uiso 1 1 calc R . . . .
C125 C 0.8446(2) -0.1619(2) 0.69922(18) 0.0176(5) Uani 1 1 d . . . . .
H125 H 0.836046 -0.218570 0.755018 0.021 Uiso 1 1 calc R . . . .
C126 C 0.8298(3) -0.1793(2) 0.62595(19) 0.0201(5) Uani 1 1 d . . . . .
H126 H 0.812431 -0.248976 0.632425 0.024 Uiso 1 1 calc R . . . .
C127 C 0.8406(2) -0.0931(2) 0.54184(18) 0.0200(5) Uani 1 1 d . . . . .
H127 H 0.830949 -0.107029 0.493520 0.024 Uiso 1 1 calc R . . . .
C128 C 0.8655(2) 0.0128(2) 0.52974(17) 0.0173(5) Uani 1 1 d . . . . .
H128 H 0.871180 0.070258 0.474529 0.021 Uiso 1 1 calc R . . . .
C129 C 0.9154(2) 0.4693(2) 0.41001(18) 0.0191(5) Uani 1 1 d . . . . .
H129 H 0.901160 0.422109 0.384648 0.023 Uiso 1 1 calc R . . . .
C130 C 0.9193(3) 0.5823(3) 0.36368(19) 0.0247(6) Uani 1 1 d . . . . .
H130 H 0.908095 0.611418 0.305871 0.030 Uiso 1 1 calc R . . . .
C131 C 0.9397(3) 0.6551(2) 0.4019(2) 0.0241(6) Uani 1 1 d . . . . .
H131 H 0.940801 0.730965 0.369028 0.029 Uiso 1 1 calc R . . . .
C132 C 0.9582(3) 0.6152(2) 0.48739(18) 0.0206(5) Uani 1 1 d . . . . .
H132 H 0.971660 0.663102 0.512470 0.025 Uiso 1 1 calc R . . . .
Ti2 Ti 0.54767(3) 0.03970(3) 0.17354(2) 0.01163(8) Uani 1 1 d . . . . .
O2 O 0.40253(16) 0.07604(16) 0.19398(13) 0.0188(4) Uani 1 1 d . . . . .
N201 N 0.61811(19) 0.13208(18) 0.22092(14) 0.0140(4) Uani 1 1 d . . . . .
N202 N 0.62281(18) 0.14741(17) 0.04736(14) 0.0133(4) Uani 1 1 d . . . . .
N203 N 0.58643(18) -0.07820(17) 0.11032(14) 0.0135(4) Uani 1 1 d . . . . .
N204 N 0.57853(19) -0.09203(18) 0.28481(14) 0.0143(4) Uani 1 1 d . . . . .
N205 N 0.64829(19) 0.30123(18) 0.08711(15) 0.0145(4) Uani 1 1 d . . . . .
N206 N 0.62636(18) 0.04286(18) -0.04803(14) 0.0133(4) Uani 1 1 d . . . . .
N207 N 0.56613(19) -0.24829(18) 0.24255(15) 0.0158(4) Uani 1 1 d . . . . .
N208 N 0.61088(19) 0.00379(18) 0.37515(14) 0.0156(4) Uani 1 1 d . . . . .
C201 C 0.6237(2) 0.1047(2) 0.30837(17) 0.0147(5) Uani 1 1 d . . . . .
C202 C 0.6519(2) 0.1992(2) 0.32009(18) 0.0150(5) Uani 1 1 d . . . . .
C203 C 0.6656(2) 0.2858(2) 0.23524(17) 0.0151(5) Uani 1 1 d . . . . .
C204 C 0.6436(2) 0.2422(2) 0.17460(17) 0.0135(5) Uani 1 1 d . . . . .
C205 C 0.6415(2) 0.2566(2) 0.02995(17) 0.0133(5) Uani 1 1 d . . . . .
C206 C 0.6582(2) 0.3177(2) -0.06664(16) 0.0130(5) Uani 1 1 d . . . . .
C207 C 0.6555(2) 0.2413(2) -0.10646(17) 0.0137(5) Uani 1 1 d . . . . .
C208 C 0.6333(2) 0.1340(2) -0.03367(16) 0.0124(4) Uani 1 1 d . . . . .
C209 C 0.6081(2) -0.0562(2) 0.01890(17) 0.0134(5) Uani 1 1 d . . . . .
C210 C 0.6065(2) -0.1589(2) 0.00409(17) 0.0137(5) Uani 1 1 d . . . . .
C211 C 0.5804(2) -0.2415(2) 0.09030(18) 0.0148(5) Uani 1 1 d . . . . .
C212 C 0.5730(2) -0.1901(2) 0.15485(17) 0.0141(5) Uani 1 1 d . . . . .
C213 C 0.5731(2) -0.2042(2) 0.29937(17) 0.0151(5) Uani 1 1 d . . . . .
C214 C 0.5837(2) -0.2700(2) 0.39048(17) 0.0167(5) Uani 1 1 d . . . . .
C215 C 0.5958(2) -0.1966(2) 0.43005(18) 0.0167(5) Uani 1 1 d . . . . .
C216 C 0.5940(2) -0.0850(2) 0.36211(17) 0.0149(5) Uani 1 1 d . . . . .
C217 C 0.6672(2) 0.2169(2) 0.39395(18) 0.0174(5) Uani 1 1 d . . . . .
H217 H 0.658764 0.160233 0.449727 0.021 Uiso 1 1 calc R . . . .
C218 C 0.6952(3) 0.3206(2) 0.3821(2) 0.0218(6) Uani 1 1 d . . . . .
H218 H 0.704112 0.333976 0.430834 0.026 Uiso 1 1 calc R . . . .
C219 C 0.7104(3) 0.4065(2) 0.2974(2) 0.0217(6) Uani 1 1 d . . . . .
H219 H 0.729717 0.475358 0.291309 0.026 Uiso 1 1 calc R . . . .
C220 C 0.6971(2) 0.3903(2) 0.22268(18) 0.0171(5) Uani 1 1 d . . . . .
H220 H 0.708623 0.446562 0.166579 0.020 Uiso 1 1 calc R . . . .
C221 C 0.6775(2) 0.4288(2) -0.11812(18) 0.0165(5) Uani 1 1 d . . . . .
H221 H 0.680120 0.479450 -0.091636 0.020 Uiso 1 1 calc R . . . .
C222 C 0.6927(2) 0.4606(2) -0.21059(18) 0.0185(5) Uani 1 1 d . . . . .
H222 H 0.704749 0.534338 -0.246645 0.022 Uiso 1 1 calc R . . . .
C223 C 0.6902(2) 0.3837(2) -0.25058(18) 0.0180(5) Uani 1 1 d . . . . .
H223 H 0.700567 0.407488 -0.312623 0.022 Uiso 1 1 calc R . . . .
C224 C 0.6725(2) 0.2728(2) -0.19936(17) 0.0157(5) Uani 1 1 d . . . . .
H224 H 0.671993 0.221639 -0.225981 0.019 Uiso 1 1 calc R . . . .
C225 C 0.6276(2) -0.1853(2) -0.07382(18) 0.0167(5) Uani 1 1 d . . . . .
H225 H 0.648231 -0.131828 -0.130913 0.020 Uiso 1 1 calc R . . . .
C226 C 0.6167(3) -0.2939(2) -0.06288(19) 0.0202(5) Uani 1 1 d . . . . .
H226 H 0.629146 -0.313216 -0.113761 0.024 Uiso 1 1 calc R . . . .
C227 C 0.5872(3) -0.3764(2) 0.0235(2) 0.0234(6) Uani 1 1 d . . . . .
H227 H 0.579457 -0.448459 0.028488 0.028 Uiso 1 1 calc R . . . .
C228 C 0.5698(2) -0.3512(2) 0.10003(19) 0.0186(5) Uani 1 1 d . . . . .
H228 H 0.551406 -0.405512 0.156878 0.022 Uiso 1 1 calc R . . . .
C229 C 0.5871(2) -0.3848(2) 0.43604(19) 0.0210(5) Uani 1 1 d . . . . .
H229 H 0.579092 -0.433529 0.409639 0.025 Uiso 1 1 calc R . . . .
C230 C 0.6029(3) -0.4234(3) 0.5227(2) 0.0260(6) Uani 1 1 d . . . . .
H230 H 0.605984 -0.499620 0.554819 0.031 Uiso 1 1 calc R . . . .
C231 C 0.6142(3) -0.3499(2) 0.56202(19) 0.0241(6) Uani 1 1 d . . . . .
H231 H 0.623978 -0.378197 0.620220 0.029 Uiso 1 1 calc R . . . .
C232 C 0.6112(2) -0.2349(2) 0.51642(18) 0.0201(5) Uani 1 1 d . . . . .
H232 H 0.619255 -0.186115 0.542821 0.024 Uiso 1 1 calc R . . . .
N4 N 0.24933(17) 0.24098(16) 0.35967(13) 0.0177(4) Uani 1 1 d . . . A 1
C401 C 0.2227(2) 0.3064(2) 0.42361(16) 0.0207(4) Uani 1 1 d . . . A 1
H40A H 0.181425 0.378294 0.397337 0.025 Uiso 1 1 calc R . . A 1
H40B H 0.167812 0.267078 0.479543 0.025 Uiso 1 1 calc R . . A 1
C402 C 0.3287(2) 0.3268(2) 0.44645(18) 0.0236(5) Uani 1 1 d . . . A 1
H40C H 0.373337 0.383303 0.395452 0.028 Uiso 1 1 calc R . . A 1
H40D H 0.381609 0.258625 0.460186 0.028 Uiso 1 1 calc R . . A 1
C403 C 0.2820(2) 0.3657(2) 0.52794(17) 0.0244(5) Uani 1 1 d . . . A 1
H40E H 0.225738 0.431373 0.514039 0.029 Uiso 1 1 calc R . . A 1
H40F H 0.238698 0.307711 0.578304 0.029 Uiso 1 1 calc R . . A 1
C404 C 0.3774(3) 0.3932(3) 0.5565(2) 0.0431(8) Uani 1 1 d . . . A 1
H40G H 0.414099 0.457582 0.509205 0.052 Uiso 1 1 calc R . . A 1
H40H H 0.438874 0.330936 0.563522 0.052 Uiso 1 1 calc R . . A 1
C405 C 0.3296(3) 0.4181(3) 0.6444(2) 0.0417(8) Uani 1 1 d . . . A 1
H40I H 0.272079 0.482412 0.636841 0.063 Uiso 1 1 calc GR . . A 1
H40J H 0.394514 0.432431 0.660521 0.063 Uiso 1 1 calc GR . . A 1
H40K H 0.292245 0.355093 0.691352 0.063 Uiso 1 1 calc GR . . A 1
C406 C 0.1324(2) 0.2474(2) 0.33720(16) 0.0202(4) Uani 1 1 d . . . A 1
H40L H 0.069047 0.232682 0.392872 0.024 Uiso 1 1 calc R . . A 1
H40M H 0.115020 0.323215 0.299113 0.024 Uiso 1 1 calc R . . A 1
C407 C 0.1285(2) 0.1685(2) 0.29018(19) 0.0227(5) Uani 1 1 d . . . A 1
H40N H 0.126561 0.092616 0.332326 0.027 Uiso 1 1 calc R . . A 1
H40O H 0.199685 0.171579 0.240555 0.027 Uiso 1 1 calc R . . A 1
C408 C 0.0171(3) 0.2024(2) 0.2545(2) 0.0227(5) Uani 1 1 d . . . A 1
H40P H 0.026056 0.273183 0.205254 0.027 Uiso 1 1 calc R . . A 1
H40Q H -0.052080 0.212804 0.302121 0.027 Uiso 1 1 calc R . . A 1
C409 C -0.0048(3) 0.1146(2) 0.22086(19) 0.0251(6) Uani 1 1 d . . . A 1
H40R H -0.063009 0.147325 0.185726 0.030 Uiso 1 1 calc R . . A 1
H40S H 0.069248 0.094405 0.181381 0.030 Uiso 1 1 calc R . . A 1
C410 C -0.0497(2) 0.0092(2) 0.29745(16) 0.0246(5) Uani 1 1 d . . . A 1
H41A H -0.055323 -0.044755 0.272666 0.037 Uiso 1 1 calc GR . . A 1
H41B H -0.127202 0.027308 0.333114 0.037 Uiso 1 1 calc GR . . A 1
H41C H 0.005004 -0.021148 0.334731 0.037 Uiso 1 1 calc GR . . A 1
C411 C 0.2953(2) 0.12027(19) 0.40254(17) 0.019(8) Uani 1 1 d . . . A 1
H41D H 0.320888 0.086187 0.356032 0.022 Uiso 1 1 calc R . . A 1
H41E H 0.366079 0.121241 0.419675 0.022 Uiso 1 1 calc R . . A 1
C412 C 0.2175(5) 0.0470(4) 0.4804(4) 0.0223(10) Uani 0.564(7) 1 d . . P A 1
H41F H 0.137014 0.062259 0.472852 0.027 Uiso 0.564(7) 1 calc R . P A 1
H41G H 0.214802 0.061950 0.534027 0.027 Uiso 0.564(7) 1 calc R . P A 1
C413 C 0.2608(5) -0.0756(4) 0.4930(3) 0.0250(11) Uani 0.564(7) 1 d . . P A 1
H41H H 0.266703 -0.088929 0.438023 0.030 Uiso 0.564(7) 1 calc R . P A 1
H41I H 0.340341 -0.090535 0.502138 0.030 Uiso 0.564(7) 1 calc R . P A 1
C414 C 0.1811(5) -0.1562(4) 0.5710(3) 0.0308(12) Uani 0.564(7) 1 d . . P A 1
H41J H 0.097278 -0.135595 0.572076 0.037 Uiso 0.564(7) 1 calc R . P A 1
H41K H 0.192643 -0.164662 0.628597 0.037 Uiso 0.564(7) 1 calc R . P A 1
C415 C 0.2305(9) -0.2591(6) 0.5443(7) 0.060(2) Uani 0.564(7) 1 d . . P A 1
H41L H 0.226194 -0.243961 0.484009 0.090 Uiso 0.564(7) 1 calc GR . P A 1
H41M H 0.184255 -0.319889 0.585155 0.090 Uiso 0.564(7) 1 calc GR . P A 1
H41N H 0.312293 -0.278570 0.546921 0.090 Uiso 0.564(7) 1 calc GR . P A 1
C422 C 0.2418(6) -0.0607(5) 0.5371(5) 0.0274(15) Uiso 0.436(7) 1 d . . P A -2
H42D H 0.327394 -0.072845 0.530300 0.033 Uiso 0.436(7) 1 calc R . P A -2
H42E H 0.202829 -0.089431 0.601106 0.033 Uiso 0.436(7) 1 calc R . P A -2
C423 C 0.2107(7) -0.1276(6) 0.4906(5) 0.0321(18) Uiso 0.436(7) 1 d . . P A -2
H42F H 0.267523 -0.122174 0.432682 0.038 Uiso 0.436(7) 1 calc R . P A -2
H42G H 0.130416 -0.105512 0.482770 0.038 Uiso 0.436(7) 1 calc R . P A -2
C421 C 0.2065(7) 0.0645(6) 0.5024(5) 0.0185(15) Uiso 0.436(7) 1 d . . P A -2
H42H H 0.212499 0.098231 0.543800 0.022 Uiso 0.436(7) 1 calc R . P A -2
H42I H 0.124332 0.078248 0.498616 0.022 Uiso 0.436(7) 1 calc R . P A -2
C424 C 0.2245(9) -0.2799(8) 0.5821(6) 0.033(2) Uiso 0.436(7) 1 d . . P A -2
H42J H 0.241341 -0.334981 0.553365 0.050 Uiso 0.436(7) 1 calc GR . P A -2
H42K H 0.150609 -0.292017 0.628463 0.050 Uiso 0.436(7) 1 calc GR . P A -2
H42L H 0.288061 -0.285746 0.608426 0.050 Uiso 0.436(7) 1 calc GR . P A -2
C416 C 0.3481(2) 0.2892(2) 0.27515(16) 0.0217(5) Uani 1 1 d . . . A 1
H41O H 0.365487 0.242755 0.237917 0.026 Uiso 1 1 calc R . . A 1
H41P H 0.419848 0.284335 0.293348 0.026 Uiso 1 1 calc R . . A 1
C417 C 0.3212(2) 0.4102(2) 0.21729(17) 0.0252(5) Uani 1 1 d . . . A 1
H41Q H 0.246427 0.441566 0.248472 0.030 Uiso 1 1 calc R . . A 1
H41R H 0.384031 0.453810 0.208725 0.030 Uiso 1 1 calc R . . A 1
C418 C 0.3122(3) 0.4175(3) 0.1256(2) 0.0395(8) Uani 1 1 d . . . A 1
H41S H 0.258654 0.364509 0.134704 0.047 Uiso 1 1 calc R . . A 1
H41T H 0.390517 0.396130 0.091451 0.047 Uiso 1 1 calc R . . A 1
C419 C 0.2671(4) 0.5339(3) 0.0703(2) 0.0487(9) Uani 1 1 d . . . A 1
H41U H 0.311074 0.588961 0.070579 0.058 Uiso 1 1 calc R . . A 1
H41V H 0.282615 0.537797 0.008259 0.058 Uiso 1 1 calc R . . A 1
C420 C 0.1345(4) 0.5621(3) 0.1067(3) 0.0585(11) Uani 1 1 d . . . A 1
H42A H 0.108910 0.632769 0.067118 0.088 Uiso 1 1 calc GR . . A 1
H42B H 0.119785 0.566154 0.165745 0.088 Uiso 1 1 calc GR . . A 1
H42C H 0.090878 0.505281 0.110173 0.088 Uiso 1 1 calc GR . . A 1
N3 N 0.28484(17) 0.98985(17) 0.93903(14) 0.0178(4) Uani 1 1 d . . . . .
C301 C 0.40829(19) 1.01253(19) 0.87496(15) 0.0183(4) Uani 1 1 d . . . . .
H30A H 0.444510 0.945644 0.860401 0.022 Uiso 1 1 calc R . . . .
H30B H 0.457068 1.025964 0.906580 0.022 Uiso 1 1 calc R . . . .
C302 C 0.4130(2) 1.1099(2) 0.78705(16) 0.0216(4) Uani 1 1 d . . . . .
H30C H 0.406644 1.179548 0.797559 0.026 Uiso 1 1 calc R . . . .
H30D H 0.346453 1.111864 0.763993 0.026 Uiso 1 1 calc R . . . .
C303 C 0.5319(3) 1.0962(3) 0.7177(2) 0.0278(6) Uani 1 1 d . . . . .
H30E H 0.545710 1.167480 0.669823 0.033 Uiso 1 1 calc R . . . .
H30F H 0.596230 1.076077 0.747051 0.033 Uiso 1 1 calc R . . . .
C304 C 0.5370(3) 1.0087(3) 0.6759(2) 0.0311(7) Uani 1 1 d . . . . .
H30G H 0.521693 0.937635 0.723877 0.037 Uiso 1 1 calc R . . . .
H30H H 0.617108 1.000367 0.638057 0.037 Uiso 1 1 calc R . . . .
C305 C 0.4478(3) 1.0364(3) 0.6194(2) 0.0364(7) Uani 1 1 d . . . . .
H30I H 0.451658 1.112321 0.579204 0.055 Uiso 1 1 calc GR . . . .
H30J H 0.368427 1.027015 0.658527 0.055 Uiso 1 1 calc GR . . . .
H30K H 0.467259 0.987373 0.584889 0.055 Uiso 1 1 calc GR . . . .
C306 C 0.3024(2) 0.9000(2) 1.02682(17) 0.0211(5) Uani 1 1 d . . . . .
H30L H 0.349092 0.835391 1.012938 0.025 Uiso 1 1 calc R . . . .
H30M H 0.348481 0.927958 1.051808 0.025 Uiso 1 1 calc R . . . .
C307 C 0.1872(2) 0.8625(2) 1.09854(17) 0.0286(5) Uani 1 1 d . . . . .
H30N H 0.138244 0.838174 1.073288 0.034 Uiso 1 1 calc R . . . .
H30O H 0.142687 0.925137 1.116568 0.034 Uiso 1 1 calc R . . . .
C308 C 0.2130(3) 0.7668(3) 1.18177(19) 0.0341(6) Uani 1 1 d . . . . .
H30P H 0.140600 0.729966 1.216136 0.041 Uiso 1 1 calc R . . . .
H30Q H 0.273153 0.712562 1.161528 0.041 Uiso 1 1 calc R . . . .
C309 C 0.2553(3) 0.8013(4) 1.2434(2) 0.0485(9) Uani 1 1 d . . . . .
H30R H 0.194150 0.852491 1.266913 0.058 Uiso 1 1 calc R . . . .
H30S H 0.326771 0.839791 1.209706 0.058 Uiso 1 1 calc R . . . .
C310 C 0.2829(4) 0.6985(5) 1.3223(2) 0.0825(18) Uani 1 1 d . . . . .
H31A H 0.349220 0.651788 1.299418 0.124 Uiso 1 1 calc GR . . . .
H31B H 0.214038 0.657299 1.352734 0.124 Uiso 1 1 calc GR . . . .
H31C H 0.302711 0.722355 1.363909 0.124 Uiso 1 1 calc GR . . . .
C311 C 0.2121(2) 0.94982(19) 0.89735(16) 0.0183(4) Uani 1 1 d . . . . .
H31D H 0.131366 0.942929 0.936301 0.022 Uiso 1 1 calc R . . . .
H31E H 0.207329 1.006374 0.839796 0.022 Uiso 1 1 calc R . . . .
C312 C 0.2613(2) 0.8390(2) 0.88225(19) 0.0250(5) Uani 1 1 d . . . . .
H31F H 0.251049 0.778971 0.939992 0.030 Uiso 1 1 calc R . . . .
H31G H 0.346216 0.839979 0.852574 0.030 Uiso 1 1 calc R . . . .
C313 C 0.1969(2) 0.8182(2) 0.82438(19) 0.0258(5) Uani 1 1 d . . . . .
H31H H 0.203772 0.880620 0.768193 0.031 Uiso 1 1 calc R . . . .
H31I H 0.112658 0.814376 0.855617 0.031 Uiso 1 1 calc R . . . .
C314 C 0.2468(3) 0.7103(2) 0.8031(2) 0.0301(6) Uani 1 1 d . . . . .
H31J H 0.239881 0.648012 0.859443 0.036 Uiso 1 1 calc R . . . .
H31K H 0.198460 0.698986 0.770192 0.036 Uiso 1 1 calc R . . . .
C315 C 0.3765(3) 0.7100(3) 0.7482(3) 0.0469(9) Uani 1 1 d . . . . .
H31L H 0.386892 0.777713 0.697213 0.070 Uiso 1 1 calc GR . . . .
H31M H 0.397524 0.647179 0.727642 0.070 Uiso 1 1 calc GR . . . .
H31N H 0.427016 0.704906 0.785171 0.070 Uiso 1 1 calc GR . . . .
C316 C 0.2185(2) 1.0958(2) 0.95516(17) 0.0201(4) Uani 1 1 d . . . . .
H31O H 0.138533 1.079984 0.993219 0.024 Uiso 1 1 calc R . . . .
H31P H 0.210546 1.150891 0.897761 0.024 Uiso 1 1 calc R . . . .
C317 C 0.2775(2) 1.1459(2) 0.99905(18) 0.0235(5) Uani 1 1 d . . . . .
H31Q H 0.360324 1.155108 0.965101 0.028 Uiso 1 1 calc R . . . .
H31R H 0.276289 1.095908 1.059952 0.028 Uiso 1 1 calc R . . . .
C318 C 0.2112(2) 1.2600(2) 1.00180(18) 0.0245(5) Uani 1 1 d . . . . .
H31S H 0.125939 1.252774 1.023206 0.029 Uiso 1 1 calc R . . . .
H31T H 0.233539 1.279346 1.045339 0.029 Uiso 1 1 calc R . . . .
C319 C 0.2352(2) 1.3557(2) 0.91175(19) 0.0247(5) Uani 1 1 d . . . . .
H31U H 0.217761 1.334836 0.866991 0.030 Uiso 1 1 calc R . . . .
H31V H 0.181218 1.420727 0.918346 0.030 Uiso 1 1 calc R . . . .
C320 C 0.3632(2) 1.3870(3) 0.8775(2) 0.0346(6) Uani 1 1 d . . . . .
H32A H 0.370774 1.451015 0.823333 0.052 Uiso 1 1 calc GR . . . .
H32B H 0.416887 1.325547 0.864882 0.052 Uiso 1 1 calc GR . . . .
H32C H 0.382771 1.404153 0.922646 0.052 Uiso 1 1 calc GR . . . .


_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 O1 1.6494(18) . ?
Ti1 N101 2.060(2) . ?
Ti1 N102 2.064(2) . ?
Ti1 N103 2.069(2) . ?
Ti1 N104 2.073(2) . ?
N101 C101 1.392(3) . ?
N101 C104 1.394(3) . ?
N102 C105 1.385(3) . ?
N102 C108 1.383(3) . ?
N103 C109 1.385(3) . ?
N103 C112 1.393(3) . ?
N104 C113 1.383(3) . ?
N104 C116 1.375(3) . ?
N105 C104 1.317(3) . ?
N105 C105 1.351(3) . ?
N106 C108 1.348(3) . ?
N106 C109 1.318(3) . ?
N107 C112 1.311(3) . ?
N107 C113 1.350(3) . ?
N108 C101 1.312(3) . ?
N108 C116 1.355(3) . ?
C101 C102 1.457(3) . ?
C102 C103 1.400(4) . ?
C102 C117 1.388(4) . ?
C103 C104 1.451(3) . ?
C103 C120 1.404(4) . ?
C105 C106 1.428(4) . ?
C106 C107 1.416(3) . ?
C106 C121 1.402(3) . ?
C107 C108 1.442(3) . ?
C107 C124 1.394(4) . ?
C109 C110 1.460(3) . ?
C110 C111 1.398(4) . ?
C110 C125 1.395(4) . ?
C111 C112 1.464(4) . ?
C111 C128 1.402(4) . ?
C113 C114 1.435(4) . ?
C114 C115 1.412(4) . ?
C114 C129 1.412(4) . ?
C115 C116 1.433(4) . ?
C115 C132 1.406(4) . ?
C117 H117 0.9300 . ?
C117 C118 1.395(4) . ?
C118 H118 0.9300 . ?
C118 C119 1.407(4) . ?
C119 H119 0.9300 . ?
C119 C120 1.393(4) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.389(4) . ?
C122 H122 0.9300 . ?
C122 C123 1.411(4) . ?
C123 H123 0.9300 . ?
C123 C124 1.385(3) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.385(4) . ?
C126 H126 0.9300 . ?
C126 C127 1.407(4) . ?
C127 H127 0.9300 . ?
C127 C128 1.395(4) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.380(4) . ?
C130 H130 0.9300 . ?
C130 C131 1.415(4) . ?
C131 H131 0.9300 . ?
C131 C132 1.386(4) . ?
C132 H132 0.9300 . ?
Ti2 O2 1.6470(18) . ?
Ti2 N201 2.073(2) . ?
Ti2 N202 2.062(2) . ?
Ti2 N203 2.072(2) . ?
Ti2 N204 2.061(2) . ?
N201 C201 1.377(3) . ?
N201 C204 1.390(3) . ?
N202 C205 1.389(3) . ?
N202 C208 1.385(3) . ?
N203 C209 1.380(3) . ?
N203 C212 1.377(3) . ?
N204 C213 1.397(3) . ?
N204 C216 1.389(3) . ?
N205 C204 1.350(3) . ?
N205 C205 1.314(3) . ?
N206 C208 1.318(3) . ?
N206 C209 1.348(3) . ?
N207 C212 1.346(3) . ?
N207 C213 1.305(3) . ?
N208 C201 1.359(3) . ?
N208 C216 1.316(3) . ?
C201 C202 1.432(4) . ?
C202 C203 1.417(4) . ?
C202 C217 1.400(4) . ?
C203 C204 1.435(3) . ?
C203 C220 1.405(4) . ?
C205 C206 1.462(3) . ?
C206 C207 1.395(3) . ?
C206 C221 1.396(4) . ?
C207 C208 1.466(4) . ?
C207 C224 1.394(4) . ?
C209 C210 1.452(3) . ?
C210 C211 1.410(4) . ?
C210 C225 1.396(4) . ?
C211 C212 1.436(4) . ?
C211 C228 1.401(4) . ?
C213 C214 1.459(4) . ?
C214 C215 1.398(4) . ?
C214 C229 1.393(4) . ?
C215 C216 1.464(4) . ?
C215 C232 1.386(4) . ?
C217 H217 0.9300 . ?
C217 C218 1.381(4) . ?
C218 H218 0.9300 . ?
C218 C219 1.410(4) . ?
C219 H219 0.9300 . ?
C219 C220 1.393(4) . ?
C220 H220 0.9300 . ?
C221 H221 0.9300 . ?
C221 C222 1.390(4) . ?
C222 H222 0.9300 . ?
C222 C223 1.404(4) . ?
C223 H223 0.9300 . ?
C223 C224 1.389(4) . ?
C224 H224 0.9300 . ?
C225 H225 0.9300 . ?
C225 C226 1.383(4) . ?
C226 H226 0.9300 . ?
C226 C227 1.414(4) . ?
C227 H227 0.9300 . ?
C227 C228 1.374(4) . ?
C228 H228 0.9300 . ?
C229 H229 0.9300 . ?
C229 C230 1.392(4) . ?
C230 H230 0.9300 . ?
C230 C231 1.392(4) . ?
C231 H231 0.9300 . ?
C231 C232 1.397(4) . ?
C232 H232 0.9300 . ?
N4 C401 1.521(3) . ?
N4 C406 1.521(3) . ?
N4 C411 1.522(3) . ?
N4 C416 1.526(3) . ?
C401 H40A 0.9700 . ?
C401 H40B 0.9700 . ?
C401 C402 1.517(4) . ?
C402 H40C 0.9700 . ?
C402 H40D 0.9700 . ?
C402 C403 1.524(3) . ?
C403 H40E 0.9700 . ?
C403 H40F 0.9700 . ?
C403 C404 1.503(4) . ?
C404 H40G 0.9700 . ?
C404 H40H 0.9700 . ?
C404 C405 1.522(4) . ?
C405 H40I 0.9600 . ?
C405 H40J 0.9600 . ?
C405 H40K 0.9600 . ?
C406 H40L 0.9700 . ?
C406 H40M 0.9700 . ?
C406 C407 1.521(3) . ?
C407 H40N 0.9700 . ?
C407 H40O 0.9700 . ?
C407 C408 1.531(4) . ?
C408 H40P 0.9700 . ?
C408 H40Q 0.9700 . ?
C408 C409 1.542(4) . ?
C409 H40R 0.9700 . ?
C409 H40S 0.9700 . ?
C409 C410 1.526(4) . ?
C410 H41A 0.9600 . ?
C410 H41B 0.9600 . ?
C410 H41C 0.9600 . ?
C411 H41D 0.9700 . ?
C411 H41E 0.9700 . ?
C411 C412 1.450(6) . ?
C412 H41F 0.9700 . ?
C412 H41G 0.9700 . ?
C412 C413 1.528(7) . ?
C413 H41H 0.9700 . ?
C413 H41I 0.9700 . ?
C413 C414 1.507(7) . ?
C414 H41J 0.9700 . ?
C414 H41K 0.9700 . ?
C414 C415 1.514(9) . ?
C415 H41L 0.9600 . ?
C415 H41M 0.9600 . ?
C415 H41N 0.9600 . ?
C416 H41O 0.9700 . ?
C416 H41P 0.9700 . ?
C416 C417 1.531(4) . ?
C417 H41Q 0.9700 . ?
C417 H41R 0.9700 . ?
C417 C418 1.523(4) . ?
C418 H41S 0.9700 . ?
C418 H41T 0.9700 . ?
C418 C419 1.532(4) . ?
C419 H41U 0.9700 . ?
C419 H41V 0.9700 . ?
C419 C420 1.515(5) . ?
C420 H42A 0.9600 . ?
C420 H42B 0.9600 . ?
C420 H42C 0.9600 . ?
N3 C301 1.521(3) . ?
N3 C306 1.527(3) . ?
N3 C311 1.524(3) . ?
N3 C316 1.514(3) . ?
C301 H30A 0.9700 . ?
C301 H30B 0.9700 . ?
C301 C302 1.521(3) . ?
C302 H30C 0.9700 . ?
C302 H30D 0.9700 . ?
C302 C303 1.539(4) . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C304 1.524(5) . ?
C304 H30G 0.9700 . ?
C304 H30H 0.9700 . ?
C304 C305 1.529(5) . ?
C305 H30I 0.9600 . ?
C305 H30J 0.9600 . ?
C305 H30K 0.9600 . ?
C306 H30L 0.9700 . ?
C306 H30M 0.9700 . ?
C306 C307 1.524(4) . ?
C307 H30N 0.9700 . ?
C307 H30O 0.9700 . ?
C307 C308 1.535(4) . ?
C308 H30P 0.9700 . ?
C308 H30Q 0.9700 . ?
C308 C309 1.505(5) . ?
C309 H30R 0.9700 . ?
C309 H30S 0.9700 . ?
C309 C310 1.540(6) . ?
C310 H31A 0.9600 . ?
C310 H31B 0.9600 . ?
C310 H31C 0.9600 . ?
C311 H31D 0.9700 . ?
C311 H31E 0.9700 . ?
C311 C312 1.523(3) . ?
C312 H31F 0.9700 . ?
C312 H31G 0.9700 . ?
C312 C313 1.523(4) . ?
C313 H31H 0.9700 . ?
C313 H31I 0.9700 . ?
C313 C314 1.532(4) . ?
C314 H31J 0.9700 . ?
C314 H31K 0.9700 . ?
C314 C315 1.518(4) . ?
C315 H31L 0.9600 . ?
C315 H31M 0.9600 . ?
C315 H31N 0.9600 . ?
C316 H31O 0.9700 . ?
C316 H31P 0.9700 . ?
C316 C317 1.521(3) . ?
C317 H31Q 0.9700 . ?
C317 H31R 0.9700 . ?
C317 C318 1.540(3) . ?
C318 H31S 0.9700 . ?
C318 H31T 0.9700 . ?
C318 C319 1.527(4) . ?
C319 H31U 0.9700 . ?
C319 H31V 0.9700 . ?
C319 C320 1.523(4) . ?
C320 H32A 0.9600 . ?
C320 H32B 0.9600 . ?
C320 H32C 0.9600 . ?
C422 H42D 0.9700 . ?
C422 H42E 0.9700 . ?
C422 C423 1.519(10) . ?
C422 C421 1.524(9) . ?
C423 H42F 0.9700 . ?
C423 H42G 0.9700 . ?
C423 C424 2.000(12) . ?
C421 H42H 0.9700 . ?
C421 H42I 0.9700 . ?
C421 C425 1.637(8) . ?
C424 H42J 0.9600 . ?
C424 H42K 0.9600 . ?
C424 H42L 0.9600 . ?

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
O1 Ti1 N101 107.75(9) . . ?
O1 Ti1 N102 106.49(9) . . ?
O1 Ti1 N103 106.93(9) . . ?
O1 Ti1 N104 108.02(9) . . ?
N101 Ti1 N102 84.76(8) . . ?
N101 Ti1 N103 145.31(8) . . ?
N101 Ti1 N104 85.34(8) . . ?
N102 Ti1 N103 84.67(8) . . ?
N102 Ti1 N104 145.49(8) . . ?
N103 Ti1 N104 84.93(8) . . ?
C101 N101 Ti1 124.65(17) . . ?
C101 N101 C104 107.7(2) . . ?
C104 N101 Ti1 127.23(17) . . ?
C105 N102 Ti1 126.25(17) . . ?
C108 N102 Ti1 123.93(16) . . ?
C108 N102 C105 108.0(2) . . ?
C109 N103 Ti1 124.02(17) . . ?
C109 N103 C112 108.8(2) . . ?
C112 N103 Ti1 125.30(17) . . ?
C113 N104 Ti1 126.14(17) . . ?
C116 N104 Ti1 124.75(17) . . ?
C116 N104 C113 108.6(2) . . ?
C104 N105 C105 123.0(2) . . ?
C109 N106 C108 122.5(2) . . ?
C112 N107 C113 123.2(2) . . ?
C101 N108 C116 122.7(2) . . ?
N101 C101 C102 109.1(2) . . ?
N108 C101 N101 128.4(2) . . ?
N108 C101 C102 122.2(2) . . ?
C103 C102 C101 106.8(2) . . ?
C117 C102 C101 131.1(2) . . ?
C117 C102 C103 121.9(2) . . ?
C102 C103 C104 107.1(2) . . ?
C102 C103 C120 120.6(2) . . ?
C120 C103 C104 132.2(2) . . ?
N101 C104 C103 109.2(2) . . ?
N105 C104 N101 127.6(2) . . ?
N105 C104 C103 123.3(2) . . ?
N102 C105 C106 109.4(2) . . ?
N105 C105 N102 127.4(2) . . ?
N105 C105 C106 123.2(2) . . ?
C107 C106 C105 107.1(2) . . ?
C121 C106 C105 132.1(2) . . ?
C121 C106 C107 120.8(2) . . ?
C106 C107 C108 106.3(2) . . ?
C124 C107 C106 120.8(2) . . ?
C124 C107 C108 132.9(2) . . ?
N102 C108 C107 109.2(2) . . ?
N106 C108 N102 127.4(2) . . ?
N106 C108 C107 123.2(2) . . ?
N103 C109 C110 108.8(2) . . ?
N106 C109 N103 128.5(2) . . ?
N106 C109 C110 122.6(2) . . ?
C111 C110 C109 106.9(2) . . ?
C125 C110 C109 132.0(2) . . ?
C125 C110 C111 121.0(2) . . ?
C110 C111 C112 107.2(2) . . ?
C110 C111 C128 121.2(2) . . ?
C128 C111 C112 131.6(2) . . ?
N103 C112 C111 108.2(2) . . ?
N107 C112 N103 128.0(2) . . ?
N107 C112 C111 123.7(2) . . ?
N104 C113 C114 108.7(2) . . ?
N107 C113 N104 127.4(2) . . ?
N107 C113 C114 123.9(2) . . ?
C115 C114 C113 106.9(2) . . ?
C129 C114 C113 132.5(2) . . ?
C129 C114 C115 120.6(2) . . ?
C114 C115 C116 106.6(2) . . ?
C132 C115 C114 121.1(2) . . ?
C132 C115 C116 132.3(3) . . ?
N104 C116 C115 109.2(2) . . ?
N108 C116 N104 127.9(2) . . ?
N108 C116 C115 122.7(2) . . ?
C102 C117 H117 121.2 . . ?
C102 C117 C118 117.5(3) . . ?
C118 C117 H117 121.2 . . ?
C117 C118 H118 119.5 . . ?
C117 C118 C119 121.0(3) . . ?
C119 C118 H118 119.5 . . ?
C118 C119 H119 119.4 . . ?
C120 C119 C118 121.3(2) . . ?
C120 C119 H119 119.4 . . ?
C103 C120 H120 121.2 . . ?
C119 C120 C103 117.6(2) . . ?
C119 C120 H120 121.2 . . ?
C106 C121 H121 121.0 . . ?
C122 C121 C106 117.9(2) . . ?
C122 C121 H121 121.0 . . ?
C121 C122 H122 119.6 . . ?
C121 C122 C123 120.9(2) . . ?
C123 C122 H122 119.6 . . ?
C122 C123 H123 119.2 . . ?
C124 C123 C122 121.5(2) . . ?
C124 C123 H123 119.2 . . ?
C107 C124 H124 121.0 . . ?
C123 C124 C107 118.1(2) . . ?
C123 C124 H124 121.0 . . ?
C110 C125 H125 120.9 . . ?
C126 C125 C110 118.1(3) . . ?
C126 C125 H125 120.9 . . ?
C125 C126 H126 119.5 . . ?
C125 C126 C127 121.1(3) . . ?
C127 C126 H126 119.5 . . ?
C126 C127 H127 119.4 . . ?
C128 C127 C126 121.1(2) . . ?
C128 C127 H127 119.4 . . ?
C111 C128 H128 121.3 . . ?
C127 C128 C111 117.5(2) . . ?
C127 C128 H128 121.3 . . ?
C114 C129 H129 121.1 . . ?
C130 C129 C114 117.7(3) . . ?
C130 C129 H129 121.1 . . ?
C129 C130 H130 119.2 . . ?
C129 C130 C131 121.7(3) . . ?
C131 C130 H130 119.2 . . ?
C130 C131 H131 119.4 . . ?
C132 C131 C130 121.2(3) . . ?
C132 C131 H131 119.4 . . ?
C115 C132 H132 121.1 . . ?
C131 C132 C115 117.7(3) . . ?
C131 C132 H132 121.1 . . ?
O2 Ti2 N201 106.69(9) . . ?
O2 Ti2 N202 106.23(9) . . ?
O2 Ti2 N203 108.00(9) . . ?
O2 Ti2 N204 107.56(9) . . ?
N202 Ti2 N201 85.01(8) . . ?
N202 Ti2 N203 85.02(8) . . ?
N203 Ti2 N201 145.31(8) . . ?
N204 Ti2 N201 84.64(9) . . ?
N204 Ti2 N202 146.21(8) . . ?
N204 Ti2 N203 85.45(8) . . ?
C201 N201 Ti2 125.95(18) . . ?
C201 N201 C204 108.1(2) . . ?
C204 N201 Ti2 124.66(17) . . ?
C205 N202 Ti2 124.14(16) . . ?
C208 N202 Ti2 125.31(17) . . ?
C208 N202 C205 108.6(2) . . ?
C209 N203 Ti2 125.98(17) . . ?
C212 N203 Ti2 124.29(17) . . ?
C212 N203 C209 108.8(2) . . ?
C213 N204 Ti2 124.93(17) . . ?
C216 N204 Ti2 126.55(17) . . ?
C216 N204 C213 108.1(2) . . ?
C205 N205 C204 123.2(2) . . ?
C208 N206 C209 122.7(2) . . ?
C213 N207 C212 123.4(2) . . ?
C216 N208 C201 122.5(2) . . ?
N201 C201 C202 109.7(2) . . ?
N208 C201 N201 127.6(2) . . ?
N208 C201 C202 122.7(2) . . ?
C203 C202 C201 106.4(2) . . ?
C217 C202 C201 133.2(3) . . ?
C217 C202 C203 120.4(2) . . ?
C202 C203 C204 107.0(2) . . ?
C220 C203 C202 121.0(2) . . ?
C220 C203 C204 132.0(2) . . ?
N201 C204 C203 108.8(2) . . ?
N205 C204 N201 127.1(2) . . ?
N205 C204 C203 124.0(2) . . ?
N202 C205 C206 108.6(2) . . ?
N205 C205 N202 128.0(2) . . ?
N205 C205 C206 123.3(2) . . ?
C207 C206 C205 107.0(2) . . ?
C207 C206 C221 121.4(2) . . ?
C221 C206 C205 131.5(2) . . ?
C206 C207 C208 107.0(2) . . ?
C224 C207 C206 121.4(2) . . ?
C224 C207 C208 131.7(2) . . ?
N202 C208 C207 108.6(2) . . ?
N206 C208 N202 128.5(2) . . ?
N206 C208 C207 122.9(2) . . ?
N203 C209 C210 108.8(2) . . ?
N206 C209 N203 127.6(2) . . ?
N206 C209 C210 123.6(2) . . ?
C211 C210 C209 106.2(2) . . ?
C225 C210 C209 132.9(2) . . ?
C225 C210 C211 120.9(2) . . ?
C210 C211 C212 107.2(2) . . ?
C228 C211 C210 120.7(2) . . ?
C228 C211 C212 132.0(2) . . ?
N203 C212 C211 108.9(2) . . ?
N207 C212 N203 127.7(2) . . ?
N207 C212 C211 123.1(2) . . ?
N204 C213 C214 108.5(2) . . ?
N207 C213 N204 128.2(2) . . ?
N207 C213 C214 123.2(2) . . ?
C215 C214 C213 107.7(2) . . ?
C229 C214 C213 130.9(3) . . ?
C229 C214 C215 121.4(2) . . ?
C214 C215 C216 106.5(2) . . ?
C232 C215 C214 121.4(2) . . ?
C232 C215 C216 132.0(3) . . ?
N204 C216 C215 109.2(2) . . ?
N208 C216 N204 128.1(2) . . ?
N208 C216 C215 122.6(2) . . ?
C202 C217 H217 120.8 . . ?
C218 C217 C202 118.4(3) . . ?
C218 C217 H217 120.8 . . ?
C217 C218 H218 119.4 . . ?
C217 C218 C219 121.3(3) . . ?
C219 C218 H218 119.4 . . ?
C218 C219 H219 119.4 . . ?
C220 C219 C218 121.3(3) . . ?
C220 C219 H219 119.4 . . ?
C203 C220 H220 121.2 . . ?
C219 C220 C203 117.5(3) . . ?
C219 C220 H220 121.2 . . ?
C206 C221 H221 121.4 . . ?
C222 C221 C206 117.3(2) . . ?
C222 C221 H221 121.4 . . ?
C221 C222 H222 119.4 . . ?
C221 C222 C223 121.3(3) . . ?
C223 C222 H222 119.4 . . ?
C222 C223 H223 119.3 . . ?
C224 C223 C222 121.3(2) . . ?
C224 C223 H223 119.3 . . ?
C207 C224 H224 121.3 . . ?
C223 C224 C207 117.4(2) . . ?
C223 C224 H224 121.3 . . ?
C210 C225 H225 121.3 . . ?
C226 C225 C210 117.5(3) . . ?
C226 C225 H225 121.3 . . ?
C225 C226 H226 119.1 . . ?
C225 C226 C227 121.9(3) . . ?
C227 C226 H226 119.1 . . ?
C226 C227 H227 119.7 . . ?
C228 C227 C226 120.6(3) . . ?
C228 C227 H227 119.7 . . ?
C211 C228 H228 120.8 . . ?
C227 C228 C211 118.3(3) . . ?
C227 C228 H228 120.8 . . ?
C214 C229 H229 121.4 . . ?
C230 C229 C214 117.3(3) . . ?
C230 C229 H229 121.4 . . ?
C229 C230 H230 119.5 . . ?
C229 C230 C231 121.1(3) . . ?
C231 C230 H230 119.5 . . ?
C230 C231 H231 119.1 . . ?
C230 C231 C232 121.8(3) . . ?
C232 C231 H231 119.1 . . ?
C215 C232 C231 117.0(3) . . ?
C215 C232 H232 121.5 . . ?
C231 C232 H232 121.5 . . ?
C401 N4 C406 106.20(17) . . ?
C401 N4 C411 111.52(18) . . ?
C401 N4 C416 110.95(18) . . ?
C406 N4 C411 110.88(17) . . ?
C406 N4 C416 111.74(18) . . ?
C411 N4 C416 105.66(17) . . ?
N4 C401 H40A 108.1 . . ?
N4 C401 H40B 108.1 . . ?
H40A C401 H40B 107.3 . . ?
C402 C401 N4 116.9(2) . . ?
C402 C401 H40A 108.1 . . ?
C402 C401 H40B 108.1 . . ?
C401 C402 H40C 110.0 . . ?
C401 C402 H40D 110.0 . . ?
C401 C402 C403 108.4(2) . . ?
H40C C402 H40D 108.4 . . ?
C403 C402 H40C 110.0 . . ?
C403 C402 H40D 110.0 . . ?
C402 C403 H40E 108.7 . . ?
C402 C403 H40F 108.7 . . ?
H40E C403 H40F 107.6 . . ?
C404 C403 C402 114.4(2) . . ?
C404 C403 H40E 108.7 . . ?
C404 C403 H40F 108.7 . . ?
C403 C404 H40G 109.0 . . ?
C403 C404 H40H 109.0 . . ?
C403 C404 C405 113.0(3) . . ?
H40G C404 H40H 107.8 . . ?
C405 C404 H40G 109.0 . . ?
C405 C404 H40H 109.0 . . ?
C404 C405 H40I 109.5 . . ?
C404 C405 H40J 109.5 . . ?
C404 C405 H40K 109.5 . . ?
H40I C405 H40J 109.5 . . ?
H40I C405 H40K 109.5 . . ?
H40J C405 H40K 109.5 . . ?
N4 C406 H40L 108.2 . . ?
N4 C406 H40M 108.2 . . ?
H40L C406 H40M 107.4 . . ?
C407 C406 N4 116.27(19) . . ?
C407 C406 H40L 108.2 . . ?
C407 C406 H40M 108.2 . . ?
C406 C407 H40N 109.8 . . ?
C406 C407 H40O 109.8 . . ?
C406 C407 C408 109.5(2) . . ?
H40N C407 H40O 108.2 . . ?
C408 C407 H40N 109.8 . . ?
C408 C407 H40O 109.8 . . ?
C407 C408 H40P 109.1 . . ?
C407 C408 H40Q 109.1 . . ?
C407 C408 C409 112.3(2) . . ?
H40P C408 H40Q 107.9 . . ?
C409 C408 H40P 109.1 . . ?
C409 C408 H40Q 109.1 . . ?
C408 C409 H40R 109.0 . . ?
C408 C409 H40S 109.0 . . ?
H40R C409 H40S 107.8 . . ?
C410 C409 C408 113.1(2) . . ?
C410 C409 H40R 109.0 . . ?
C410 C409 H40S 109.0 . . ?
C409 C410 H41A 109.5 . . ?
C409 C410 H41B 109.5 . . ?
C409 C410 H41C 109.5 . . ?
H41A C410 H41B 109.5 . . ?
H41A C410 H41C 109.5 . . ?
H41B C410 H41C 109.5 . . ?
N4 C411 H41D 107.4 . . ?
N4 C411 H41E 107.4 . . ?
H41D C411 H41E 106.9 . . ?
C412 C411 N4 119.7(3) . . ?
C412 C411 H41D 107.4 . . ?
C412 C411 H41E 107.4 . . ?
C411 C412 H41F 109.3 . . ?
C411 C412 H41G 109.3 . . ?
C411 C412 C413 111.5(4) . . ?
H41F C412 H41G 108.0 . . ?
C413 C412 H41F 109.3 . . ?
C413 C412 H41G 109.3 . . ?
C412 C413 H41H 108.7 . . ?
C412 C413 H41I 108.7 . . ?
H41H C413 H41I 107.6 . . ?
C414 C413 C412 114.1(4) . . ?
C414 C413 H41H 108.7 . . ?
C414 C413 H41I 108.7 . . ?
C413 C414 H41J 112.2 . . ?
C413 C414 H41K 112.2 . . ?
C413 C414 C415 97.6(5) . . ?
H41J C414 H41K 109.8 . . ?
C415 C414 H41J 112.2 . . ?
C415 C414 H41K 112.2 . . ?
C414 C415 H41L 109.5 . . ?
C414 C415 H41M 109.5 . . ?
C414 C415 H41N 109.5 . . ?
H41L C415 H41M 109.5 . . ?
H41L C415 H41N 109.5 . . ?
H41M C415 H41N 109.5 . . ?
N4 C416 H41O 108.3 . . ?
N4 C416 H41P 108.3 . . ?
N4 C416 C417 115.84(19) . . ?
H41O C416 H41P 107.4 . . ?
C417 C416 H41O 108.3 . . ?
C417 C416 H41P 108.3 . . ?
C416 C417 H41Q 109.4 . . ?
C416 C417 H41R 109.4 . . ?
H41Q C417 H41R 108.0 . . ?
C418 C417 C416 111.3(2) . . ?
C418 C417 H41Q 109.4 . . ?
C418 C417 H41R 109.4 . . ?
C417 C418 H41S 108.8 . . ?
C417 C418 H41T 108.8 . . ?
C417 C418 C419 113.6(3) . . ?
H41S C418 H41T 107.7 . . ?
C419 C418 H41S 108.8 . . ?
C419 C418 H41T 108.8 . . ?
C418 C419 H41U 109.1 . . ?
C418 C419 H41V 109.1 . . ?
H41U C419 H41V 107.9 . . ?
C420 C419 C418 112.4(3) . . ?
C420 C419 H41U 109.1 . . ?
C420 C419 H41V 109.1 . . ?
C419 C420 H42A 109.5 . . ?
C419 C420 H42B 109.5 . . ?
C419 C420 H42C 109.5 . . ?
H42A C420 H42B 109.5 . . ?
H42A C420 H42C 109.5 . . ?
H42B C420 H42C 109.5 . . ?
C301 N3 C306 107.33(17) . . ?
C301 N3 C311 109.73(18) . . ?
C311 N3 C306 110.48(18) . . ?
C316 N3 C301 110.35(18) . . ?
C316 N3 C306 111.29(19) . . ?
C316 N3 C311 107.67(17) . . ?
N3 C301 H30A 108.2 . . ?
N3 C301 H30B 108.2 . . ?
N3 C301 C302 116.27(18) . . ?
H30A C301 H30B 107.4 . . ?
C302 C301 H30A 108.2 . . ?
C302 C301 H30B 108.2 . . ?
C301 C302 H30C 109.8 . . ?
C301 C302 H30D 109.8 . . ?
C301 C302 C303 109.2(2) . . ?
H30C C302 H30D 108.3 . . ?
C303 C302 H30C 109.8 . . ?
C303 C302 H30D 109.8 . . ?
C302 C303 H30E 108.7 . . ?
C302 C303 H30F 108.7 . . ?
H30E C303 H30F 107.6 . . ?
C304 C303 C302 114.4(2) . . ?
C304 C303 H30E 108.7 . . ?
C304 C303 H30F 108.7 . . ?
C303 C304 H30G 108.7 . . ?
C303 C304 H30H 108.7 . . ?
C303 C304 C305 114.1(3) . . ?
H30G C304 H30H 107.6 . . ?
C305 C304 H30G 108.7 . . ?
C305 C304 H30H 108.7 . . ?
C304 C305 H30I 109.5 . . ?
C304 C305 H30J 109.5 . . ?
C304 C305 H30K 109.5 . . ?
H30I C305 H30J 109.5 . . ?
H30I C305 H30K 109.5 . . ?
H30J C305 H30K 109.5 . . ?
N3 C306 H30L 108.5 . . ?
N3 C306 H30M 108.5 . . ?
H30L C306 H30M 107.5 . . ?
C307 C306 N3 114.9(2) . . ?
C307 C306 H30L 108.5 . . ?
C307 C306 H30M 108.5 . . ?
C306 C307 H30N 109.3 . . ?
C306 C307 H30O 109.3 . . ?
C306 C307 C308 111.5(2) . . ?
H30N C307 H30O 108.0 . . ?
C308 C307 H30N 109.3 . . ?
C308 C307 H30O 109.3 . . ?
C307 C308 H30P 108.5 . . ?
C307 C308 H30Q 108.5 . . ?
H30P C308 H30Q 107.5 . . ?
C309 C308 C307 114.9(3) . . ?
C309 C308 H30P 108.5 . . ?
C309 C308 H30Q 108.5 . . ?
C308 C309 H30R 109.6 . . ?
C308 C309 H30S 109.6 . . ?
C308 C309 C310 110.4(4) . . ?
H30R C309 H30S 108.1 . . ?
C310 C309 H30R 109.6 . . ?
C310 C309 H30S 109.6 . . ?
C309 C310 H31A 109.5 . . ?
C309 C310 H31B 109.5 . . ?
C309 C310 H31C 109.5 . . ?
H31A C310 H31B 109.5 . . ?
H31A C310 H31C 109.5 . . ?
H31B C310 H31C 109.5 . . ?
N3 C311 H31D 108.5 . . ?
N3 C311 H31E 108.5 . . ?
H31D C311 H31E 107.5 . . ?
C312 C311 N3 115.04(18) . . ?
C312 C311 H31D 108.5 . . ?
C312 C311 H31E 108.5 . . ?
C311 C312 H31F 109.5 . . ?
C311 C312 H31G 109.5 . . ?
C311 C312 C313 110.5(2) . . ?
H31F C312 H31G 108.1 . . ?
C313 C312 H31F 109.5 . . ?
C313 C312 H31G 109.5 . . ?
C312 C313 H31H 109.0 . . ?
C312 C313 H31I 109.0 . . ?
C312 C313 C314 112.9(2) . . ?
H31H C313 H31I 107.8 . . ?
C314 C313 H31H 109.0 . . ?
C314 C313 H31I 109.0 . . ?
C313 C314 H31J 108.8 . . ?
C313 C314 H31K 108.8 . . ?
H31J C314 H31K 107.7 . . ?
C315 C314 C313 113.8(2) . . ?
C315 C314 H31J 108.8 . . ?
C315 C314 H31K 108.8 . . ?
C314 C315 H31L 109.5 . . ?
C314 C315 H31M 109.5 . . ?
C314 C315 H31N 109.5 . . ?
H31L C315 H31M 109.5 . . ?
H31L C315 H31N 109.5 . . ?
H31M C315 H31N 109.5 . . ?
N3 C316 H31O 108.6 . . ?
N3 C316 H31P 108.6 . . ?
N3 C316 C317 114.69(19) . . ?
H31O C316 H31P 107.6 . . ?
C317 C316 H31O 108.6 . . ?
C317 C316 H31P 108.6 . . ?
C316 C317 H31Q 109.6 . . ?
C316 C317 H31R 109.6 . . ?
C316 C317 C318 110.2(2) . . ?
H31Q C317 H31R 108.1 . . ?
C318 C317 H31Q 109.6 . . ?
C318 C317 H31R 109.6 . . ?
C317 C318 H31S 108.5 . . ?
C317 C318 H31T 108.5 . . ?
H31S C318 H31T 107.5 . . ?
C319 C318 C317 115.1(2) . . ?
C319 C318 H31S 108.5 . . ?
C319 C318 H31T 108.5 . . ?
C318 C319 H31U 108.8 . . ?
C318 C319 H31V 108.8 . . ?
H31U C319 H31V 107.7 . . ?
C320 C319 C318 113.7(2) . . ?
C320 C319 H31U 108.8 . . ?
C320 C319 H31V 108.8 . . ?
C319 C320 H32A 109.5 . . ?
C319 C320 H32B 109.5 . . ?
C319 C320 H32C 109.5 . . ?
H32A C320 H32B 109.5 . . ?
H32A C320 H32C 109.5 . . ?
H32B C320 H32C 109.5 . . ?
H42D C422 H42E 107.5 . . ?
C423 C422 H42D 108.5 . . ?
C423 C422 H42E 108.5 . . ?
C423 C422 C421 115.2(6) . . ?
C421 C422 H42D 108.5 . . ?
C421 C422 H42E 108.5 . . ?
C422 C423 H42F 112.0 . . ?
C422 C423 H42G 112.0 . . ?
C422 C423 C424 99.0(5) . . ?
H42F C423 H42G 109.6 . . ?
C424 C423 H42F 112.0 . . ?
C424 C423 H42G 112.0 . . ?
C422 C421 H42H 109.8 . . ?
C422 C421 H42I 109.8 . . ?
C422 C421 C425 109.5(5) . . ?
H42H C421 H42I 108.2 . . ?
C425 C421 H42H 109.8 . . ?
C425 C421 H42I 109.8 . . ?
C423 C424 H42J 109.5 . . ?
C423 C424 H42K 109.5 . . ?
C423 C424 H42L 109.5 . . ?
H42J C424 H42K 109.5 . . ?
H42J C424 H42L 109.5 . . ?
H42K C424 H42L 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.920
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.609(14)
2 0.391(14)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane/o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_TiOPcTPCMDABCO
_database_code_depnum_ccdc_archive 'CCDC 1581410'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'salt of titanyl phthalocyanine with N-mehyldiazabicyclooctanium cation and neutral trypticene molecule'
_chemical_name_common            no
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '(C32 H16 N8 O Ti), (C20 H14), (C7 H15, N2)'
_chemical_formula_sum            'C59 H45 N10 O Ti'
_chemical_formula_weight         957.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.4984(3)
_cell_length_b                   24.7177(5)
_cell_length_c                   13.8468(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.086(2)
_cell_angle_gamma                90
_cell_volume                     4574.04(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6537
_cell_measurement_theta_min      4.5410
_cell_measurement_theta_max      25.3580

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             1996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.051
_exptl_absorpt_coefficient_mu    0.244
_shelx_estimated_absorpt_T_min   0.955
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_T_min  0.97360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_reflns_number            45629
_diffrn_reflns_av_unetI/netI     0.2068
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.648
_diffrn_reflns_theta_max         29.054
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11107
_reflns_number_gt                4654
_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.
;

_diffrn_measurement_method       'ω scans'

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;

_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX

_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)+(0.0288P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11107
_refine_ls_number_parameters     640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   0.733
_refine_ls_restrained_S_all      0.733
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O 0.05787(10) 0.11726(6) 0.76525(10) 0.0264(4) Uani 1 1 d . . . . .
N103 N 0.16975(12) 0.07865(6) 0.95416(12) 0.0209(4) Uani 1 1 d . . . . .
N106 N 0.03978(13) 0.09302(7) 1.05826(12) 0.0222(4) Uani 1 1 d . . . . .
N101 N 0.01212(12) -0.00001(7) 0.73759(12) 0.0220(4) Uani 1 1 d . . . . .
C107 C -0.13786(15) 0.06913(8) 1.01843(15) 0.0209(5) Uani 1 1 d . . . . .
C109 C 0.13417(17) 0.09478(8) 1.03900(15) 0.0231(5) Uani 1 1 d . . . . .
C108 C -0.03495(16) 0.07210(8) 0.99846(15) 0.0214(5) Uani 1 1 d . . . . .
C128 C 0.39791(17) 0.11951(9) 1.11548(17) 0.0331(6) Uani 1 1 d . . . . .
H105 H 0.4571 0.1152 1.0865 0.040 Uiso 1 1 calc R U . . .
C101 C 0.05035(17) -0.02497(8) 0.66068(15) 0.0242(5) Uani 1 1 d . . . . .
C105 C -0.12550(16) 0.03065(8) 0.87019(15) 0.0223(5) Uani 1 1 d . . . . .
C124 C -0.18323(16) 0.08683(8) 1.09730(15) 0.0258(6) Uani 1 1 d . . . . .
H113 H -0.1456 0.1042 1.1517 0.031 Uiso 1 1 calc R U . . .
C112 C 0.27250(17) 0.08593(8) 0.96746(15) 0.0245(5) Uani 1 1 d . . . . .
C110 C 0.21708(16) 0.11305(8) 1.10787(15) 0.0241(5) Uani 1 1 d . . . . .
C116 C 0.21922(17) -0.00242(9) 0.70220(16) 0.0253(6) Uani 1 1 d . . . . .
C122 C -0.34088(16) 0.05182(9) 1.01490(16) 0.0282(6) Uani 1 1 d . . . . .
H115 H -0.4106 0.0463 1.0146 0.034 Uiso 1 1 calc R U . . .
C113 C 0.30771(16) 0.04636(9) 0.82263(16) 0.0234(5) Uani 1 1 d . . . . .
C104 C -0.08985(16) -0.00858(8) 0.72503(15) 0.0218(5) Uani 1 1 d . . . . .
C123 C -0.28510(17) 0.07820(9) 1.09331(16) 0.0282(6) Uani 1 1 d . . . . .
H114 H -0.3179 0.0906 1.1455 0.034 Uiso 1 1 calc R U . . .
Ti Ti 0.08269(3) 0.05990(2) 0.82450(3) 0.02138(11) Uani 1 1 d . . . . .
N108 N 0.14614(14) -0.02746(7) 0.64612(12) 0.0251(5) Uani 1 1 d . . . . .
N105 N -0.15453(13) 0.00625(7) 0.78619(12) 0.0227(4) Uani 1 1 d . . . . .
C106 C -0.19359(15) 0.04343(8) 0.93980(15) 0.0210(5) Uani 1 1 d . . . . .
N107 N 0.33620(13) 0.07299(7) 0.90480(13) 0.0245(5) Uani 1 1 d . . . . .
C111 C 0.30393(16) 0.10760(8) 1.06356(15) 0.0239(5) Uani 1 1 d . . . . .
C121 C -0.29512(16) 0.03362(8) 0.93726(16) 0.0262(6) Uani 1 1 d . . . . .
H116 H -0.3322 0.0150 0.8840 0.031 Uiso 1 1 calc R U . . .
N102 N -0.03069(12) 0.04890(7) 0.90708(12) 0.0202(4) Uani 1 1 d . . . . .
C103 C -0.11934(16) -0.03763(8) 0.63585(15) 0.0226(5) Uani 1 1 d . . . . .
N104 N 0.21229(13) 0.02995(7) 0.78334(12) 0.0220(4) Uani 1 1 d . . . . .
C114 C 0.37817(16) 0.02589(9) 0.75973(16) 0.0253(5) Uani 1 1 d . . . . .
C117 C -0.03608(18) -0.07410(8) 0.50573(15) 0.0283(6) Uani 1 1 d . . . . .
H124 H 0.0231 -0.0809 0.4778 0.034 Uiso 1 1 calc R U . . .
C120 C -0.21194(16) -0.05358(9) 0.58716(15) 0.0268(5) Uani 1 1 d . . . . .
H121 H -0.2715 -0.0467 0.6144 0.032 Uiso 1 1 calc R U . . .
C115 C 0.32359(16) -0.00467(9) 0.68741(16) 0.0267(6) Uani 1 1 d . . . . .
C119 C -0.21554(18) -0.07955(8) 0.49882(15) 0.0308(6) Uani 1 1 d . . . . .
H122 H -0.2782 -0.0907 0.4647 0.037 Uiso 1 1 calc R U . . .
C118 C -0.12743(19) -0.08979(9) 0.45859(16) 0.0307(6) Uani 1 1 d . . . . .
H123 H -0.1314 -0.1079 0.3977 0.037 Uiso 1 1 calc R U . . .
C125 C 0.22248(18) 0.13116(9) 1.20353(16) 0.0317(6) Uani 1 1 d . . . . .
H108 H 0.1636 0.1348 1.2334 0.038 Uiso 1 1 calc R U . . .
C102 C -0.03127(16) -0.04806(8) 0.59545(15) 0.0228(5) Uani 1 1 d . . . . .
C131 C 0.47235(19) -0.02440(10) 0.62125(18) 0.0414(7) Uani 1 1 d . . . . .
H130 H 0.5062 -0.0418 0.5742 0.050 Uiso 1 1 calc R U . . .
C129 C 0.48110(17) 0.03226(9) 0.76474(17) 0.0344(6) Uani 1 1 d . . . . .
H132 H 0.5182 0.0533 0.8147 0.041 Uiso 1 1 calc R U . . .
C132 C 0.37033(18) -0.03059(9) 0.61564(17) 0.0350(6) Uani 1 1 d . . . . .
H129 H 0.3332 -0.0515 0.5654 0.042 Uiso 1 1 calc R U . . .
C127 C 0.40196(19) 0.13775(10) 1.21044(17) 0.0392(7) Uani 1 1 d . . . . .
H106 H 0.4650 0.1464 1.2468 0.047 Uiso 1 1 calc R U . . .
C130 C 0.52753(18) 0.00674(11) 0.69408(19) 0.0427(7) Uani 1 1 d . . . . .
H131 H 0.5977 0.0105 0.6952 0.051 Uiso 1 1 calc R U . . .
C126 C 0.31484(19) 0.14374(10) 1.25410(17) 0.0387(7) Uani 1 1 d . . . . .
H107 H 0.3197 0.1566 1.3192 0.046 Uiso 1 1 calc R U . . .
C209 C -0.0473(2) 0.21331(12) 0.60621(19) 0.0617(9) Uani 1 1 d . . . . .
H20A H 0.0091 0.1902 0.6323 0.093 Uiso 1 1 calc R U . A 1
H20B H -0.0314 0.2511 0.6236 0.093 Uiso 1 1 calc R U . A 1
H20C H -0.0599 0.2097 0.5351 0.093 Uiso 1 1 calc R U . A 1
C207 C -0.11825(16) 0.20272(10) 0.75684(14) 0.0299(6) Uani 1 1 d . . . B 1
H20D H -0.1146 0.2416 0.7741 0.036 Uiso 1 1 calc R U . B 1
H20E H -0.0533 0.1858 0.7822 0.036 Uiso 1 1 calc R U . B 1
C206 C -0.26324(19) 0.12369(10) 0.6547(2) 0.0518(8) Uani 1 1 d . . . B 1
H20F H -0.2584 0.0879 0.6870 0.062 Uiso 1 1 calc R U . B 1
H20G H -0.3153 0.1216 0.5968 0.062 Uiso 1 1 calc R U . B 1
C205 C -0.16304(18) 0.13841(10) 0.62315(17) 0.0403(7) Uani 1 1 d . . . B 1
H20H H -0.1100 0.1146 0.6566 0.048 Uiso 1 1 calc R U . B 1
H20I H -0.1663 0.1329 0.5519 0.048 Uiso 1 1 calc R U . B 1
C208 C -0.2012(2) 0.17589(11) 0.80297(18) 0.0480(8) Uani 1 1 d . . . B 1
H20J H -0.2203 0.1992 0.8555 0.058 Uiso 1 1 calc R U . B 1
H20K H -0.1775 0.1408 0.8321 0.058 Uiso 1 1 calc R U . B 1
N201 N -0.13802(14) 0.19660(8) 0.64822(13) 0.0323(5) Uani 1 1 d . . . B 1
C203 C -0.22640(19) 0.23102(10) 0.60995(17) 0.0464(7) Uani 1 1 d . . . B 1
H20L H -0.2474 0.2231 0.5400 0.056 Uiso 1 1 calc R U . B 1
H20M H -0.2079 0.2697 0.6164 0.056 Uiso 1 1 calc R U . B 1
N202 N -0.2921(2) 0.16671(12) 0.7253(2) 0.0852(9) Uani 1 1 d . . . B 1
C204 C -0.31188(19) 0.21934(11) 0.6669(2) 0.0575(8) Uani 1 1 d . . . B 1
H20N H -0.3750 0.2160 0.6214 0.069 Uiso 1 1 calc R U . B 1
H20O H -0.3192 0.2497 0.7120 0.069 Uiso 1 1 calc R U . B 1
C307 C -0.09916(17) -0.20508(10) 0.59470(16) 0.0286(6) Uani 1 1 d . . . . .
H307 H -0.1149 -0.1684 0.6061 0.034 Uiso 1 1 calc R U . . .
C320 C 0.15974(16) -0.20954(9) 0.69181(15) 0.0271(6) Uani 1 1 d . . . . .
C315 C 0.18342(17) -0.26395(10) 0.67878(15) 0.0295(6) Uani 1 1 d . . . . .
C303 C 0.00581(17) -0.28323(9) 0.63141(15) 0.0251(6) Uani 1 1 d . . . . .
C309 C 0.08183(16) -0.29157(9) 0.80022(15) 0.0268(6) Uani 1 1 d . . . . .
C314 C 0.06210(16) -0.23753(9) 0.81747(16) 0.0281(6) Uani 1 1 d . . . . .
C302 C 0.05779(16) -0.20249(9) 0.72568(15) 0.0272(6) Uani 1 1 d . . . . .
H302 H 0.0414 -0.1638 0.7374 0.033 Uiso 1 1 calc R U . . .
C304 C -0.05443(18) -0.31296(10) 0.56222(16) 0.0334(6) Uani 1 1 d . . . . .
H304 H -0.0396 -0.3499 0.5515 0.040 Uiso 1 1 calc R U . . .
C313 C 0.04924(16) -0.22057(10) 0.90948(17) 0.0336(6) Uani 1 1 d . . . . .
H313 H 0.0371 -0.1835 0.9220 0.040 Uiso 1 1 calc R U . . .
C317 C 0.34390(19) -0.23706(12) 0.64247(18) 0.0457(7) Uani 1 1 d . . . . .
H317 H 0.4082 -0.2463 0.6272 0.055 Uiso 1 1 calc R U . . .
C308 C -0.01671(16) -0.22906(9) 0.64823(15) 0.0240(5) Uani 1 1 d . . . . .
C319 C 0.22696(18) -0.16945(10) 0.67724(15) 0.0338(6) Uani 1 1 d . . . . .
H319 H 0.2101 -0.1325 0.6843 0.041 Uiso 1 1 calc R U . . .
C306 C -0.15906(18) -0.23494(11) 0.52410(16) 0.0351(6) Uani 1 1 d . . . . .
H306 H -0.2153 -0.2184 0.4866 0.042 Uiso 1 1 calc R U . . .
C301 C 0.09967(17) -0.30271(9) 0.69587(15) 0.0297(6) Uani 1 1 d . . . . .
H301 H 0.1159 -0.3414 0.6843 0.036 Uiso 1 1 calc R U . . .
C318 C 0.31966(19) -0.18357(12) 0.65207(17) 0.0409(7) Uani 1 1 d . . . . .
H318 H 0.3663 -0.1562 0.6415 0.049 Uiso 1 1 calc R U . . .
C310 C 0.08345(17) -0.32975(10) 0.87298(17) 0.0367(6) Uani 1 1 d . . . . .
H310 H 0.0941 -0.3669 0.8599 0.044 Uiso 1 1 calc R U . . .
C312 C 0.05434(17) -0.25876(12) 0.98375(18) 0.0412(7) Uani 1 1 d . . . . .
H312 H 0.0475 -0.2473 1.0480 0.049 Uiso 1 1 calc R U . . .
C305 C -0.13733(18) -0.28838(11) 0.50813(16) 0.0373(7) Uani 1 1 d . . . . .
H305 H -0.1790 -0.3086 0.4601 0.045 Uiso 1 1 calc R U . . .
C316 C 0.27603(18) -0.27796(11) 0.65467(16) 0.0386(7) Uani 1 1 d . . . . .
H316 H 0.2930 -0.3148 0.6466 0.046 Uiso 1 1 calc R U . . .
C311 C 0.06908(17) -0.31291(12) 0.96625(18) 0.0405(7) Uani 1 1 d . . . . .
H311 H 0.0695 -0.3386 1.0173 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O Ti 1.6489(14) . ?
N103 C112 1.385(3) . ?
N103 C109 1.389(2) . ?
N103 Ti 2.0557(17) . ?
N106 C108 1.317(3) . ?
N106 C109 1.339(2) . ?
N101 C104 1.379(3) . ?
N101 C101 1.391(2) . ?
N101 Ti 2.0557(18) . ?
C107 C106 1.387(3) . ?
C107 C124 1.395(3) . ?
C107 C108 1.456(3) . ?
C109 C110 1.437(3) . ?
C108 N102 1.398(2) . ?
C128 C127 1.384(3) . ?
C128 C111 1.399(3) . ?
C128 H105 0.9500 . ?
C101 N108 1.338(2) . ?
C101 C102 1.441(3) . ?
C105 N105 1.320(2) . ?
C105 N102 1.385(3) . ?
C105 C106 1.457(3) . ?
C124 C123 1.385(3) . ?
C124 H113 0.9500 . ?
C112 N107 1.343(2) . ?
C112 C111 1.442(3) . ?
C110 C125 1.390(3) . ?
C110 C111 1.404(3) . ?
C116 N108 1.320(3) . ?
C116 N104 1.393(3) . ?
C116 C115 1.453(3) . ?
C122 C121 1.388(3) . ?
C122 C123 1.393(3) . ?
C122 H115 0.9500 . ?
C113 N107 1.324(3) . ?
C113 N104 1.387(3) . ?
C113 C114 1.467(3) . ?
C104 N105 1.350(2) . ?
C104 C103 1.435(3) . ?
C123 H114 0.9500 . ?
Ti N104 2.0527(16) . ?
Ti N102 2.0533(16) . ?
C106 C121 1.387(3) . ?
C121 H116 0.9500 . ?
C103 C120 1.391(3) . ?
C103 C102 1.407(3) . ?
C114 C115 1.381(3) . ?
C114 C129 1.390(3) . ?
C117 C118 1.368(3) . ?
C117 C102 1.393(3) . ?
C117 H124 0.9500 . ?
C120 C119 1.376(3) . ?
C120 H121 0.9500 . ?
C115 C132 1.404(3) . ?
C119 C118 1.405(3) . ?
C119 H122 0.9500 . ?
C118 H123 0.9500 . ?
C125 C126 1.377(3) . ?
C125 H108 0.9500 . ?
C131 C132 1.377(3) . ?
C131 C130 1.397(3) . ?
C131 H130 0.9500 . ?
C129 C130 1.386(3) . ?
C129 H132 0.9500 . ?
C132 H129 0.9500 . ?
C127 C126 1.404(3) . ?
C127 H106 0.9500 . ?
C130 H131 0.9500 . ?
C126 H107 0.9500 . ?
C209 N201 1.486(3) . ?
C209 H20A 0.9800 . ?
C209 H20B 0.9800 . ?
C209 H20C 0.9800 . ?
C207 N201 1.498(3) . ?
C207 C208 1.518(3) . ?
C207 H20D 0.9900 . ?
C207 H20E 0.9900 . ?
C206 C205 1.523(3) . ?
C206 N202 1.532(3) . ?
C206 H20F 0.9900 . ?
C206 H20G 0.9900 . ?
C205 N201 1.507(3) . ?
C205 H20H 0.9900 . ?
C205 H20I 0.9900 . ?
C208 N202 1.530(3) . ?
C208 H20J 0.9900 . ?
C208 H20K 0.9900 . ?
N201 C203 1.500(3) . ?
C203 C204 1.514(3) . ?
C203 H20L 0.9900 . ?
C203 H20M 0.9900 . ?
N202 C204 1.535(3) . ?
C204 H20N 0.9900 . ?
C204 H20O 0.9900 . ?
C307 C308 1.381(3) . ?
C307 C306 1.390(3) . ?
C307 H307 0.9500 . ?
C320 C319 1.378(3) . ?
C320 C315 1.400(3) . ?
C320 C302 1.525(3) . ?
C315 C316 1.383(3) . ?
C315 C301 1.526(3) . ?
C303 C304 1.378(3) . ?
C303 C308 1.400(3) . ?
C303 C301 1.522(3) . ?
C309 C310 1.378(3) . ?
C309 C314 1.389(3) . ?
C309 C301 1.523(3) . ?
C314 C313 1.375(3) . ?
C314 C302 1.532(3) . ?
C302 C308 1.513(3) . ?
C302 H302 1.0000 . ?
C304 C305 1.395(3) . ?
C304 H304 0.9500 . ?
C313 C312 1.391(3) . ?
C313 H313 0.9500 . ?
C317 C318 1.373(3) . ?
C317 C316 1.390(3) . ?
C317 H317 0.9500 . ?
C319 C318 1.390(3) . ?
C319 H319 0.9500 . ?
C306 C305 1.378(3) . ?
C306 H306 0.9500 . ?
C301 H301 1.0000 . ?
C318 H318 0.9500 . ?
C310 C311 1.396(3) . ?
C310 H310 0.9500 . ?
C312 C311 1.380(3) . ?
C312 H312 0.9500 . ?
C305 H305 0.9500 . ?
C316 H316 0.9500 . ?
C311 H311 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
C112 N103 C109 108.02(18) . . ?
C112 N103 Ti 125.74(13) . . ?
C109 N103 Ti 125.47(14) . . ?
C108 N106 C109 123.61(17) . . ?
C104 N101 C101 107.84(17) . . ?
C104 N101 Ti 123.82(13) . . ?
C101 N101 Ti 125.18(14) . . ?
C106 C107 C124 120.58(19) . . ?
C106 C107 C108 107.49(17) . . ?
C124 C107 C108 131.9(2) . . ?
N106 C109 N103 127.7(2) . . ?
N106 C109 C110 123.52(19) . . ?
N103 C109 C110 108.77(18) . . ?
N106 C108 N102 127.21(18) . . ?
N106 C108 C107 124.55(18) . . ?
N102 C108 C107 108.24(19) . . ?
C127 C128 C111 118.0(2) . . ?
C127 C128 H105 121.0 . . ?
C111 C128 H105 121.0 . . ?
N108 C101 N101 127.3(2) . . ?
N108 C101 C102 123.88(19) . . ?
N101 C101 C102 108.80(18) . . ?
N105 C105 N102 128.19(18) . . ?
N105 C105 C106 123.1(2) . . ?
N102 C105 C106 108.75(18) . . ?
C123 C124 C107 117.6(2) . . ?
C123 C124 H113 121.2 . . ?
C107 C124 H113 121.2 . . ?
N107 C112 N103 127.1(2) . . ?
N107 C112 C111 123.5(2) . . ?
N103 C112 C111 109.28(18) . . ?
C125 C110 C111 120.8(2) . . ?
C125 C110 C109 131.7(2) . . ?
C111 C110 C109 107.46(18) . . ?
N108 C116 N104 127.89(19) . . ?
N108 C116 C115 123.9(2) . . ?
N104 C116 C115 108.2(2) . . ?
C121 C122 C123 120.3(2) . . ?
C121 C122 H115 119.8 . . ?
C123 C122 H115 119.8 . . ?
N107 C113 N104 128.63(19) . . ?
N107 C113 C114 123.2(2) . . ?
N104 C113 C114 108.07(19) . . ?
N105 C104 N101 126.96(19) . . ?
N105 C104 C103 123.4(2) . . ?
N101 C104 C103 109.67(18) . . ?
C124 C123 C122 121.9(2) . . ?
C124 C123 H114 119.1 . . ?
C122 C123 H114 119.1 . . ?
O Ti N104 107.07(6) . . ?
O Ti N102 106.01(7) . . ?
N104 Ti N102 146.92(7) . . ?
O Ti N103 106.97(7) . . ?
N104 Ti N103 85.36(7) . . ?
N102 Ti N103 85.58(6) . . ?
O Ti N101 106.44(7) . . ?
N104 Ti N101 85.44(7) . . ?
N102 Ti N101 84.85(6) . . ?
N103 Ti N101 146.58(7) . . ?
C116 N108 C101 123.20(18) . . ?
C105 N105 C104 122.61(18) . . ?
C107 C106 C121 121.64(18) . . ?
C107 C106 C105 107.20(18) . . ?
C121 C106 C105 131.2(2) . . ?
C113 N107 C112 122.58(18) . . ?
C128 C111 C110 120.5(2) . . ?
C128 C111 C112 132.9(2) . . ?
C110 C111 C112 106.47(19) . . ?
C106 C121 C122 118.0(2) . . ?
C106 C121 H116 121.0 . . ?
C122 C121 H116 121.0 . . ?
C105 N102 C108 108.30(16) . . ?
C105 N102 Ti 124.07(13) . . ?
C108 N102 Ti 125.34(14) . . ?
C120 C103 C102 120.5(2) . . ?
C120 C103 C104 132.9(2) . . ?
C102 C103 C104 106.62(19) . . ?
C113 N104 C116 108.69(17) . . ?
C113 N104 Ti 124.50(14) . . ?
C116 N104 Ti 125.98(15) . . ?
C115 C114 C129 121.7(2) . . ?
C115 C114 C113 107.14(19) . . ?
C129 C114 C113 131.2(2) . . ?
C118 C117 C102 118.9(2) . . ?
C118 C117 H124 120.6 . . ?
C102 C117 H124 120.6 . . ?
C119 C120 C103 118.7(2) . . ?
C119 C120 H121 120.7 . . ?
C103 C120 H121 120.7 . . ?
C114 C115 C132 121.0(2) . . ?
C114 C115 C116 107.80(18) . . ?
C132 C115 C116 131.2(2) . . ?
C120 C119 C118 120.7(2) . . ?
C120 C119 H122 119.7 . . ?
C118 C119 H122 119.7 . . ?
C117 C118 C119 121.1(2) . . ?
C117 C118 H123 119.5 . . ?
C119 C118 H123 119.5 . . ?
C126 C125 C110 118.7(2) . . ?
C126 C125 H108 120.7 . . ?
C110 C125 H108 120.7 . . ?
C117 C102 C103 120.2(2) . . ?
C117 C102 C101 132.7(2) . . ?
C103 C102 C101 107.02(18) . . ?
C132 C131 C130 121.9(2) . . ?
C132 C131 H130 119.0 . . ?
C130 C131 H130 119.0 . . ?
C130 C129 C114 117.5(2) . . ?
C130 C129 H132 121.3 . . ?
C114 C129 H132 121.3 . . ?
C131 C132 C115 117.1(2) . . ?
C131 C132 H129 121.5 . . ?
C115 C132 H129 121.5 . . ?
C128 C127 C126 121.3(2) . . ?
C128 C127 H106 119.3 . . ?
C126 C127 H106 119.3 . . ?
C129 C130 C131 120.8(2) . . ?
C129 C130 H131 119.6 . . ?
C131 C130 H131 119.6 . . ?
C125 C126 C127 120.7(2) . . ?
C125 C126 H107 119.6 . . ?
C127 C126 H107 119.6 . . ?
N201 C209 H20A 109.5 . . ?
N201 C209 H20B 109.5 . . ?
H20A C209 H20B 109.5 . . ?
N201 C209 H20C 109.5 . . ?
H20A C209 H20C 109.5 . . ?
H20B C209 H20C 109.5 . . ?
N201 C207 C208 109.92(19) . . ?
N201 C207 H20D 109.7 . . ?
C208 C207 H20D 109.7 . . ?
N201 C207 H20E 109.7 . . ?
C208 C207 H20E 109.7 . . ?
H20D C207 H20E 108.2 . . ?
C205 C206 N202 109.5(2) . . ?
C205 C206 H20F 109.8 . . ?
N202 C206 H20F 109.8 . . ?
C205 C206 H20G 109.8 . . ?
N202 C206 H20G 109.8 . . ?
H20F C206 H20G 108.2 . . ?
N201 C205 C206 109.96(18) . . ?
N201 C205 H20H 109.7 . . ?
C206 C205 H20H 109.7 . . ?
N201 C205 H20I 109.7 . . ?
C206 C205 H20I 109.7 . . ?
H20H C205 H20I 108.2 . . ?
C207 C208 N202 109.6(2) . . ?
C207 C208 H20J 109.8 . . ?
N202 C208 H20J 109.8 . . ?
C207 C208 H20K 109.8 . . ?
N202 C208 H20K 109.8 . . ?
H20J C208 H20K 108.2 . . ?
C209 N201 C207 108.95(19) . . ?
C209 N201 C203 111.22(19) . . ?
C207 N201 C203 108.54(16) . . ?
C209 N201 C205 110.22(18) . . ?
C207 N201 C205 109.29(18) . . ?
C203 N201 C205 108.58(19) . . ?
N201 C203 C204 109.5(2) . . ?
N201 C203 H20L 109.8 . . ?
C204 C203 H20L 109.8 . . ?
N201 C203 H20M 109.8 . . ?
C204 C203 H20M 109.8 . . ?
H20L C203 H20M 108.2 . . ?
C208 N202 C206 107.5(2) . . ?
C208 N202 C204 107.9(2) . . ?
C206 N202 C204 107.0(2) . . ?
C203 C204 N202 110.3(2) . . ?
C203 C204 H20N 109.6 . . ?
N202 C204 H20N 109.6 . . ?
C203 C204 H20O 109.6 . . ?
N202 C204 H20O 109.6 . . ?
H20N C204 H20O 108.1 . . ?
C308 C307 C306 119.6(2) . . ?
C308 C307 H307 120.2 . . ?
C306 C307 H307 120.2 . . ?
C319 C320 C315 120.3(2) . . ?
C319 C320 C302 127.2(2) . . ?
C315 C320 C302 112.44(19) . . ?
C316 C315 C320 120.2(2) . . ?
C316 C315 C301 126.5(2) . . ?
C320 C315 C301 113.31(19) . . ?
C304 C303 C308 120.3(2) . . ?
C304 C303 C301 126.9(2) . . ?
C308 C303 C301 112.8(2) . . ?
C310 C309 C314 121.1(2) . . ?
C310 C309 C301 125.5(2) . . ?
C314 C309 C301 113.4(2) . . ?
C313 C314 C309 120.3(2) . . ?
C313 C314 C302 126.9(2) . . ?
C309 C314 C302 112.75(18) . . ?
C308 C302 C320 105.72(16) . . ?
C308 C302 C314 106.64(17) . . ?
C320 C302 C314 105.07(18) . . ?
C308 C302 H302 112.9 . . ?
C320 C302 H302 112.9 . . ?
C314 C302 H302 112.9 . . ?
C303 C304 C305 119.4(2) . . ?
C303 C304 H304 120.3 . . ?
C305 C304 H304 120.3 . . ?
C314 C313 C312 118.6(2) . . ?
C314 C313 H313 120.7 . . ?
C312 C313 H313 120.7 . . ?
C318 C317 C316 121.2(2) . . ?
C318 C317 H317 119.4 . . ?
C316 C317 H317 119.4 . . ?
C307 C308 C303 119.9(2) . . ?
C307 C308 C302 126.8(2) . . ?
C303 C308 C302 113.3(2) . . ?
C320 C319 C318 119.4(2) . . ?
C320 C319 H319 120.3 . . ?
C318 C319 H319 120.3 . . ?
C305 C306 C307 120.4(2) . . ?
C305 C306 H306 119.8 . . ?
C307 C306 H306 119.8 . . ?
C303 C301 C309 105.64(17) . . ?
C303 C301 C315 106.52(18) . . ?
C309 C301 C315 104.66(18) . . ?
C303 C301 H301 113.1 . . ?
C309 C301 H301 113.1 . . ?
C315 C301 H301 113.1 . . ?
C317 C318 C319 120.1(2) . . ?
C317 C318 H318 120.0 . . ?
C319 C318 H318 120.0 . . ?
C309 C310 C311 118.8(2) . . ?
C309 C310 H310 120.6 . . ?
C311 C310 H310 120.6 . . ?
C311 C312 C313 121.5(2) . . ?
C311 C312 H312 119.3 . . ?
C313 C312 H312 119.3 . . ?
C306 C305 C304 120.3(2) . . ?
C306 C305 H305 119.9 . . ?
C304 C305 H305 119.9 . . ?
C315 C316 C317 118.7(2) . . ?
C315 C316 H316 120.6 . . ?
C317 C316 H316 120.6 . . ?
C312 C311 C310 119.6(2) . . ?
C312 C311 H311 120.2 . . ?
C310 C311 H311 120.2 . . ?

_refine_diff_density_max         0.427
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.055

_shelxl_version_number           2013-2


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_VOPcHexyl4NC6H4Cl2
_database_code_depnum_ccdc_archive 'CCDC 1581403'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-03-23
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.03.22 svn.r3403 for OlexSys, GUI svn.r5332)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of vanadyl phthalocyanine with tetrahexylammonium cation, o-dichlobenzene solvate'
_chemical_formula_moiety         'C32 H16 N8 O V, C24 H52 N, C6 H4 Cl2'
_chemical_formula_sum            'C62 H72 Cl2 N9 O V'
_chemical_formula_weight         1081.12
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
_chemical_oxdiff_formula         'C248 H288 Cl8 N36 O4 V4'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   22.9200(6)
_cell_length_b                   11.7027(3)
_cell_length_c                   21.2051(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.783(3)
_cell_angle_gamma                90
_cell_volume                     5658.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9240
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      30.4550
_cell_measurement_theta_min      1.9430
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -1 0.0674
1 1 1 0.0945
-1 1 1 0.0760
-1 1 -1 0.0829
-1 0 1 0.1115
1 0 -1 0.1115
-1 -1 1 0.0727
-1 -1 -1 0.0700
1 -1 -1 0.0636
1 -1 1 0.0819

_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.14
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9998 1.0000 -0.9998 -0.0384 0.0587 0.0254
0.9996 1.0001 0.9992 -0.0549 0.0003 0.0545
-0.9998 1.0001 0.9991 -0.0728 -0.0160 -0.0028
-0.9995 1.0001 -1.0000 -0.0563 0.0424 -0.0319
-0.9998 0.0001 0.9995 -0.0172 -0.0373 -0.0141
0.9998 -0.0001 -0.9995 0.0172 0.0373 0.0141
-0.9998 -1.0000 0.9998 0.0384 -0.0587 -0.0254
-0.9996 -1.0001 -0.9992 0.0549 -0.0003 -0.0545
0.9998 -1.0001 -0.9991 0.0728 0.0160 0.0028
0.9995 -1.0001 1.0000 0.0563 -0.0424 0.0319

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22958
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.027
_diffrn_reflns_theta_min         1.956
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 -17.00   1.00  100.00    --   15.86 -19.00-120.00   27
  2  ω    -13.00  38.00   1.00  100.00    --   15.86 -57.00  30.00   51
  3  ω    -48.00  38.00   1.00  100.00    --   15.86 -57.00 120.00   86
  4  ω    -45.00 -19.00   1.00  100.00    --  -16.01 -37.00 -60.00   26
  5  ω    -74.00  14.00   1.00  100.00    --  -16.01 -57.00-120.00   88
  6  ω    -84.00 -50.00   1.00  100.00    --  -16.01 -59.00 176.32   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089578000
_diffrn_orient_matrix_UB_12      -0.0555962000
_diffrn_orient_matrix_UB_13      -0.0082265000
_diffrn_orient_matrix_UB_21      0.0081487000
_diffrn_orient_matrix_UB_22      0.0213253000
_diffrn_orient_matrix_UB_23      -0.0291812000
_diffrn_orient_matrix_UB_31      0.0286652000
_diffrn_orient_matrix_UB_32      0.0113271000
_diffrn_orient_matrix_UB_33      0.0145524000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                10847
_reflns_number_total             12469
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.367(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12469
_refine_ls_number_restraints     206
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      1.029
_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)+(0.0395P)²+2.1419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0898
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.633(18)
 0.367(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C22A \\sim C24A \\sim C203 \\sim C24B: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C106 \\sim C107 \\sim C121 \\sim C122 \\sim C123 \\sim C124: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C102 \\sim C103 \\sim C117 \\sim C118 \\sim C119 \\sim C120: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C110 \\sim C111 \\sim C125 \\sim C126 \\sim C127 \\sim C128: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C114 \\sim C115 \\sim C129 \\sim C130 \\sim C131 \\sim C132: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C24B) = Uanis(C24A)
Uanis(C25B) = Uanis(C25A)
Uanis(C26B) = Uanis(C26A)
4. Others
 Sof(H20K)=Sof(H20L)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=
 Sof(H25D)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(H20I)=Sof(H20J)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C207(H20C,H20D), C208(H20E,H20F), C209(H20G,H20H), C210(H21A,
 H21B), C211(H21C,H21D), C213(H21H,H21I), C214(H21J,H21K), C215(H21L,H21M),
 C216(H21N,H21O), C217(H21P,H21Q), C219(H21U,H21V), C220(H22A,H22B), C221(H22C,
 H22D), C222(H22E,H22F), C223(H22G,H22H), C22A(H22L,H22M), C24A(H24A,H24B),
 C25A(H25A,H25B), C203(H20I,H20J), C203(H20K,H20L), C24B(H24C,H24D), C25B(H25C,
 H25D)
5.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A)
5.c Idealised Me refined as rotating group:
 C212(H21E,H21F,H21G), C218(H21R,H21S,H21T), C224(H22I,H22J,H22K), C26A(H26A,
 H26B,H26C), C26B(H26D,H26E,H26F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
N201 N 0.73466(15) 0.2439(2) 0.38051(14) 0.0376(7) Uani 1 1 d . . . . .
C201 C 0.68912(19) 0.3208(3) 0.34447(17) 0.0450(10) Uani 1 1 d . . . . .
H20A H 0.706174 0.398053 0.341093 0.054 Uiso 1 1 calc R . . . .
H20B H 0.654972 0.327821 0.369325 0.054 Uiso 1 1 calc R . . . .
C207 C 0.74965(17) 0.2975(3) 0.44581(16) 0.0380(9) Uani 1 1 d . . . . .
H20C H 0.762871 0.376998 0.439881 0.046 Uiso 1 1 calc R . . . .
H20D H 0.713367 0.301256 0.467404 0.046 Uiso 1 1 calc R . . . .
C208 C 0.79635(18) 0.2362(3) 0.48913(17) 0.0449(10) Uani 1 1 d . . . . .
H20E H 0.834015 0.237973 0.470031 0.054 Uiso 1 1 calc R . . . .
H20F H 0.784914 0.155261 0.493625 0.054 Uiso 1 1 calc R . . . .
C209 C 0.80426(17) 0.2921(3) 0.55414(16) 0.0350(8) Uani 1 1 d . . . . .
H20G H 0.816042 0.372739 0.549292 0.042 Uiso 1 1 calc R . . . .
H20H H 0.766200 0.291728 0.572460 0.042 Uiso 1 1 calc R . . . .
C210 C 0.84978(17) 0.2328(3) 0.59969(16) 0.0367(8) Uani 1 1 d . . . . .
H21A H 0.838707 0.151395 0.603030 0.044 Uiso 1 1 calc R . . . .
H21B H 0.888055 0.235599 0.581871 0.044 Uiso 1 1 calc R . . . .
C211 C 0.85690(17) 0.2840(3) 0.66527(16) 0.0388(8) Uani 1 1 d . . . . .
H21C H 0.818605 0.281896 0.683065 0.047 Uiso 1 1 calc R . . . .
H21D H 0.868536 0.365100 0.662135 0.047 Uiso 1 1 calc R . . . .
C212 C 0.90238(17) 0.2224(3) 0.71060(18) 0.0422(9) Uani 1 1 d . . . . .
H21E H 0.890720 0.142382 0.714785 0.063 Uiso 1 1 calc GR . . . .
H21F H 0.904942 0.259441 0.752225 0.063 Uiso 1 1 calc GR . . . .
H21G H 0.940679 0.225725 0.693887 0.063 Uiso 1 1 calc GR . . . .
C213 C 0.71091(16) 0.1220(3) 0.38666(16) 0.0369(8) Uani 1 1 d . . . . .
H21H H 0.705609 0.087816 0.343772 0.044 Uiso 1 1 calc R . . . .
H21I H 0.741245 0.076613 0.412035 0.044 Uiso 1 1 calc R . . . .
C214 C 0.65365(17) 0.1089(3) 0.41638(19) 0.0442(9) Uani 1 1 d . . . . .
H21J H 0.623318 0.158910 0.394243 0.053 Uiso 1 1 calc R . . . .
H21K H 0.659307 0.132186 0.461472 0.053 Uiso 1 1 calc R . . . .
C215 C 0.63351(18) -0.0162(3) 0.41135(19) 0.0447(10) Uani 1 1 d . . . . .
H21L H 0.633544 -0.041708 0.366847 0.054 Uiso 1 1 calc R . . . .
H21M H 0.661918 -0.064114 0.437803 0.054 Uiso 1 1 calc R . . . .
C216 C 0.57265(17) -0.0344(3) 0.43231(17) 0.0416(9) Uani 1 1 d . . . . .
H21N H 0.544956 0.019587 0.409160 0.050 Uiso 1 1 calc R . . . .
H21O H 0.573650 -0.017058 0.478103 0.050 Uiso 1 1 calc R . . . .
C217 C 0.55030(19) -0.1561(3) 0.42051(19) 0.0460(10) Uani 1 1 d . . . . .
H21P H 0.551654 -0.174987 0.375177 0.055 Uiso 1 1 calc R . . . .
H21Q H 0.576734 -0.209613 0.445713 0.055 Uiso 1 1 calc R . . . .
C218 C 0.48785(19) -0.1732(3) 0.4378(2) 0.0500(11) Uani 1 1 d . . . . .
H21R H 0.486756 -0.160207 0.483275 0.075 Uiso 1 1 calc GR . . . .
H21S H 0.475108 -0.251449 0.427205 0.075 Uiso 1 1 calc GR . . . .
H21T H 0.461577 -0.119002 0.413859 0.075 Uiso 1 1 calc GR . . . .
C219 C 0.78878(17) 0.2324(3) 0.34458(16) 0.0371(8) Uani 1 1 d . . . . .
H21U H 0.816534 0.179504 0.368521 0.045 Uiso 1 1 calc R . . . .
H21V H 0.776653 0.196350 0.303080 0.045 Uiso 1 1 calc R . . . .
C220 C 0.82141(19) 0.3423(3) 0.33274(19) 0.0449(9) Uani 1 1 d . . . . .
H22A H 0.836854 0.376663 0.373727 0.054 Uiso 1 1 calc R . . . .
H22B H 0.794127 0.397715 0.310149 0.054 Uiso 1 1 calc R . . . .
C221 C 0.87200(18) 0.3174(3) 0.29312(18) 0.0421(9) Uani 1 1 d . . . . .
H22C H 0.856037 0.283350 0.252246 0.050 Uiso 1 1 calc R . . . .
H22D H 0.898403 0.260471 0.315624 0.050 Uiso 1 1 calc R . . . .
C222 C 0.90757(19) 0.4236(3) 0.27992(17) 0.0426(9) Uani 1 1 d . . . . .
H22E H 0.882835 0.475460 0.251674 0.051 Uiso 1 1 calc R . . . .
H22F H 0.918369 0.464437 0.320307 0.051 Uiso 1 1 calc R . . . .
C223 C 0.9630(2) 0.3958(3) 0.24935(19) 0.0499(10) Uani 1 1 d . . . . .
H22G H 0.951881 0.359861 0.207594 0.060 Uiso 1 1 calc R . . . .
H22H H 0.986145 0.339237 0.276087 0.060 Uiso 1 1 calc R . . . .
C224 C 1.0016(2) 0.4995(4) 0.2400(2) 0.0616(12) Uani 1 1 d . . . . .
H22I H 0.979050 0.556344 0.213843 0.092 Uiso 1 1 calc GR . . . .
H22J H 1.035704 0.475669 0.218767 0.092 Uiso 1 1 calc GR . . . .
H22K H 1.014936 0.532906 0.281305 0.092 Uiso 1 1 calc GR . . . .
C22A C 0.6677(2) 0.2789(4) 0.27808(19) 0.0620(12) Uani 1 1 d . U . . .
H22L H 0.652635 0.199894 0.280469 0.074 Uiso 1 1 calc R . . . .
H22M H 0.700810 0.278036 0.251501 0.074 Uiso 1 1 calc R . . . .
C24A C 0.5880(4) 0.3118(9) 0.1848(5) 0.0536(14) Uani 0.588(5) 1 d . U P A 1
H24A H 0.548419 0.346773 0.181062 0.064 Uiso 0.588(5) 1 calc R . P A 1
H24B H 0.608889 0.347012 0.151052 0.064 Uiso 0.588(5) 1 calc R . P A 1
C25A C 0.5802(3) 0.2107(5) 0.1690(3) 0.0407(12) Uani 0.588(5) 1 d . . P A 1
H25A H 0.552424 0.177042 0.196604 0.049 Uiso 0.588(5) 1 calc R . P A 1
H25B H 0.618061 0.170329 0.178387 0.049 Uiso 0.588(5) 1 calc R . P A 1
C26A C 0.5576(4) 0.1843(7) 0.1009(4) 0.062(2) Uani 0.588(5) 1 d . . P A 1
H26A H 0.522729 0.230775 0.088490 0.093 Uiso 0.588(5) 1 calc GR . P A 1
H26B H 0.547331 0.103139 0.096992 0.093 Uiso 0.588(5) 1 calc GR . P A 1
H26C H 0.588054 0.201952 0.073073 0.093 Uiso 0.588(5) 1 calc GR . P A 1
C203 C 0.61912(18) 0.3567(3) 0.24781(17) 0.0461(9) Uani 1 1 d . U . . .
H20I H 0.636199 0.432528 0.240165 0.055 Uiso 0.588(5) 1 calc R . P A 1
H20J H 0.589516 0.367333 0.278222 0.055 Uiso 0.588(5) 1 calc R . P A 1
H20K H 0.582503 0.342569 0.267661 0.055 Uiso 0.412(5) 1 calc R . P A 2
H20L H 0.630411 0.437584 0.255262 0.055 Uiso 0.412(5) 1 calc R . P A 2
C24B C 0.6085(6) 0.3342(13) 0.1765(7) 0.0536(14) Uani 0.412(5) 1 d . U P A 2
H24C H 0.565748 0.344777 0.166392 0.064 Uiso 0.412(5) 1 calc R . P A 2
H24D H 0.626992 0.400141 0.156980 0.064 Uiso 0.412(5) 1 calc R . P A 2
C25B C 0.6207(4) 0.2502(8) 0.1433(4) 0.0407(12) Uani 0.412(5) 1 d . . P A 2
H25C H 0.617744 0.182385 0.170677 0.049 Uiso 0.412(5) 1 calc R . P A 2
H25D H 0.662815 0.258519 0.137517 0.049 Uiso 0.412(5) 1 calc R . P A 2
C26B C 0.5911(6) 0.2158(12) 0.0787(6) 0.062(2) Uani 0.412(5) 1 d . . P A 2
H26D H 0.563586 0.153241 0.083679 0.093 Uiso 0.412(5) 1 calc GR . P A 2
H26E H 0.620925 0.190672 0.051623 0.093 Uiso 0.412(5) 1 calc GR . P A 2
H26F H 0.569849 0.281469 0.059017 0.093 Uiso 0.412(5) 1 calc GR . P A 2
V1 V 0.74091(2) 0.70289(3) 0.38602(2) 0.01358(9) Uani 1 1 d . . . . .
O1 O 0.77911(8) 0.60056(16) 0.36060(9) 0.0207(4) Uani 1 1 d . . . . .
N101 N 0.65607(9) 0.66726(18) 0.35462(10) 0.0153(4) Uani 1 1 d . . . . .
N102 N 0.73577(10) 0.82600(18) 0.31735(10) 0.0152(4) Uani 1 1 d . . . . .
N103 N 0.79768(10) 0.81231(18) 0.43654(10) 0.0154(4) Uani 1 1 d . . . . .
N104 N 0.71950(10) 0.64952(19) 0.47245(10) 0.0160(4) Uani 1 1 d . . . . .
N105 N 0.64673(10) 0.76669(19) 0.25259(11) 0.0172(5) Uani 1 1 d . . . . .
N106 N 0.82303(10) 0.93880(19) 0.35144(11) 0.0176(5) Uani 1 1 d . . . . .
N107 N 0.80287(10) 0.72350(19) 0.54154(11) 0.0175(5) Uani 1 1 d . . . . .
N108 N 0.62887(10) 0.54506(19) 0.44086(11) 0.0173(5) Uani 1 1 d . . . . .
C101 C 0.61980(11) 0.5934(2) 0.38347(12) 0.0154(5) Uani 1 1 d . . . . .
C102 C 0.56679(11) 0.5740(2) 0.34174(12) 0.0160(5) Uani 1 1 d . U . . .
C103 C 0.57240(12) 0.6357(2) 0.28563(13) 0.0161(5) Uani 1 1 d . U . . .
C104 C 0.62799(11) 0.6956(2) 0.29490(12) 0.0149(5) Uani 1 1 d . . . . .
C105 C 0.69613(12) 0.8263(2) 0.26313(12) 0.0163(5) Uani 1 1 d . . . . .
C106 C 0.71612(12) 0.9072(2) 0.21779(13) 0.0175(5) Uani 1 1 d . U . . .
C107 C 0.76846(12) 0.9561(2) 0.24647(13) 0.0176(5) Uani 1 1 d . U . . .
C108 C 0.77928(11) 0.9050(2) 0.30904(12) 0.0156(5) Uani 1 1 d . . . . .
C109 C 0.82968(11) 0.8978(2) 0.41074(13) 0.0161(5) Uani 1 1 d . . . . .
C110 C 0.87422(12) 0.9396(2) 0.45867(13) 0.0173(5) Uani 1 1 d . U . . .
C111 C 0.86941(12) 0.8745(2) 0.51396(13) 0.0177(5) Uani 1 1 d . U . . .
C112 C 0.82095(12) 0.7968(2) 0.49930(13) 0.0165(5) Uani 1 1 d . . . . .
C113 C 0.75640(12) 0.6560(2) 0.52900(12) 0.0172(5) Uani 1 1 d . . . . .
C114 C 0.73537(12) 0.5781(2) 0.57503(13) 0.0187(5) Uani 1 1 d . U . . .
C115 C 0.68443(12) 0.5258(2) 0.54539(13) 0.0187(5) Uani 1 1 d . U . . .
C116 C 0.67515(12) 0.5728(2) 0.48151(13) 0.0173(5) Uani 1 1 d . . . . .
C117 C 0.51624(12) 0.5117(2) 0.34993(13) 0.0202(5) Uani 1 1 d . U . . .
H117 H 0.512256 0.472196 0.388407 0.024 Uiso 1 1 calc R . . . .
C118 C 0.47197(13) 0.5090(3) 0.30034(13) 0.0232(6) Uani 1 1 d . U . . .
H118 H 0.436971 0.467646 0.304927 0.028 Uiso 1 1 calc R . . . .
C119 C 0.47838(12) 0.5670(2) 0.24312(13) 0.0221(6) Uani 1 1 d . U . . .
H119 H 0.447925 0.562192 0.209348 0.027 Uiso 1 1 calc R . . . .
C120 C 0.52805(12) 0.6308(2) 0.23495(13) 0.0198(5) Uani 1 1 d . U . . .
H120 H 0.531943 0.669822 0.196328 0.024 Uiso 1 1 calc R . . . .
C121 C 0.69291(13) 0.9406(3) 0.15685(14) 0.0254(6) Uani 1 1 d . U . . .
H121 H 0.657769 0.907656 0.137276 0.030 Uiso 1 1 calc R . . . .
C122 C 0.72287(14) 1.0234(3) 0.12604(15) 0.0309(7) Uani 1 1 d . U . . .
H122 H 0.707803 1.047372 0.084790 0.037 Uiso 1 1 calc R . . . .
C123 C 0.77499(14) 1.0724(3) 0.15449(14) 0.0267(6) Uani 1 1 d . U . . .
H123 H 0.794366 1.129182 0.132257 0.032 Uiso 1 1 calc R . . . .
C124 C 0.79858(13) 1.0393(2) 0.21448(14) 0.0203(6) Uani 1 1 d . U . . .
H124 H 0.834055 1.071881 0.233451 0.024 Uiso 1 1 calc R . . . .
C125 C 0.91759(12) 1.0236(2) 0.45757(14) 0.0212(6) Uani 1 1 d . U . . .
H125 H 0.920206 1.069435 0.420978 0.025 Uiso 1 1 calc R . . . .
C126 C 0.95659(13) 1.0381(3) 0.51128(14) 0.0246(6) Uani 1 1 d . U . . .
H126 H 0.986771 1.093782 0.511272 0.030 Uiso 1 1 calc R . . . .
C127 C 0.95207(13) 0.9712(3) 0.56613(14) 0.0245(6) Uani 1 1 d . U . . .
H127 H 0.979438 0.982395 0.602317 0.029 Uiso 1 1 calc R . . . .
C128 C 0.90866(12) 0.8900(3) 0.56808(13) 0.0220(6) Uani 1 1 d . U . . .
H128 H 0.905553 0.845790 0.605182 0.026 Uiso 1 1 calc R . . . .
C129 C 0.75627(13) 0.5508(3) 0.63759(13) 0.0227(6) Uani 1 1 d . U . . .
H129 H 0.790199 0.586746 0.658064 0.027 Uiso 1 1 calc R . . . .
C130 C 0.72554(14) 0.4688(3) 0.66876(14) 0.0247(6) Uani 1 1 d . U . . .
H130 H 0.739337 0.447260 0.710829 0.030 Uiso 1 1 calc R . . . .
C131 C 0.67431(14) 0.4174(3) 0.63891(14) 0.0274(6) Uani 1 1 d . U . . .
H131 H 0.653740 0.362932 0.661458 0.033 Uiso 1 1 calc R . . . .
C132 C 0.65357(13) 0.4452(2) 0.57707(14) 0.0238(6) Uani 1 1 d . U . . .
H132 H 0.619205 0.410275 0.556923 0.029 Uiso 1 1 calc R . . . .
Cl1A Cl 0.42985(4) 0.03337(9) 0.57404(4) 0.0471(2) Uani 1 1 d . . . . .
Cl2A Cl 0.54376(4) 0.19026(8) 0.57938(4) 0.0397(2) Uani 1 1 d . . . . .
C1A C 0.44558(14) 0.1124(3) 0.50868(15) 0.0279(6) Uani 1 1 d . U . . .
C2A C 0.49508(13) 0.1813(3) 0.51060(15) 0.0279(7) Uani 1 1 d . U . . .
C3A C 0.50653(13) 0.2442(3) 0.45811(15) 0.0274(6) Uani 1 1 d . U . . .
H3A H 0.539934 0.292635 0.459922 0.033 Uiso 1 1 calc R . . . .
C4A C 0.46869(14) 0.2363(3) 0.40234(16) 0.0290(7) Uani 1 1 d . U . . .
H4A H 0.476939 0.277748 0.365763 0.035 Uiso 1 1 calc R . . . .
C5A C 0.41926(14) 0.1681(3) 0.40031(15) 0.0278(6) Uani 1 1 d . U . . .
H5A H 0.393280 0.163862 0.362533 0.033 Uiso 1 1 calc R . . . .
C6A C 0.40748(14) 0.1059(3) 0.45311(15) 0.0276(6) Uani 1 1 d . U . . .
H6A H 0.373569 0.058844 0.451530 0.033 Uiso 1 1 calc R . . . .


_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
N201 C201 1.524(4) . ?
N201 C207 1.527(4) . ?
N201 C213 1.537(5) . ?
N201 C219 1.526(5) . ?
C201 H20A 0.9900 . ?
C201 H20B 0.9900 . ?
C201 C22A 1.525(5) . ?
C207 H20C 0.9900 . ?
C207 H20D 0.9900 . ?
C207 C208 1.519(5) . ?
C208 H20E 0.9900 . ?
C208 H20F 0.9900 . ?
C208 C209 1.520(5) . ?
C209 H20G 0.9900 . ?
C209 H20H 0.9900 . ?
C209 C210 1.517(5) . ?
C210 H21A 0.9900 . ?
C210 H21B 0.9900 . ?
C210 C211 1.508(5) . ?
C211 H21C 0.9900 . ?
C211 H21D 0.9900 . ?
C211 C212 1.526(5) . ?
C212 H21E 0.9800 . ?
C212 H21F 0.9800 . ?
C212 H21G 0.9800 . ?
C213 H21H 0.9900 . ?
C213 H21I 0.9900 . ?
C213 C214 1.520(5) . ?
C214 H21J 0.9900 . ?
C214 H21K 0.9900 . ?
C214 C215 1.535(5) . ?
C215 H21L 0.9900 . ?
C215 H21M 0.9900 . ?
C215 C216 1.521(5) . ?
C216 H21N 0.9900 . ?
C216 H21O 0.9900 . ?
C216 C217 1.525(5) . ?
C217 H21P 0.9900 . ?
C217 H21Q 0.9900 . ?
C217 C218 1.526(6) . ?
C218 H21R 0.9800 . ?
C218 H21S 0.9800 . ?
C218 H21T 0.9800 . ?
C219 H21U 0.9900 . ?
C219 H21V 0.9900 . ?
C219 C220 1.522(5) . ?
C220 H22A 0.9900 . ?
C220 H22B 0.9900 . ?
C220 C221 1.527(5) . ?
C221 H22C 0.9900 . ?
C221 H22D 0.9900 . ?
C221 C222 1.527(5) . ?
C222 H22E 0.9900 . ?
C222 H22F 0.9900 . ?
C222 C223 1.519(6) . ?
C223 H22G 0.9900 . ?
C223 H22H 0.9900 . ?
C223 C224 1.527(6) . ?
C224 H22I 0.9800 . ?
C224 H22J 0.9800 . ?
C224 H22K 0.9800 . ?
C22A H22L 0.9900 . ?
C22A H22M 0.9900 . ?
C22A C203 1.528(5) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C24A C25A 1.238(11) . ?
C24A C203 1.543(10) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C25A C26A 1.517(9) . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C203 H20I 0.9900 . ?
C203 H20J 0.9900 . ?
C203 H20K 0.9900 . ?
C203 H20L 0.9900 . ?
C203 C24B 1.530(14) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
C24B C25B 1.257(17) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C25B C26B 1.520(14) . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
V1 O1 1.6081(19) . ?
V1 N101 2.034(2) . ?
V1 N102 2.043(2) . ?
V1 N103 2.049(2) . ?
V1 N104 2.042(2) . ?
N101 C101 1.384(3) . ?
N101 C104 1.401(3) . ?
N102 C105 1.392(3) . ?
N102 C108 1.384(3) . ?
N103 C109 1.385(3) . ?
N103 C112 1.395(3) . ?
N104 C113 1.398(3) . ?
N104 C116 1.384(3) . ?
N105 C104 1.327(3) . ?
N105 C105 1.329(3) . ?
N106 C108 1.337(3) . ?
N106 C109 1.340(3) . ?
N107 C112 1.336(3) . ?
N107 C113 1.331(4) . ?
N108 C101 1.339(3) . ?
N108 C116 1.338(4) . ?
C101 C102 1.447(4) . ?
C102 C103 1.409(4) . ?
C102 C117 1.395(4) . ?
C103 C104 1.450(4) . ?
C103 C120 1.404(4) . ?
C105 C106 1.456(4) . ?
C106 C107 1.410(4) . ?
C106 C121 1.402(4) . ?
C107 C108 1.453(4) . ?
C107 C124 1.407(4) . ?
C109 C110 1.451(4) . ?
C110 C111 1.412(4) . ?
C110 C125 1.400(4) . ?
C111 C112 1.445(4) . ?
C111 C128 1.397(4) . ?
C113 C114 1.453(4) . ?
C114 C115 1.409(4) . ?
C114 C129 1.401(4) . ?
C115 C116 1.458(4) . ?
C115 C132 1.391(4) . ?
C117 H117 0.9500 . ?
C117 C118 1.386(4) . ?
C118 H118 0.9500 . ?
C118 C119 1.411(4) . ?
C119 H119 0.9500 . ?
C119 C120 1.387(4) . ?
C120 H120 0.9500 . ?
C121 H121 0.9500 . ?
C121 C122 1.388(4) . ?
C122 H122 0.9500 . ?
C122 C123 1.406(4) . ?
C123 H123 0.9500 . ?
C123 C124 1.387(4) . ?
C124 H124 0.9500 . ?
C125 H125 0.9500 . ?
C125 C126 1.386(4) . ?
C126 H126 0.9500 . ?
C126 C127 1.415(4) . ?
C127 H127 0.9500 . ?
C127 C128 1.380(4) . ?
C128 H128 0.9500 . ?
C129 H129 0.9500 . ?
C129 C130 1.395(4) . ?
C130 H130 0.9500 . ?
C130 C131 1.411(4) . ?
C131 H131 0.9500 . ?
C131 C132 1.388(4) . ?
C132 H132 0.9500 . ?
Cl1A C1A 1.734(3) . ?
Cl2A C2A 1.748(3) . ?
C1A C2A 1.389(5) . ?
C1A C6A 1.396(4) . ?
C2A C3A 1.381(5) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.397(4) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.383(5) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.385(5) . ?
C6A H6A 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
C201 N201 C207 107.0(2) . . ?
C201 N201 C213 111.1(3) . . ?
C201 N201 C219 110.6(3) . . ?
C207 N201 C213 110.7(3) . . ?
C219 N201 C207 111.7(3) . . ?
C219 N201 C213 105.8(2) . . ?
N201 C201 H20A 108.7 . . ?
N201 C201 H20B 108.7 . . ?
N201 C201 C22A 114.4(3) . . ?
H20A C201 H20B 107.6 . . ?
C22A C201 H20A 108.7 . . ?
C22A C201 H20B 108.7 . . ?
N201 C207 H20C 108.3 . . ?
N201 C207 H20D 108.3 . . ?
H20C C207 H20D 107.4 . . ?
C208 C207 N201 115.8(3) . . ?
C208 C207 H20C 108.3 . . ?
C208 C207 H20D 108.3 . . ?
C207 C208 H20E 109.4 . . ?
C207 C208 H20F 109.4 . . ?
C207 C208 C209 111.0(3) . . ?
H20E C208 H20F 108.0 . . ?
C209 C208 H20E 109.4 . . ?
C209 C208 H20F 109.4 . . ?
C208 C209 H20G 109.0 . . ?
C208 C209 H20H 109.0 . . ?
H20G C209 H20H 107.8 . . ?
C210 C209 C208 113.1(3) . . ?
C210 C209 H20G 109.0 . . ?
C210 C209 H20H 109.0 . . ?
C209 C210 H21A 108.7 . . ?
C209 C210 H21B 108.7 . . ?
H21A C210 H21B 107.6 . . ?
C211 C210 C209 114.1(3) . . ?
C211 C210 H21A 108.7 . . ?
C211 C210 H21B 108.7 . . ?
C210 C211 H21C 108.9 . . ?
C210 C211 H21D 108.9 . . ?
C210 C211 C212 113.4(3) . . ?
H21C C211 H21D 107.7 . . ?
C212 C211 H21C 108.9 . . ?
C212 C211 H21D 108.9 . . ?
C211 C212 H21E 109.5 . . ?
C211 C212 H21F 109.5 . . ?
C211 C212 H21G 109.5 . . ?
H21E C212 H21F 109.5 . . ?
H21E C212 H21G 109.5 . . ?
H21F C212 H21G 109.5 . . ?
N201 C213 H21H 108.0 . . ?
N201 C213 H21I 108.0 . . ?
H21H C213 H21I 107.2 . . ?
C214 C213 N201 117.2(3) . . ?
C214 C213 H21H 108.0 . . ?
C214 C213 H21I 108.0 . . ?
C213 C214 H21J 109.8 . . ?
C213 C214 H21K 109.8 . . ?
C213 C214 C215 109.5(3) . . ?
H21J C214 H21K 108.2 . . ?
C215 C214 H21J 109.8 . . ?
C215 C214 H21K 109.8 . . ?
C214 C215 H21L 109.0 . . ?
C214 C215 H21M 109.0 . . ?
H21L C215 H21M 107.8 . . ?
C216 C215 C214 113.1(3) . . ?
C216 C215 H21L 109.0 . . ?
C216 C215 H21M 109.0 . . ?
C215 C216 H21N 109.1 . . ?
C215 C216 H21O 109.1 . . ?
C215 C216 C217 112.7(3) . . ?
H21N C216 H21O 107.8 . . ?
C217 C216 H21N 109.1 . . ?
C217 C216 H21O 109.1 . . ?
C216 C217 H21P 109.0 . . ?
C216 C217 H21Q 109.0 . . ?
H21P C217 H21Q 107.8 . . ?
C218 C217 C216 113.0(3) . . ?
C218 C217 H21P 109.0 . . ?
C218 C217 H21Q 109.0 . . ?
C217 C218 H21R 109.5 . . ?
C217 C218 H21S 109.5 . . ?
C217 C218 H21T 109.5 . . ?
H21R C218 H21S 109.5 . . ?
H21R C218 H21T 109.5 . . ?
H21S C218 H21T 109.5 . . ?
N201 C219 H21U 108.2 . . ?
N201 C219 H21V 108.2 . . ?
H21U C219 H21V 107.3 . . ?
C220 C219 N201 116.4(3) . . ?
C220 C219 H21U 108.2 . . ?
C220 C219 H21V 108.2 . . ?
C219 C220 H22A 109.7 . . ?
C219 C220 H22B 109.7 . . ?
C219 C220 C221 110.0(3) . . ?
H22A C220 H22B 108.2 . . ?
C221 C220 H22A 109.7 . . ?
C221 C220 H22B 109.7 . . ?
C220 C221 H22C 108.9 . . ?
C220 C221 H22D 108.9 . . ?
C220 C221 C222 113.2(3) . . ?
H22C C221 H22D 107.7 . . ?
C222 C221 H22C 108.9 . . ?
C222 C221 H22D 108.9 . . ?
C221 C222 H22E 109.0 . . ?
C221 C222 H22F 109.0 . . ?
H22E C222 H22F 107.8 . . ?
C223 C222 C221 112.9(3) . . ?
C223 C222 H22E 109.0 . . ?
C223 C222 H22F 109.0 . . ?
C222 C223 H22G 108.8 . . ?
C222 C223 H22H 108.8 . . ?
C222 C223 C224 114.0(3) . . ?
H22G C223 H22H 107.7 . . ?
C224 C223 H22G 108.8 . . ?
C224 C223 H22H 108.8 . . ?
C223 C224 H22I 109.5 . . ?
C223 C224 H22J 109.5 . . ?
C223 C224 H22K 109.5 . . ?
H22I C224 H22J 109.5 . . ?
H22I C224 H22K 109.5 . . ?
H22J C224 H22K 109.5 . . ?
C201 C22A H22L 109.6 . . ?
C201 C22A H22M 109.6 . . ?
C201 C22A C203 110.4(3) . . ?
H22L C22A H22M 108.1 . . ?
C203 C22A H22L 109.6 . . ?
C203 C22A H22M 109.6 . . ?
H24A C24A H24B 106.1 . . ?
C25A C24A H24A 105.6 . . ?
C25A C24A H24B 105.6 . . ?
C25A C24A C203 126.9(8) . . ?
C203 C24A H24A 105.6 . . ?
C203 C24A H24B 105.6 . . ?
C24A C25A H25A 107.7 . . ?
C24A C25A H25B 107.7 . . ?
C24A C25A C26A 118.6(7) . . ?
H25A C25A H25B 107.1 . . ?
C26A C25A H25A 107.7 . . ?
C26A C25A H25B 107.7 . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C22A C203 C24A 114.5(4) . . ?
C22A C203 H20I 108.6 . . ?
C22A C203 H20J 108.6 . . ?
C22A C203 H20K 109.6 . . ?
C22A C203 H20L 109.6 . . ?
C24A C203 H20I 108.6 . . ?
C24A C203 H20J 108.6 . . ?
H20I C203 H20J 107.6 . . ?
H20K C203 H20L 108.1 . . ?
C24B C203 C22A 110.4(6) . . ?
C24B C203 H20K 109.6 . . ?
C24B C203 H20L 109.6 . . ?
C203 C24B H24C 104.3 . . ?
C203 C24B H24D 104.3 . . ?
H24C C24B H24D 105.6 . . ?
C25B C24B C203 131.7(12) . . ?
C25B C24B H24C 104.3 . . ?
C25B C24B H24D 104.3 . . ?
C24B C25B H25C 105.4 . . ?
C24B C25B H25D 105.4 . . ?
C24B C25B C26B 127.4(11) . . ?
H25C C25B H25D 106.0 . . ?
C26B C25B H25C 105.4 . . ?
C26B C25B H25D 105.4 . . ?
C25B C26B H26D 109.5 . . ?
C25B C26B H26E 109.5 . . ?
C25B C26B H26F 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
O1 V1 N101 105.81(9) . . ?
O1 V1 N102 106.29(9) . . ?
O1 V1 N103 107.58(9) . . ?
O1 V1 N104 105.14(10) . . ?
N101 V1 N102 85.80(9) . . ?
N101 V1 N103 146.61(9) . . ?
N101 V1 N104 85.58(9) . . ?
N102 V1 N103 85.40(9) . . ?
N104 V1 N102 148.57(9) . . ?
N104 V1 N103 85.37(9) . . ?
C101 N101 V1 125.47(17) . . ?
C101 N101 C104 107.8(2) . . ?
C104 N101 V1 125.76(17) . . ?
C105 N102 V1 125.18(17) . . ?
C108 N102 V1 124.84(18) . . ?
C108 N102 C105 108.2(2) . . ?
C109 N103 V1 125.33(17) . . ?
C109 N103 C112 107.7(2) . . ?
C112 N103 V1 125.38(17) . . ?
C113 N104 V1 125.03(18) . . ?
C116 N104 V1 124.69(18) . . ?
C116 N104 C113 107.8(2) . . ?
C104 N105 C105 122.9(2) . . ?
C108 N106 C109 122.1(2) . . ?
C113 N107 C112 122.9(2) . . ?
C116 N108 C101 121.6(2) . . ?
N101 C101 C102 109.4(2) . . ?
N108 C101 N101 128.4(2) . . ?
N108 C101 C102 122.2(2) . . ?
C103 C102 C101 107.1(2) . . ?
C117 C102 C101 131.5(3) . . ?
C117 C102 C103 121.4(2) . . ?
C102 C103 C104 106.7(2) . . ?
C120 C103 C102 120.3(2) . . ?
C120 C103 C104 133.0(3) . . ?
N101 C104 C103 109.0(2) . . ?
N105 C104 N101 127.5(2) . . ?
N105 C104 C103 123.5(2) . . ?
N102 C105 C106 108.9(2) . . ?
N105 C105 N102 127.7(2) . . ?
N105 C105 C106 123.3(2) . . ?
C107 C106 C105 106.8(2) . . ?
C121 C106 C105 132.4(3) . . ?
C121 C106 C107 120.8(2) . . ?
C106 C107 C108 106.7(2) . . ?
C124 C107 C106 120.7(3) . . ?
C124 C107 C108 132.7(3) . . ?
N102 C108 C107 109.4(2) . . ?
N106 C108 N102 127.8(2) . . ?
N106 C108 C107 122.7(2) . . ?
N103 C109 C110 109.3(2) . . ?
N106 C109 N103 127.9(2) . . ?
N106 C109 C110 122.8(2) . . ?
C111 C110 C109 106.9(2) . . ?
C125 C110 C109 132.5(3) . . ?
C125 C110 C111 120.5(3) . . ?
C110 C111 C112 106.5(2) . . ?
C128 C111 C110 121.0(3) . . ?
C128 C111 C112 132.5(3) . . ?
N103 C112 C111 109.6(2) . . ?
N107 C112 N103 127.5(2) . . ?
N107 C112 C111 122.9(2) . . ?
N104 C113 C114 109.2(2) . . ?
N107 C113 N104 127.3(2) . . ?
N107 C113 C114 123.4(2) . . ?
C115 C114 C113 106.8(2) . . ?
C129 C114 C113 132.4(3) . . ?
C129 C114 C115 120.8(3) . . ?
C114 C115 C116 106.7(2) . . ?
C132 C115 C114 121.2(3) . . ?
C132 C115 C116 132.1(3) . . ?
N104 C116 C115 109.5(2) . . ?
N108 C116 N104 127.9(2) . . ?
N108 C116 C115 122.6(2) . . ?
C102 C117 H117 120.9 . . ?
C118 C117 C102 118.1(3) . . ?
C118 C117 H117 120.9 . . ?
C117 C118 H118 119.7 . . ?
C117 C118 C119 120.6(3) . . ?
C119 C118 H118 119.7 . . ?
C118 C119 H119 119.2 . . ?
C120 C119 C118 121.6(3) . . ?
C120 C119 H119 119.2 . . ?
C103 C120 H120 121.1 . . ?
C119 C120 C103 117.8(3) . . ?
C119 C120 H120 121.1 . . ?
C106 C121 H121 121.0 . . ?
C122 C121 C106 117.9(3) . . ?
C122 C121 H121 121.0 . . ?
C121 C122 H122 119.2 . . ?
C121 C122 C123 121.5(3) . . ?
C123 C122 H122 119.2 . . ?
C122 C123 H123 119.5 . . ?
C124 C123 C122 121.0(3) . . ?
C124 C123 H123 119.5 . . ?
C107 C124 H124 120.9 . . ?
C123 C124 C107 118.1(3) . . ?
C123 C124 H124 120.9 . . ?
C110 C125 H125 120.9 . . ?
C126 C125 C110 118.2(3) . . ?
C126 C125 H125 120.9 . . ?
C125 C126 H126 119.6 . . ?
C125 C126 C127 120.9(3) . . ?
C127 C126 H126 119.6 . . ?
C126 C127 H127 119.4 . . ?
C128 C127 C126 121.3(3) . . ?
C128 C127 H127 119.4 . . ?
C111 C128 H128 120.9 . . ?
C127 C128 C111 118.1(3) . . ?
C127 C128 H128 120.9 . . ?
C114 C129 H129 121.2 . . ?
C130 C129 C114 117.7(3) . . ?
C130 C129 H129 121.2 . . ?
C129 C130 H130 119.4 . . ?
C129 C130 C131 121.2(3) . . ?
C131 C130 H130 119.4 . . ?
C130 C131 H131 119.5 . . ?
C132 C131 C130 120.9(3) . . ?
C132 C131 H131 119.5 . . ?
C115 C132 H132 120.9 . . ?
C131 C132 C115 118.2(3) . . ?
C131 C132 H132 120.9 . . ?
C2A C1A Cl1A 121.4(2) . . ?
C2A C1A C6A 119.8(3) . . ?
C6A C1A Cl1A 118.8(3) . . ?
C1A C2A Cl2A 120.7(3) . . ?
C3A C2A Cl2A 118.9(2) . . ?
C3A C2A C1A 120.4(3) . . ?
C2A C3A H3A 120.2 . . ?
C2A C3A C4A 119.6(3) . . ?
C4A C3A H3A 120.2 . . ?
C3A C4A H4A 120.0 . . ?
C5A C4A C3A 120.1(3) . . ?
C5A C4A H4A 120.0 . . ?
C4A C5A H5A 119.9 . . ?
C4A C5A C6A 120.3(3) . . ?
C6A C5A H5A 119.9 . . ?
C1A C6A H6A 120.1 . . ?
C5A C6A C1A 119.8(3) . . ?
C5A C6A H6A 120.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.134
_oxdiff_exptl_absorpt_empirical_full_min 0.915
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.633(18)
2 0.367(18)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane-o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_TiOPcMDABCO
_database_code_depnum_ccdc_archive 'CCDC 1581407'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of titanyl phthalocyanine with N-methyldiazabicyclooctanium cation'
_chemical_formula_moiety         'C32 H16 N8 O Ti, 1(C7 H15 N2)'
_chemical_formula_sum            'C39 H31 N10 O Ti'
_chemical_formula_weight         703.64
_chemical_melting_point          'not measured'
_chemical_oxdiff_formula         'C39 H31 N10 Ti1 O1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.5955(11)
_cell_length_b                   17.1171(10)
_cell_length_c                   19.1812(13)
_cell_angle_alpha                90
_cell_angle_beta                 99.444(6)
_cell_angle_gamma                90
_cell_volume                     6346.5(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      28.2600
_cell_measurement_theta_min      2.1040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2920
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 5 4 0.0346
-4 -4 5 0.0418
5 -5 -4 0.0346
1 1 0 0.0707
-1 -1 0 0.0707
-4 5 -3 0.0636
-5 0 -2 0.0775
5 -5 1 0.0669
4 5 -4 0.0418

_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.069
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9877 4.9824 3.9870 -0.0003 0.2964 0.0405
-3.9846 -3.9908 4.9922 0.2681 0.0333 0.0422
4.9877 -4.9824 -3.9870 0.0003 -0.2964 -0.0405
0.9966 0.9967 -0.0015 -0.0370 0.0144 -0.0383
-0.9966 -0.9967 0.0015 0.0370 -0.0144 0.0383
-3.9930 4.9878 -2.9944 -0.1774 0.1537 0.1638
-4.9868 0.0027 -1.9918 -0.0039 0.0392 0.2047
4.9895 -4.9864 0.9993 0.1205 -0.2052 -0.1514
3.9843 4.9869 -3.9959 -0.2722 0.0145 -0.0706

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19120
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.111
_diffrn_reflns_theta_min         1.589
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -91.00  16.00   0.50  150.00    --  -14.62 -77.00  90.00  214
  2  ω    -66.00  41.00   0.50  150.00    --   16.65 -37.00 150.00  214
  3  ω    -71.00 -23.00   0.50  150.00    --  -14.62 -77.00  30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0088603000
_diffrn_orient_matrix_UB_12      -0.0282053000
_diffrn_orient_matrix_UB_13      0.0240793000
_diffrn_orient_matrix_UB_21      -0.0151518000
_diffrn_orient_matrix_UB_22      0.0296675000
_diffrn_orient_matrix_UB_23      0.0183007000
_diffrn_orient_matrix_UB_31      -0.0321752000
_diffrn_orient_matrix_UB_32      -0.0062824000
_diffrn_orient_matrix_UB_33      -0.0222471000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4546
_reflns_number_total             7370
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7370
_refine_ls_number_restraints     346
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      0.997
_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)+(0.0584P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1467
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim
C301 \\sim C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306 \\sim C307 \\sim
C401 \\sim C402 \\sim C403 \\sim C404 \\sim C405 \\sim C406 \\sim C407: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N201 \\sim N302 \\sim N402 \\sim N202 \\sim N301 \\sim N401: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N301) = Uanis(N302)
Uanis(C303) = Uanis(C207)
Uanis(C203) = Uanis(C307)
Uanis(C206) = Uanis(C306)
Uanis(C407) = Uanis(C307)
Uanis(N202) = Uanis(N201)
Uanis(N401) = Uanis(N402)
3. Same fragment restrains
{N201, N202, C201, C202, C203, C204, C205, C206, C207} sigma for 1-2: 0.001,
1-3: 0.001
as
{N301, N302, C301, C302, C303, C304, C305, C306, C307}
{N201, N202, C201, C202, C203, C204, C205, C206, C207} sigma for 1-2: 0.001,
1-3: 0.001
as
{N401, N402, C401, C402, C403, C404, C405, C406, C407}
4. Others
 1*[Sof(N201)+Sof(N202)+Sof(C201)+Sof(H20A)+Sof(H20B)+Sof(C202)+Sof(H20C)+
 Sof(H20D)+Sof(C203)+Sof(H20E)+Sof(H20F)+Sof(C204)+Sof(H20G)+Sof(H20H)+
 Sof(C205)+Sof(H20I)+Sof(H20J)+Sof(C206)+Sof(H20K)+Sof(H20L)+Sof(C207)+
 Sof(H20M)+Sof(H20N)+Sof(H20O)]+1*[Sof(N301)+Sof(N302)+Sof(C301)+Sof(H30A)+
 Sof(H30B)+Sof(C302)+Sof(H30C)+Sof(H30D)+Sof(C303)+Sof(H30E)+Sof(H30F)+
 Sof(C304)+Sof(H30G)+Sof(H30H)+Sof(C305)+Sof(H30I)+Sof(H30J)+Sof(C306)+
 Sof(H30K)+Sof(H30L)+Sof(C307)+Sof(H30M)+Sof(H30N)+Sof(H30O)]+1*[Sof(N401)+
 Sof(N402)+Sof(C401)+Sof(H40A)+Sof(H40B)+Sof(C402)+Sof(H40C)+Sof(H40D)+
 Sof(C403)+Sof(H40E)+Sof(H40F)+Sof(C404)+Sof(H40G)+Sof(H40H)+Sof(C405)+
 Sof(H40I)+Sof(H40J)+Sof(C406)+Sof(H40K)+Sof(H40L)+Sof(C407)+Sof(H40M)+
 Sof(H40N)+Sof(H40O)]=1 with esd of 0.0001
 Sof(N201)=Sof(N202)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(C202)=Sof(H20C)=
 Sof(H20D)=Sof(C203)=Sof(H20E)=Sof(H20F)=Sof(C204)=Sof(H20G)=Sof(H20H)=
 Sof(C205)=Sof(H20I)=Sof(H20J)=Sof(C206)=Sof(H20K)=Sof(H20L)=Sof(C207)=
 Sof(H20M)=Sof(H20N)=Sof(H20O)=FVAR(1)
 Sof(N301)=Sof(N302)=Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(C302)=Sof(H30C)=
 Sof(H30D)=Sof(C303)=Sof(H30E)=Sof(H30F)=Sof(C304)=Sof(H30G)=Sof(H30H)=
 Sof(C305)=Sof(H30I)=Sof(H30J)=Sof(C306)=Sof(H30K)=Sof(H30L)=Sof(C307)=
 Sof(H30M)=Sof(H30N)=Sof(H30O)=FVAR(2)
 Sof(N401)=Sof(N402)=Sof(C401)=Sof(H40A)=Sof(H40B)=Sof(C402)=Sof(H40C)=
 Sof(H40D)=Sof(C403)=Sof(H40E)=Sof(H40F)=Sof(C404)=Sof(H40G)=Sof(H40H)=
 Sof(C405)=Sof(H40I)=Sof(H40J)=Sof(C406)=Sof(H40K)=Sof(H40L)=Sof(C407)=
 Sof(H40M)=Sof(H40N)=Sof(H40O)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F),
 C304(H30G,H30H), C305(H30I,H30J), C306(H30K,H30L), C401(H40A,H40B), C402(H40C,
 H40D), C403(H40E,H40F), C404(H40G,H40H), C405(H40I,H40J), C406(H40K,H40L)
5.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132)
5.c Idealised Me refined with everything fixed:
 C407(H40M,H40N,H40O)
5.d Idealised Me refined as rotating group:
 C207(H20M,H20N,H20O), C307(H30M,H30N,H30O)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti01 Ti 0.34429(2) 0.66119(3) 0.49073(3) 0.02233(15) Uani 1 1 d . . . . .
O101 O 0.38103(9) 0.58058(11) 0.46840(10) 0.0321(5) Uani 1 1 d . . . . .
N101 N 0.33570(10) 0.73811(12) 0.40715(12) 0.0221(5) Uani 1 1 d . . . . .
N102 N 0.42364(10) 0.73095(13) 0.53737(12) 0.0233(5) Uani 1 1 d . . . . .
N103 N 0.32714(11) 0.64232(13) 0.59229(12) 0.0255(5) Uani 1 1 d . . . . .
N104 N 0.23939(10) 0.64848(12) 0.46166(12) 0.0225(5) Uani 1 1 d . . . . .
N105 N 0.44790(11) 0.80266(13) 0.43509(13) 0.0262(6) Uani 1 1 d . . . . .
N106 N 0.43900(11) 0.68263(14) 0.65808(13) 0.0281(6) Uani 1 1 d . . . . .
N107 N 0.21404(11) 0.57966(13) 0.56514(13) 0.0257(5) Uani 1 1 d . . . . .
N108 N 0.22394(11) 0.69666(13) 0.34138(12) 0.0237(5) Uani 1 1 d . . . . .
C101 C 0.28475(13) 0.73601(16) 0.34825(15) 0.0233(6) Uani 1 1 d . . . . .
C102 C 0.30660(13) 0.78153(16) 0.29285(15) 0.0244(6) Uani 1 1 d . . . . .
C103 C 0.37206(13) 0.81210(16) 0.32106(15) 0.0263(7) Uani 1 1 d . . . . .
C104 C 0.38889(13) 0.78445(16) 0.39161(15) 0.0241(6) Uani 1 1 d . . . . .
C105 C 0.46220(13) 0.77938(16) 0.50065(16) 0.0255(6) Uani 1 1 d . . . . .
C106 C 0.52502(13) 0.80205(16) 0.54879(16) 0.0257(6) Uani 1 1 d . . . . .
C107 C 0.52232(13) 0.76683(16) 0.61397(15) 0.0254(6) Uani 1 1 d . . . . .
C108 C 0.45827(13) 0.72269(16) 0.60611(15) 0.0248(6) Uani 1 1 d . . . . .
C109 C 0.37763(14) 0.64527(16) 0.65146(16) 0.0271(7) Uani 1 1 d . . . . .
C110 C 0.35589(15) 0.59995(17) 0.70684(16) 0.0320(7) Uani 1 1 d . . . . .
C111 C 0.29003(14) 0.57072(17) 0.67951(16) 0.0283(7) Uani 1 1 d . . . . .
C112 C 0.27270(13) 0.59891(16) 0.60895(15) 0.0259(6) Uani 1 1 d . . . . .
C113 C 0.19990(13) 0.60309(16) 0.49906(16) 0.0246(6) Uani 1 1 d . . . . .
C114 C 0.13762(13) 0.57962(16) 0.45236(15) 0.0243(6) Uani 1 1 d . . . . .
C115 C 0.13925(13) 0.61330(15) 0.38647(15) 0.0231(6) Uani 1 1 d . . . . .
C116 C 0.20422(13) 0.65770(15) 0.39355(15) 0.0223(6) Uani 1 1 d . . . . .
C117 C 0.27597(14) 0.79896(17) 0.22384(15) 0.0289(7) Uani 1 1 d . . . . .
H117 H 0.232335 0.779733 0.205462 0.035 Uiso 1 1 calc R . . . .
C118 C 0.31145(15) 0.84501(18) 0.18362(17) 0.0355(8) Uani 1 1 d . . . . .
H118 H 0.291828 0.856663 0.137302 0.043 Uiso 1 1 calc R . . . .
C119 C 0.37737(15) 0.87502(19) 0.21147(17) 0.0389(8) Uani 1 1 d . . . . .
H119 H 0.400516 0.906153 0.183185 0.047 Uiso 1 1 calc R . . . .
C120 C 0.40767(15) 0.85917(18) 0.27906(17) 0.0344(8) Uani 1 1 d . . . . .
H120 H 0.451133 0.879160 0.297045 0.041 Uiso 1 1 calc R . . . .
C121 C 0.57917(13) 0.85024(16) 0.53909(16) 0.0299(7) Uani 1 1 d . . . . .
H121 H 0.581146 0.872937 0.495416 0.036 Uiso 1 1 calc R . . . .
C122 C 0.63019(14) 0.86353(18) 0.59637(17) 0.0355(8) Uani 1 1 d . . . . .
H122 H 0.666918 0.896317 0.591367 0.043 Uiso 1 1 calc R . . . .
C123 C 0.62786(14) 0.82881(17) 0.66169(17) 0.0330(7) Uani 1 1 d . . . . .
H123 H 0.662860 0.839143 0.699516 0.040 Uiso 1 1 calc R . . . .
C124 C 0.57445(13) 0.77932(16) 0.67118(16) 0.0298(7) Uani 1 1 d . . . . .
H124 H 0.573462 0.755191 0.714449 0.036 Uiso 1 1 calc R . . . .
C125 C 0.38925(17) 0.57910(19) 0.77421(17) 0.0431(9) Uani 1 1 d . . . . .
H125 H 0.432742 0.598682 0.792644 0.052 Uiso 1 1 calc R . . . .
C126 C 0.35503(18) 0.5282(2) 0.81233(18) 0.0516(10) Uani 1 1 d . . . . .
H126 H 0.376173 0.513007 0.857260 0.062 Uiso 1 1 calc R . . . .
C127 C 0.28995(17) 0.4991(2) 0.78546(18) 0.0460(9) Uani 1 1 d . . . . .
H127 H 0.268735 0.464585 0.812623 0.055 Uiso 1 1 calc R . . . .
C128 C 0.25605(16) 0.52017(18) 0.71961(17) 0.0371(8) Uani 1 1 d . . . . .
H128 H 0.211985 0.501383 0.702346 0.045 Uiso 1 1 calc R . . . .
C129 C 0.08408(13) 0.53146(16) 0.46423(16) 0.0282(7) Uani 1 1 d . . . . .
H129 H 0.083270 0.509715 0.508524 0.034 Uiso 1 1 calc R . . . .
C130 C 0.03173(13) 0.51665(17) 0.40809(16) 0.0298(7) Uani 1 1 d . . . . .
H130 H -0.004288 0.483273 0.414132 0.036 Uiso 1 1 calc R . . . .
C131 C 0.03257(13) 0.55103(16) 0.34322(16) 0.0280(7) Uani 1 1 d . . . . .
H131 H -0.003683 0.541186 0.306509 0.034 Uiso 1 1 calc R . . . .
C132 C 0.08572(13) 0.59968(16) 0.33115(16) 0.0274(7) Uani 1 1 d . . . . .
H132 H 0.085500 0.622589 0.287154 0.033 Uiso 1 1 calc R . . . .
N201 N 0.3039(2) 0.3525(3) 0.5084(3) 0.0565(12) Uani 0.597(2) 1 d D U P A 1
N202 N 0.4223(2) 0.3847(3) 0.5827(3) 0.0565(12) Uani 0.597(2) 1 d D U P A 1
C201 C 0.3035(3) 0.4286(3) 0.5417(4) 0.077(2) Uani 0.597(2) 1 d D U P A 1
H20A H 0.263397 0.432292 0.565162 0.092 Uiso 0.597(2) 1 calc R . P A 1
H20B H 0.299332 0.468723 0.505515 0.092 Uiso 0.597(2) 1 calc R . P A 1
C202 C 0.3698(3) 0.4438(3) 0.5964(4) 0.0546(19) Uani 0.597(2) 1 d D U P A 1
H20C H 0.386899 0.496281 0.590867 0.066 Uiso 0.597(2) 1 calc R . P A 1
H20D H 0.360003 0.438284 0.644070 0.066 Uiso 0.597(2) 1 calc R . P A 1
C203 C 0.3598(3) 0.3553(4) 0.4631(4) 0.068(2) Uani 0.597(2) 1 d D U P A 1
H20E H 0.368284 0.303059 0.446825 0.082 Uiso 0.597(2) 1 calc R . P A 1
H20F H 0.344803 0.387697 0.421922 0.082 Uiso 0.597(2) 1 calc R . P A 1
C204 C 0.4254(3) 0.3879(3) 0.5042(3) 0.0512(17) Uani 0.597(2) 1 d D U P A 1
H20G H 0.431379 0.441491 0.490023 0.061 Uiso 0.597(2) 1 calc R . P A 1
H20H H 0.464604 0.357715 0.494286 0.061 Uiso 0.597(2) 1 calc R . P A 1
C205 C 0.3240(3) 0.2953(3) 0.5601(3) 0.0602(18) Uani 0.597(2) 1 d D U P A 1
H20I H 0.318718 0.244256 0.537926 0.072 Uiso 0.597(2) 1 calc R . P A 1
H20J H 0.293173 0.297649 0.594745 0.072 Uiso 0.597(2) 1 calc R . P A 1
C206 C 0.3950(4) 0.3036(3) 0.5964(4) 0.0567(13) Uani 0.597(2) 1 d D U P A 1
H20K H 0.423880 0.264083 0.579563 0.068 Uiso 0.597(2) 1 calc R . P A 1
H20L H 0.396683 0.296005 0.646756 0.068 Uiso 0.597(2) 1 calc R . P A 1
C207 C 0.4885(3) 0.4028(4) 0.6250(4) 0.0674(18) Uani 0.597(2) 1 d D U P A 1
H20M H 0.504015 0.452916 0.611449 0.101 Uiso 0.597(2) 1 calc GR . P A 1
H20N H 0.521640 0.363589 0.617537 0.101 Uiso 0.597(2) 1 calc GR . P A 1
H20O H 0.483937 0.403819 0.674043 0.101 Uiso 0.597(2) 1 calc GR . P A 1
N301 N 0.4647(4) 0.3739(5) 0.6802(4) 0.068(3) Uani 0.246(3) 1 d D U P B 2
N302 N 0.3823(4) 0.3712(5) 0.5611(4) 0.068(3) Uani 0.246(3) 1 d D U P B 2
C301 C 0.4119(5) 0.4338(5) 0.6769(5) 0.072(4) Uani 0.246(3) 1 d D U P B 2
H30A H 0.433539 0.484776 0.676491 0.087 Uiso 0.246(3) 1 calc R . P B 2
H30B H 0.390608 0.430656 0.719054 0.087 Uiso 0.246(3) 1 calc R . P B 2
C302 C 0.3551(5) 0.4259(5) 0.6108(5) 0.075(5) Uani 0.246(3) 1 d D U P B 2
H30C H 0.312853 0.405386 0.623926 0.089 Uiso 0.246(3) 1 calc R . P B 2
H30D H 0.345099 0.476485 0.588575 0.089 Uiso 0.246(3) 1 calc R . P B 2
C303 C 0.5031(4) 0.3896(8) 0.6197(5) 0.0674(18) Uani 0.246(3) 1 d D U P B 2
H30E H 0.531314 0.436042 0.629692 0.081 Uiso 0.246(3) 1 calc R . P B 2
H30F H 0.533539 0.345981 0.614625 0.081 Uiso 0.246(3) 1 calc R . P B 2
C304 C 0.4534(4) 0.4007(6) 0.5523(4) 0.058(4) Uani 0.246(3) 1 d D U P B 2
H30G H 0.469597 0.372378 0.514349 0.070 Uiso 0.246(3) 1 calc R . P B 2
H30H H 0.450707 0.455691 0.539836 0.070 Uiso 0.246(3) 1 calc R . P B 2
C305 C 0.4334(5) 0.3005(5) 0.6675(5) 0.064(4) Uani 0.246(3) 1 d D U P B 2
H30I H 0.402827 0.291843 0.701757 0.077 Uiso 0.246(3) 1 calc R . P B 2
H30J H 0.469020 0.260620 0.674916 0.077 Uiso 0.246(3) 1 calc R . P B 2
C306 C 0.3939(6) 0.2915(4) 0.5968(6) 0.0567(13) Uani 0.246(3) 1 d D U P B 2
H30K H 0.349639 0.267358 0.599614 0.068 Uiso 0.246(3) 1 calc R . P B 2
H30L H 0.418786 0.257778 0.568998 0.068 Uiso 0.246(3) 1 calc R . P B 2
C307 C 0.3354(6) 0.3694(8) 0.4944(5) 0.068(2) Uani 0.246(3) 1 d D U P B 2
H30M H 0.290046 0.354556 0.502397 0.102 Uiso 0.246(3) 1 calc GR . P B 2
H30N H 0.351632 0.332152 0.463444 0.102 Uiso 0.246(3) 1 calc GR . P B 2
H30O H 0.333331 0.420241 0.473031 0.102 Uiso 0.246(3) 1 calc GR . P B 2
N401 N 0.4655(5) 0.3847(6) 0.6917(4) 0.062(4) Uani 0.157(2) 1 d D U P C 3
N402 N 0.3968(5) 0.3866(5) 0.5653(4) 0.062(4) Uani 0.157(2) 1 d D U P C 3
C401 C 0.4824(6) 0.4529(6) 0.6530(6) 0.086(6) Uani 0.157(2) 1 d D U P C 3
H40A H 0.529924 0.448832 0.645236 0.104 Uiso 0.157(2) 1 calc R . P C 3
H40B H 0.478684 0.499181 0.681309 0.104 Uiso 0.157(2) 1 calc R . P C 3
C402 C 0.4344(6) 0.4622(5) 0.5807(6) 0.080(5) Uani 0.157(2) 1 d D U P C 3
H40C H 0.401741 0.504426 0.582730 0.097 Uiso 0.157(2) 1 calc R . P C 3
H40D H 0.461466 0.473972 0.543946 0.097 Uiso 0.157(2) 1 calc R . P C 3
C403 C 0.3889(5) 0.3882(9) 0.6925(5) 0.067(6) Uani 0.157(2) 1 d D U P C 3
H40E H 0.376157 0.347556 0.723201 0.080 Uiso 0.157(2) 1 calc R . P C 3
H40F H 0.377231 0.438242 0.711107 0.080 Uiso 0.157(2) 1 calc R . P C 3
C404 C 0.3490(4) 0.3775(8) 0.6195(5) 0.081(5) Uani 0.157(2) 1 d D U P C 3
H40G H 0.312300 0.416034 0.610795 0.098 Uiso 0.157(2) 1 calc R . P C 3
H40H H 0.328078 0.326016 0.615337 0.098 Uiso 0.157(2) 1 calc R . P C 3
C405 C 0.4773(6) 0.3167(6) 0.6546(6) 0.077(5) Uani 0.157(2) 1 d D U P C 3
H40I H 0.456876 0.272674 0.675351 0.093 Uiso 0.157(2) 1 calc R . P C 3
H40J H 0.526763 0.307702 0.660044 0.093 Uiso 0.157(2) 1 calc R . P C 3
C406 C 0.4492(6) 0.3200(6) 0.5794(6) 0.069(5) Uani 0.157(2) 1 d D U P C 3
H40K H 0.426867 0.270846 0.564489 0.083 Uiso 0.157(2) 1 calc R . P C 3
H40L H 0.486365 0.328358 0.552483 0.083 Uiso 0.157(2) 1 calc R . P C 3
C407 C 0.3588(7) 0.3876(9) 0.4939(5) 0.068(2) Uani 0.157(2) 1 d D U P C 3
H40M H 0.321813 0.424854 0.490746 0.102 Uiso 0.1569 1 calc . . P C 3
H40N H 0.340052 0.336625 0.481854 0.102 Uiso 0.1569 1 calc . . P C 3
H40O H 0.389353 0.401992 0.461684 0.102 Uiso 0.1569 1 calc . . P C 3


_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
Ti01 O101 1.6453(19) . ?
Ti01 N101 2.060(2) . ?
Ti01 N102 2.046(2) . ?
Ti01 N103 2.056(2) . ?
Ti01 N104 2.051(2) . ?
N101 C101 1.380(3) . ?
N101 C104 1.381(3) . ?
N102 C105 1.389(3) . ?
N102 C108 1.388(3) . ?
N103 C109 1.379(3) . ?
N103 C112 1.380(3) . ?
N104 C113 1.378(3) . ?
N104 C116 1.382(3) . ?
N105 C104 1.347(3) . ?
N105 C105 1.305(3) . ?
N106 C108 1.315(3) . ?
N106 C109 1.349(3) . ?
N107 C112 1.349(3) . ?
N107 C113 1.315(3) . ?
N108 C101 1.356(3) . ?
N108 C116 1.312(3) . ?
C101 C102 1.438(4) . ?
C102 C103 1.409(4) . ?
C102 C117 1.393(4) . ?
C103 C104 1.420(4) . ?
C103 C120 1.403(4) . ?
C105 C106 1.465(4) . ?
C106 C107 1.397(4) . ?
C106 C121 1.380(4) . ?
C107 C108 1.452(4) . ?
C107 C124 1.388(4) . ?
C109 C110 1.435(4) . ?
C110 C111 1.403(4) . ?
C110 C125 1.396(4) . ?
C111 C112 1.425(4) . ?
C111 C128 1.397(4) . ?
C113 C114 1.447(4) . ?
C114 C115 1.394(4) . ?
C114 C129 1.382(4) . ?
C115 C116 1.470(3) . ?
C115 C132 1.384(4) . ?
C117 H117 0.9300 . ?
C117 C118 1.370(4) . ?
C118 H118 0.9300 . ?
C118 C119 1.411(4) . ?
C119 H119 0.9300 . ?
C119 C120 1.362(4) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.378(4) . ?
C122 H122 0.9300 . ?
C122 C123 1.394(4) . ?
C123 H123 0.9300 . ?
C123 C124 1.382(4) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.380(4) . ?
C126 H126 0.9300 . ?
C126 C127 1.387(4) . ?
C127 H127 0.9300 . ?
C127 C128 1.375(4) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.383(4) . ?
C130 H130 0.9300 . ?
C130 C131 1.379(4) . ?
C131 H131 0.9300 . ?
C131 C132 1.382(4) . ?
C132 H132 0.9300 . ?
N201 C201 1.451(7) . ?
N201 C203 1.507(7) . ?
N201 C205 1.403(6) . ?
N202 C202 1.496(5) . ?
N202 C204 1.518(7) . ?
N202 C206 1.527(6) . ?
N202 C207 1.447(8) . ?
C201 H20A 0.9700 . ?
C201 H20B 0.9700 . ?
C201 C202 1.553(9) . ?
C202 H20C 0.9700 . ?
C202 H20D 0.9700 . ?
C203 H20E 0.9700 . ?
C203 H20F 0.9700 . ?
C203 C204 1.500(8) . ?
C204 H20G 0.9700 . ?
C204 H20H 0.9700 . ?
C205 H20I 0.9700 . ?
C205 H20J 0.9700 . ?
C205 C206 1.457(10) . ?
C206 H20K 0.9700 . ?
C206 H20L 0.9700 . ?
C207 H20M 0.9600 . ?
C207 H20N 0.9600 . ?
C207 H20O 0.9600 . ?
N301 C301 1.450(7) . ?
N301 C303 1.506(7) . ?
N301 C305 1.403(6) . ?
N302 C302 1.495(5) . ?
N302 C304 1.518(7) . ?
N302 C306 1.526(6) . ?
N302 C307 1.448(8) . ?
C301 H30A 0.9700 . ?
C301 H30B 0.9700 . ?
C301 C302 1.552(9) . ?
C302 H30C 0.9700 . ?
C302 H30D 0.9700 . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C304 1.499(8) . ?
C304 H30G 0.9700 . ?
C304 H30H 0.9700 . ?
C305 H30I 0.9700 . ?
C305 H30J 0.9700 . ?
C305 C306 1.456(10) . ?
C306 H30K 0.9700 . ?
C306 H30L 0.9700 . ?
C307 H30M 0.9600 . ?
C307 H30N 0.9600 . ?
C307 H30O 0.9600 . ?
N401 C401 1.450(7) . ?
N401 C403 1.505(7) . ?
N401 C405 1.403(6) . ?
N402 C402 1.495(6) . ?
N402 C404 1.517(7) . ?
N402 C406 1.527(6) . ?
N402 C407 1.448(8) . ?
C401 H40A 0.9700 . ?
C401 H40B 0.9700 . ?
C401 C402 1.552(9) . ?
C402 H40C 0.9700 . ?
C402 H40D 0.9700 . ?
C403 H40E 0.9700 . ?
C403 H40F 0.9700 . ?
C403 C404 1.498(8) . ?
C404 H40G 0.9700 . ?
C404 H40H 0.9700 . ?
C405 H40I 0.9700 . ?
C405 H40J 0.9700 . ?
C405 C406 1.457(10) . ?
C406 H40K 0.9700 . ?
C406 H40L 0.9700 . ?
C407 H40M 0.9600 . ?
C407 H40N 0.9600 . ?
C407 H40O 0.9600 . ?

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
O101 Ti01 N101 108.47(9) . . ?
O101 Ti01 N102 105.64(9) . . ?
O101 Ti01 N103 105.16(10) . . ?
O101 Ti01 N104 107.58(9) . . ?
N102 Ti01 N101 85.78(9) . . ?
N102 Ti01 N103 84.72(9) . . ?
N102 Ti01 N104 146.77(9) . . ?
N103 Ti01 N101 146.37(9) . . ?
N104 Ti01 N101 84.61(8) . . ?
N104 Ti01 N103 85.91(9) . . ?
C101 N101 Ti01 125.18(17) . . ?
C101 N101 C104 108.0(2) . . ?
C104 N101 Ti01 124.54(17) . . ?
C105 N102 Ti01 124.35(18) . . ?
C108 N102 Ti01 125.03(17) . . ?
C108 N102 C105 108.7(2) . . ?
C109 N103 Ti01 124.57(18) . . ?
C109 N103 C112 107.9(2) . . ?
C112 N103 Ti01 123.83(18) . . ?
C113 N104 Ti01 122.79(18) . . ?
C113 N104 C116 108.7(2) . . ?
C116 N104 Ti01 124.52(16) . . ?
C105 N105 C104 123.6(2) . . ?
C108 N106 C109 122.5(3) . . ?
C113 N107 C112 123.3(2) . . ?
C116 N108 C101 122.8(2) . . ?
N101 C101 C102 109.1(2) . . ?
N108 C101 N101 126.8(2) . . ?
N108 C101 C102 124.1(3) . . ?
C103 C102 C101 106.3(2) . . ?
C117 C102 C101 133.2(2) . . ?
C117 C102 C103 120.6(2) . . ?
C102 C103 C104 107.3(2) . . ?
C120 C103 C102 120.0(3) . . ?
C120 C103 C104 132.7(3) . . ?
N101 C104 C103 109.4(2) . . ?
N105 C104 N101 127.0(3) . . ?
N105 C104 C103 123.7(2) . . ?
N102 C105 C106 108.0(2) . . ?
N105 C105 N102 128.5(2) . . ?
N105 C105 C106 123.5(3) . . ?
C107 C106 C105 107.4(2) . . ?
C121 C106 C105 131.2(3) . . ?
C121 C106 C107 121.4(3) . . ?
C106 C107 C108 106.9(2) . . ?
C124 C107 C106 120.7(3) . . ?
C124 C107 C108 132.4(3) . . ?
N102 C108 C107 109.0(2) . . ?
N106 C108 N102 128.1(2) . . ?
N106 C108 C107 122.9(3) . . ?
N103 C109 C110 109.2(2) . . ?
N106 C109 N103 127.1(3) . . ?
N106 C109 C110 123.7(3) . . ?
C111 C110 C109 106.4(3) . . ?
C125 C110 C109 132.3(3) . . ?
C125 C110 C111 121.1(3) . . ?
C110 C111 C112 107.2(2) . . ?
C128 C111 C110 120.5(3) . . ?
C128 C111 C112 132.2(3) . . ?
N103 C112 C111 109.2(2) . . ?
N107 C112 N103 126.8(3) . . ?
N107 C112 C111 123.7(3) . . ?
N104 C113 C114 108.8(2) . . ?
N107 C113 N104 128.8(3) . . ?
N107 C113 C114 122.3(2) . . ?
C115 C114 C113 107.7(2) . . ?
C129 C114 C113 130.5(3) . . ?
C129 C114 C115 121.8(3) . . ?
C114 C115 C116 106.2(2) . . ?
C132 C115 C114 119.9(2) . . ?
C132 C115 C116 134.0(3) . . ?
N104 C116 C115 108.6(2) . . ?
N108 C116 N104 128.0(2) . . ?
N108 C116 C115 123.4(3) . . ?
C102 C117 H117 120.7 . . ?
C118 C117 C102 118.6(3) . . ?
C118 C117 H117 120.7 . . ?
C117 C118 H118 119.5 . . ?
C117 C118 C119 120.9(3) . . ?
C119 C118 H118 119.5 . . ?
C118 C119 H119 119.4 . . ?
C120 C119 C118 121.1(3) . . ?
C120 C119 H119 119.4 . . ?
C103 C120 H120 120.6 . . ?
C119 C120 C103 118.7(3) . . ?
C119 C120 H120 120.6 . . ?
C106 C121 H121 121.2 . . ?
C122 C121 C106 117.7(3) . . ?
C122 C121 H121 121.2 . . ?
C121 C122 H122 119.3 . . ?
C121 C122 C123 121.3(3) . . ?
C123 C122 H122 119.3 . . ?
C122 C123 H123 119.4 . . ?
C124 C123 C122 121.1(3) . . ?
C124 C123 H123 119.4 . . ?
C107 C124 H124 121.1 . . ?
C123 C124 C107 117.7(3) . . ?
C123 C124 H124 121.1 . . ?
C110 C125 H125 121.4 . . ?
C126 C125 C110 117.2(3) . . ?
C126 C125 H125 121.4 . . ?
C125 C126 H126 119.1 . . ?
C125 C126 C127 121.8(3) . . ?
C127 C126 H126 119.1 . . ?
C126 C127 H127 119.2 . . ?
C128 C127 C126 121.6(3) . . ?
C128 C127 H127 119.2 . . ?
C111 C128 H128 121.1 . . ?
C127 C128 C111 117.8(3) . . ?
C127 C128 H128 121.1 . . ?
C114 C129 H129 121.1 . . ?
C114 C129 C130 117.8(3) . . ?
C130 C129 H129 121.1 . . ?
C129 C130 H130 119.8 . . ?
C131 C130 C129 120.5(3) . . ?
C131 C130 H130 119.8 . . ?
C130 C131 H131 119.0 . . ?
C130 C131 C132 121.9(3) . . ?
C132 C131 H131 119.0 . . ?
C115 C132 H132 121.0 . . ?
C131 C132 C115 118.0(3) . . ?
C131 C132 H132 121.0 . . ?
C201 N201 C203 106.4(4) . . ?
C205 N201 C201 109.7(4) . . ?
C205 N201 C203 106.5(4) . . ?
C202 N202 C204 106.9(4) . . ?
C202 N202 C206 108.4(4) . . ?
C204 N202 C206 106.0(4) . . ?
C207 N202 C202 109.7(5) . . ?
C207 N202 C204 111.7(4) . . ?
C207 N202 C206 113.9(5) . . ?
N201 C201 H20A 109.1 . . ?
N201 C201 H20B 109.1 . . ?
N201 C201 C202 112.6(4) . . ?
H20A C201 H20B 107.8 . . ?
C202 C201 H20A 109.1 . . ?
C202 C201 H20B 109.1 . . ?
N202 C202 C201 106.9(5) . . ?
N202 C202 H20C 110.3 . . ?
N202 C202 H20D 110.3 . . ?
C201 C202 H20C 110.3 . . ?
C201 C202 H20D 110.3 . . ?
H20C C202 H20D 108.6 . . ?
N201 C203 H20E 109.6 . . ?
N201 C203 H20F 109.6 . . ?
H20E C203 H20F 108.1 . . ?
C204 C203 N201 110.5(5) . . ?
C204 C203 H20E 109.6 . . ?
C204 C203 H20F 109.6 . . ?
N202 C204 H20G 109.7 . . ?
N202 C204 H20H 109.7 . . ?
C203 C204 N202 109.8(4) . . ?
C203 C204 H20G 109.7 . . ?
C203 C204 H20H 109.7 . . ?
H20G C204 H20H 108.2 . . ?
N201 C205 H20I 108.8 . . ?
N201 C205 H20J 108.8 . . ?
N201 C205 C206 113.9(4) . . ?
H20I C205 H20J 107.7 . . ?
C206 C205 H20I 108.8 . . ?
C206 C205 H20J 108.8 . . ?
N202 C206 H20K 109.7 . . ?
N202 C206 H20L 109.7 . . ?
C205 C206 N202 109.8(5) . . ?
C205 C206 H20K 109.7 . . ?
C205 C206 H20L 109.7 . . ?
H20K C206 H20L 108.2 . . ?
N202 C207 H20M 109.5 . . ?
N202 C207 H20N 109.5 . . ?
N202 C207 H20O 109.5 . . ?
H20M C207 H20N 109.5 . . ?
H20M C207 H20O 109.5 . . ?
H20N C207 H20O 109.5 . . ?
C301 N301 C303 106.5(4) . . ?
C305 N301 C301 109.7(4) . . ?
C305 N301 C303 106.6(4) . . ?
C302 N302 C304 107.0(4) . . ?
C302 N302 C306 108.5(4) . . ?
C304 N302 C306 106.0(4) . . ?
C307 N302 C302 109.6(5) . . ?
C307 N302 C304 111.7(4) . . ?
C307 N302 C306 113.8(5) . . ?
N301 C301 H30A 109.1 . . ?
N301 C301 H30B 109.1 . . ?
N301 C301 C302 112.6(4) . . ?
H30A C301 H30B 107.8 . . ?
C302 C301 H30A 109.1 . . ?
C302 C301 H30B 109.1 . . ?
N302 C302 C301 107.0(5) . . ?
N302 C302 H30C 110.3 . . ?
N302 C302 H30D 110.3 . . ?
C301 C302 H30C 110.3 . . ?
C301 C302 H30D 110.3 . . ?
H30C C302 H30D 108.6 . . ?
N301 C303 H30E 109.5 . . ?
N301 C303 H30F 109.5 . . ?
H30E C303 H30F 108.1 . . ?
C304 C303 N301 110.6(5) . . ?
C304 C303 H30E 109.5 . . ?
C304 C303 H30F 109.5 . . ?
N302 C304 H30G 109.7 . . ?
N302 C304 H30H 109.7 . . ?
C303 C304 N302 109.9(4) . . ?
C303 C304 H30G 109.7 . . ?
C303 C304 H30H 109.7 . . ?
H30G C304 H30H 108.2 . . ?
N301 C305 H30I 108.7 . . ?
N301 C305 H30J 108.7 . . ?
N301 C305 C306 114.0(4) . . ?
H30I C305 H30J 107.6 . . ?
C306 C305 H30I 108.7 . . ?
C306 C305 H30J 108.7 . . ?
N302 C306 H30K 109.7 . . ?
N302 C306 H30L 109.7 . . ?
C305 C306 N302 109.9(5) . . ?
C305 C306 H30K 109.7 . . ?
C305 C306 H30L 109.7 . . ?
H30K C306 H30L 108.2 . . ?
N302 C307 H30M 109.5 . . ?
N302 C307 H30N 109.5 . . ?
N302 C307 H30O 109.5 . . ?
H30M C307 H30N 109.5 . . ?
H30M C307 H30O 109.5 . . ?
H30N C307 H30O 109.5 . . ?
C401 N401 C403 106.5(4) . . ?
C405 N401 C401 109.7(4) . . ?
C405 N401 C403 106.6(4) . . ?
C402 N402 C404 107.0(4) . . ?
C402 N402 C406 108.5(4) . . ?
C404 N402 C406 106.0(4) . . ?
C407 N402 C402 109.6(5) . . ?
C407 N402 C404 111.7(4) . . ?
C407 N402 C406 113.8(5) . . ?
N401 C401 H40A 109.1 . . ?
N401 C401 H40B 109.1 . . ?
N401 C401 C402 112.7(4) . . ?
H40A C401 H40B 107.8 . . ?
C402 C401 H40A 109.1 . . ?
C402 C401 H40B 109.1 . . ?
N402 C402 C401 107.1(5) . . ?
N402 C402 H40C 110.3 . . ?
N402 C402 H40D 110.3 . . ?
C401 C402 H40C 110.3 . . ?
C401 C402 H40D 110.3 . . ?
H40C C402 H40D 108.6 . . ?
N401 C403 H40E 109.5 . . ?
N401 C403 H40F 109.5 . . ?
H40E C403 H40F 108.1 . . ?
C404 C403 N401 110.7(5) . . ?
C404 C403 H40E 109.5 . . ?
C404 C403 H40F 109.5 . . ?
N402 C404 H40G 109.7 . . ?
N402 C404 H40H 109.7 . . ?
C403 C404 N402 110.0(4) . . ?
C403 C404 H40G 109.7 . . ?
C403 C404 H40H 109.7 . . ?
H40G C404 H40H 108.2 . . ?
N401 C405 H40I 108.8 . . ?
N401 C405 H40J 108.8 . . ?
N401 C405 C406 113.8(4) . . ?
H40I C405 H40J 107.7 . . ?
C406 C405 H40I 108.8 . . ?
C406 C405 H40J 108.8 . . ?
N402 C406 H40K 109.7 . . ?
N402 C406 H40L 109.7 . . ?
C405 C406 N402 109.7(5) . . ?
C405 C406 H40K 109.7 . . ?
C405 C406 H40L 109.7 . . ?
H40K C406 H40L 108.2 . . ?
N402 C407 H40M 109.5 . . ?
N402 C407 H40N 109.5 . . ?
N402 C407 H40O 109.5 . . ?
H40M C407 H40N 109.5 . . ?
H40M C407 H40O 109.5 . . ?
H40N C407 H40O 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.927
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_VoPcPentyl4N
_database_code_depnum_ccdc_archive 'CCDC 1581402'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-10-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of vanadyl phthalocyanine with tetrapentylammonium cation'
_chemical_formula_moiety         
'0.5(C19.52 H43.19 N), 0.5(C16.77 H38.32 N), C32 H16 N8 O V, 0.23(C5 H9), 0.24(C3 H5)'
_chemical_formula_sum            'C52 H60 N9 O V'
_chemical_formula_weight         878.03
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   11.8287(4)
_cell_length_b                   13.0419(4)
_cell_length_c                   16.6492(5)
_cell_angle_alpha                67.700(3)
_cell_angle_beta                 71.527(3)
_cell_angle_gamma                78.147(2)
_cell_volume                     2243.27(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17872
_cell_measurement_temperature    116.7(6)
_cell_measurement_theta_max      32.5610
_cell_measurement_theta_min      1.7570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             932
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0984
-3 -5 0 0.0677
5 -1 -3 0.0361
-5 0 2 0.0378
2 2 5 0.1775
-2 -2 -5 0.1881
5 1 3 0.1078

_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.097
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0001 0.9979 -0.0003 0.0030 -0.0589 0.0007
-2.9944 -4.9912 -0.0049 0.1672 0.2847 -0.0559
4.9908 -0.9934 -2.9818 -0.3808 0.0212 -0.0232
-4.9905 -0.0040 1.9845 0.3532 0.0197 -0.0142
1.9942 1.9948 4.9911 0.0073 -0.0219 0.2198
-1.9942 -1.9948 -4.9911 -0.0073 0.0219 -0.2198
4.9887 0.9997 3.0026 -0.2273 0.0108 0.1983
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44912
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.783
_diffrn_ambient_temperature      116.7(6)
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  62.00   1.00   60.00    --   20.14 -99.00 -30.00   84
  2  ω     -9.00  94.00   1.00   60.00    --   20.14  57.00 -30.00  103
  3  ω    -14.00  97.00   1.00   60.00    --   20.14  77.00  90.00  111
  4  ω    -56.00  45.00   1.00   60.00    --   20.14 -37.00-180.00  101
  5  ω    -56.00  39.00   1.00   60.00    --   20.14 -37.00  30.00   95
  6  ω      7.00  93.00   1.00   60.00    --   20.14  57.00-150.00   86
  7  ω     35.00  81.00   1.00   60.00    --   20.14 178.00-150.00   46
  8  ω    -94.00 -57.00   1.00   60.00    --  -20.45 150.00  19.99   37
  9  ω    -80.00 -49.00   1.00   60.00    --  -20.45 128.00 177.85   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22238
_reflns_number_total             26754
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.074(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         26754
_refine_ls_number_restraints     699
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.016
_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)+(0.0492P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1019
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.926(15)
 0.074(15)
2. 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
3. Shared sites
{C316, C325}
{C313, C328}
{C203, C223}
4. Uiso/Uaniso restraints and constraints
C313 \\sim C314 \\sim C315 \\sim C325 \\sim C327: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq, Uanis(C303) \\sim Ueq,
Uanis(C304) \\sim Ueq, Uanis(C305) \\sim Ueq, Uanis(C306) \\sim Ueq,
Uanis(C307) \\sim Ueq, Uanis(C308) \\sim Ueq, Uanis(C309) \\sim Ueq,
Uanis(C310) \\sim Ueq, Uanis(C311) \\sim Ueq, Uanis(C312) \\sim Ueq,
Uanis(C313) \\sim Ueq, Uanis(C314) \\sim Ueq, Uanis(C315) \\sim Ueq,
Uanis(C316) \\sim Ueq, Uanis(C317) \\sim Ueq, Uanis(C318) \\sim Ueq,
Uanis(C319) \\sim Ueq, Uanis(C320) \\sim Ueq, Uanis(C322) \\sim Ueq,
Uanis(C323) \\sim Ueq, Uanis(C324) \\sim Ueq, Uanis(C325) \\sim Ueq,
Uanis(C327) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq,
Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq, Uanis(C205) \\sim Ueq,
Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq, Uanis(C208) \\sim Ueq,
Uanis(C209) \\sim Ueq, Uanis(C210) \\sim Ueq, Uanis(C211) \\sim Ueq,
Uanis(C212) \\sim Ueq, Uanis(C213) \\sim Ueq, Uanis(C214) \\sim Ueq,
Uanis(C215) \\sim Ueq, Uanis(C216) \\sim Ueq, Uanis(C217) \\sim Ueq,
Uanis(C218) \\sim Ueq, Uanis(C219) \\sim Ueq, Uanis(C220) \\sim Ueq,
Uanis(C501) \\sim Ueq, Uanis(C502) \\sim Ueq, Uanis(C503) \\sim Ueq,
Uanis(C504) \\sim Ueq, Uanis(C505) \\sim Ueq, Uanis(C506) \\sim Ueq,
Uanis(C507) \\sim Ueq, Uanis(C508) \\sim Ueq, Uanis(C509) \\sim Ueq,
Uanis(C510) \\sim Ueq, Uanis(C511) \\sim Ueq, Uanis(C512) \\sim Ueq,
Uanis(C513) \\sim Ueq, Uanis(C514) \\sim Ueq, Uanis(C515) \\sim Ueq,
Uanis(C516) \\sim Ueq, Uanis(C517) \\sim Ueq, Uanis(C518) \\sim Ueq,
Uanis(C519) \\sim Ueq, Uanis(C520) \\sim Ueq, Uanis(C521) \\sim Ueq,
Uanis(C522) \\sim Ueq, Uanis(C523) \\sim Ueq, Uanis(C524) \\sim Ueq,
Uanis(C525) \\sim Ueq, Uanis(C526) \\sim Ueq, Uanis(C527) \\sim Ueq,
Uanis(C528) \\sim Ueq, Uanis(C529) \\sim Ueq, Uanis(C530) \\sim Ueq,
Uanis(C531) \\sim Ueq, Uanis(C532) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C111) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113) \\sim Ueq,
Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq,
Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq,
Uanis(C120) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq,
Uanis(C126) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C128) \\sim Ueq,
Uanis(C129) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C131) \\sim Ueq,
Uanis(C132) \\sim Ueq, Uanis(C222) \\sim Ueq, Uanis(C321) \\sim Ueq,
Uanis(C221) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C204) = Uanis(C221)
Uanis(C222) = Uanis(C205)
Uanis(C317) = Uanis(C321)
Uanis(C314) = Uanis(C325)
Uanis(C316) = Uanis(C325)
Uanis(C313) = Uanis(C328)
Uanis(C326) = Uanis(C315)
Uanis(C314) = Uanis(C327)
Uanis(C203) = Uanis(C223)
5. Others
 Fixed Sof: C203(0.83876) C204(0.83876) H20G(0.83876) H20H(0.83876)
 C205(0.83876) H20I(0.83876) H20J(0.83876) H20K(0.83876) C313(0.68078)
 C314(0.68078) H31J(0.68078) H31K(0.68078) C315(0.68078) H31L(0.68078)
 H31M(0.68078) H31N(0.68078) C316(0.54568) C317(0.54568) H31Q(0.54568)
 H31R(0.54568) C318(0.54568) H31S(0.54568) H31T(0.54568) C319(0.54568)
 H31U(0.54568) H31V(0.54568) C320(0.54568) H32A(0.54568) H32B(0.54568)
 H32C(0.54568) C321(0.45432) H32D(0.45432) H32E(0.45432) C322(0.45432)
 H32F(0.45432) H32G(0.45432) C323(0.45432) H32H(0.45432) H32I(0.45432)
 C324(0.45432) H32J(0.45432) H32K(0.45432) H32L(0.45432) C325(0.45432)
 C326(0.31922) H32M(0.31922) H32N(0.31922) H32O(0.31922) C327(0.31922)
 H32P(0.31922) H32Q(0.31922) C328(0.31922) C221(0.16124) H22D(0.16124)
 H22E(0.16124) C222(0.16124) H22F(0.16124) H22G(0.16124) H22H(0.16124)
 C223(0.16124)
6.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C206(H20L,
 H20M), C207(H20N,H20O), C208(H20P,H20Q), C209(H20R,H20S), C211(H21D,H21E),
 C212(H21F,H21G), C213(H21H,H21I), C214(H21J,H21K), C216(H21O,H21P), C217(H21Q,
 H21R), C218(H21S,H21T), C219(H21U,H21V), C301(H30A,H30B), C302(H30C,H30D),
 C303(H30E,H30F), C304(H30G,H30H), C306(H30L,H30M), C307(H30N,H30O), C308(H30P,
 H30Q), C309(H30R,H30S), C311(H31D,H31E), C312(H31F,H31G), C313(H31H,H31I),
 C314(H31J,H31K), C316(H31O,H31P), C317(H31Q,H31R), C318(H31S,H31T), C319(H31U,
 H31V), C321(H32D,H32E), C322(H32F,H32G), C323(H32H,H32I), C327(H32P,H32Q),
 C221(H22D,H22E)
6.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C517(H517), C518(H518),
 C519(H519), C520(H520), C521(H521), C522(H522), C523(H523), C524(H524),
 C525(H525), C526(H526), C527(H527), C528(H528), C529(H529), C530(H530),
 C531(H531), C532(H532)
6.c Idealised Me refined as rotating group:
 C205(H20I,H20J,H20K), C210(H21A,H21B,H21C), C215(H21L,H21M,H21N), C220(H22A,
 H22B,H22C), C305(H30I,H30J,H30K), C310(H31A,H31B,H31C), C315(H31L,H31M,H31N),
 C320(H32A,H32B,H32C), C324(H32J,H32K,H32L), C326(H32M,H32N,H32O), C222(H22F,
 H22G,H22H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
N201 N 0.7870(2) 0.7016(2) 0.11063(16) 0.0182(5) Uani 1 1 d . . . A 1
C201 C 0.8042(3) 0.6111(3) 0.1988(2) 0.0222(7) Uani 1 1 d . U . A 1
H20A H 0.850709 0.546562 0.184884 0.027 Uiso 1 1 calc R . . A 1
H20B H 0.850650 0.638680 0.223656 0.027 Uiso 1 1 calc R . . A 1
C202 C 0.6891(3) 0.5741(3) 0.2703(2) 0.0275(7) Uani 1 1 d . U . A 1
H20C H 0.639932 0.549757 0.245355 0.033 Uiso 1 1 calc R . . A 1
H20D H 0.644651 0.636623 0.288293 0.033 Uiso 1 1 calc R . . A 1
C203 C 0.7155(3) 0.4782(3) 0.3535(2) 0.0332(7) Uani 0.8388 1 d . U P A 1
H20E H 0.642863 0.441631 0.387586 0.040 Uiso 1 1 calc R . . A 1
H20F H 0.775125 0.424155 0.332662 0.040 Uiso 1 1 calc R . . A 1
C204 C 0.7582(6) 0.5081(4) 0.4155(5) 0.0385(13) Uani 0.8388 1 d . U P A 1
H20G H 0.696863 0.557843 0.440498 0.046 Uiso 0.8388 1 calc R . P A 1
H20H H 0.829012 0.547508 0.381932 0.046 Uiso 0.8388 1 calc R . P A 1
C205 C 0.7886(5) 0.4039(6) 0.4937(4) 0.065(2) Uani 0.8388 1 d . U P A 1
H20I H 0.848902 0.354173 0.469184 0.097 Uiso 0.8388 1 calc GR . P A 1
H20J H 0.717802 0.366510 0.528718 0.097 Uiso 0.8388 1 calc GR . P A 1
H20K H 0.817831 0.426747 0.531254 0.097 Uiso 0.8388 1 calc GR . P A 1
C206 C 0.9108(2) 0.7240(2) 0.04684(18) 0.0186(5) Uani 1 1 d . U . A 1
H20L H 0.946831 0.657312 0.032161 0.022 Uiso 1 1 calc R . . A 1
H20M H 0.959646 0.736822 0.078582 0.022 Uiso 1 1 calc R . . A 1
C207 C 0.9164(3) 0.8221(2) -0.04127(19) 0.0228(6) Uani 1 1 d . U . A 1
H20N H 0.910742 0.891285 -0.030566 0.027 Uiso 1 1 calc R . . A 1
H20O H 0.849694 0.824854 -0.064297 0.027 Uiso 1 1 calc R . . A 1
C208 C 1.0354(3) 0.8081(3) -0.1107(2) 0.0278(8) Uani 1 1 d . U . A 1
H20P H 1.049617 0.879347 -0.158298 0.033 Uiso 1 1 calc R . . A 1
H20Q H 1.099935 0.787408 -0.081562 0.033 Uiso 1 1 calc R . . A 1
C209 C 1.0399(3) 0.7217(3) -0.1527(3) 0.0307(9) Uani 1 1 d . U . A 1
H20R H 1.025600 0.650462 -0.105032 0.037 Uiso 1 1 calc R . . A 1
H20S H 1.119836 0.714012 -0.191140 0.037 Uiso 1 1 calc R . . A 1
C210 C 0.9496(4) 0.7485(3) -0.2081(3) 0.0386(9) Uani 1 1 d . U . A 1
H21A H 0.954978 0.823259 -0.249949 0.058 Uiso 1 1 calc GR . . A 1
H21B H 0.870135 0.741568 -0.168688 0.058 Uiso 1 1 calc GR . . A 1
H21C H 0.967052 0.697511 -0.240545 0.058 Uiso 1 1 calc GR . . A 1
C211 C 0.7201(3) 0.8071(3) 0.1274(2) 0.0219(6) Uani 1 1 d . U . A 1
H21D H 0.640380 0.790746 0.165892 0.026 Uiso 1 1 calc R . . A 1
H21E H 0.711290 0.862127 0.070442 0.026 Uiso 1 1 calc R . . A 1
C212 C 0.7797(3) 0.8578(3) 0.1709(2) 0.0243(6) Uani 1 1 d . U . A 1
H21F H 0.862458 0.867260 0.136671 0.029 Uiso 1 1 calc R . . A 1
H21G H 0.778869 0.808046 0.231569 0.029 Uiso 1 1 calc R . . A 1
C213 C 0.7127(3) 0.9716(3) 0.1737(2) 0.0254(7) Uani 1 1 d . U . A 1
H21H H 0.627404 0.963864 0.195544 0.030 Uiso 1 1 calc R . . A 1
H21I H 0.735211 0.991207 0.216785 0.030 Uiso 1 1 calc R . . A 1
C214 C 0.7353(3) 1.0671(3) 0.0843(2) 0.0254(7) Uani 1 1 d . U . A 1
H21J H 0.681199 1.131699 0.091505 0.030 Uiso 1 1 calc R . . A 1
H21K H 0.716709 1.046346 0.040082 0.030 Uiso 1 1 calc R . . A 1
C215 C 0.8633(3) 1.0993(3) 0.0482(3) 0.0359(8) Uani 1 1 d . U . A 1
H21L H 0.886068 1.111210 0.094160 0.054 Uiso 1 1 calc GR . . A 1
H21M H 0.868063 1.166413 -0.003121 0.054 Uiso 1 1 calc GR . . A 1
H21N H 0.916290 1.040465 0.030763 0.054 Uiso 1 1 calc GR . . A 1
C216 C 0.7141(2) 0.6615(2) 0.06924(19) 0.0193(5) Uani 1 1 d . U . A 1
H21O H 0.633080 0.655387 0.107907 0.023 Uiso 1 1 calc R . . A 1
H21P H 0.709914 0.717635 0.011625 0.023 Uiso 1 1 calc R . . A 1
C217 C 0.7623(3) 0.5505(3) 0.0548(2) 0.0253(6) Uani 1 1 d . U . A 1
H21Q H 0.750384 0.490924 0.112624 0.030 Uiso 1 1 calc R . . A 1
H21R H 0.847609 0.550330 0.026217 0.030 Uiso 1 1 calc R . . A 1
C218 C 0.6992(3) 0.5296(3) -0.0039(2) 0.0264(7) Uani 1 1 d . U . A 1
H21S H 0.614500 0.526463 0.026422 0.032 Uiso 1 1 calc R . . A 1
H21T H 0.707195 0.591819 -0.060087 0.032 Uiso 1 1 calc R . . A 1
C219 C 0.7485(3) 0.4223(3) -0.0249(2) 0.0310(7) Uani 1 1 d . U . A 1
H21U H 0.740332 0.360123 0.031321 0.037 Uiso 1 1 calc R . . A 1
H21V H 0.700539 0.411660 -0.058287 0.037 Uiso 1 1 calc R . . A 1
C220 C 0.8793(4) 0.4208(3) -0.0789(3) 0.0474(10) Uani 1 1 d . U . A 1
H22A H 0.890358 0.487272 -0.130777 0.071 Uiso 1 1 calc GR . . A 1
H22B H 0.900853 0.356856 -0.097824 0.071 Uiso 1 1 calc GR . . A 1
H22C H 0.929058 0.417392 -0.042054 0.071 Uiso 1 1 calc GR . . A 1
N301 N 0.7529(2) -0.04752(19) 0.53166(15) 0.0185(5) Uani 1 1 d . . . B 1
C301 C 0.7250(3) 0.0179(3) 0.59529(19) 0.0207(6) Uani 1 1 d . U . B 1
H30A H 0.669560 -0.021183 0.650832 0.025 Uiso 1 1 calc R . . B 1
H30B H 0.684088 0.089649 0.568730 0.025 Uiso 1 1 calc R . . B 1
C302 C 0.8307(3) 0.0382(3) 0.6188(2) 0.0252(7) Uani 1 1 d . U . B 1
H30C H 0.875846 0.094505 0.568138 0.030 Uiso 1 1 calc R . . B 1
H30D H 0.883582 -0.029863 0.632806 0.030 Uiso 1 1 calc R . . B 1
C303 C 0.7829(3) 0.0773(3) 0.70024(19) 0.0245(6) Uani 1 1 d . U . B 1
H30E H 0.726858 0.142896 0.686051 0.029 Uiso 1 1 calc R . . B 1
H30F H 0.739088 0.019511 0.750282 0.029 Uiso 1 1 calc R . . B 1
C304 C 0.8785(3) 0.1047(4) 0.7297(2) 0.0435(9) Uani 1 1 d . U . B 1
H30G H 0.916237 0.168475 0.682573 0.052 Uiso 1 1 calc R . . B 1
H30H H 0.939583 0.042186 0.737685 0.052 Uiso 1 1 calc R . . B 1
C305 C 0.8286(4) 0.1305(4) 0.8170(2) 0.0427(10) Uani 1 1 d . U . B 1
H30I H 0.770549 0.194304 0.808697 0.064 Uiso 1 1 calc GR . . B 1
H30J H 0.892632 0.145792 0.833364 0.064 Uiso 1 1 calc GR . . B 1
H30K H 0.791262 0.067644 0.863888 0.064 Uiso 1 1 calc GR . . B 1
C306 C 0.6360(2) -0.0411(2) 0.50841(19) 0.0198(5) Uani 1 1 d . U . B 1
H30L H 0.571879 -0.055284 0.563629 0.024 Uiso 1 1 calc R . . B 1
H30M H 0.619063 0.034428 0.470009 0.024 Uiso 1 1 calc R . . B 1
C307 C 0.6326(3) -0.1205(3) 0.4617(2) 0.0232(7) Uani 1 1 d . U . B 1
H30N H 0.630970 -0.196214 0.503762 0.028 Uiso 1 1 calc R . . B 1
H30O H 0.703783 -0.117275 0.412016 0.028 Uiso 1 1 calc R . . B 1
C308 C 0.5200(3) -0.0867(3) 0.4264(2) 0.0237(7) Uani 1 1 d . U . B 1
H30P H 0.528789 -0.016144 0.377209 0.028 Uiso 1 1 calc R . . B 1
H30Q H 0.450942 -0.076355 0.474042 0.028 Uiso 1 1 calc R . . B 1
C309 C 0.4980(3) -0.1747(3) 0.3932(2) 0.0245(7) Uani 1 1 d . U . B 1
H30R H 0.439437 -0.142243 0.358421 0.029 Uiso 1 1 calc R . . B 1
H30S H 0.572016 -0.194849 0.353641 0.029 Uiso 1 1 calc R . . B 1
C310 C 0.4532(3) -0.2800(2) 0.47026(19) 0.0239(6) Uani 1 1 d . U . B 1
H31A H 0.509910 -0.311743 0.505711 0.036 Uiso 1 1 calc GR . . B 1
H31B H 0.444282 -0.333016 0.445936 0.036 Uiso 1 1 calc GR . . B 1
H31C H 0.377220 -0.261403 0.507461 0.036 Uiso 1 1 calc GR . . B 1
C311 C 0.8525(2) 0.0002(2) 0.44749(19) 0.0214(6) Uani 1 1 d . U . B 1
H31D H 0.870602 -0.046770 0.410812 0.026 Uiso 1 1 calc R . . B 1
H31E H 0.923769 -0.004120 0.465945 0.026 Uiso 1 1 calc R . . B 1
C312 C 0.8258(3) 0.1207(2) 0.3888(2) 0.0251(6) Uani 1 1 d . U . B 1
H31F H 0.751812 0.152922 0.420109 0.030 Uiso 1 1 calc R . . B 1
H31G H 0.889638 0.163904 0.378912 0.030 Uiso 1 1 calc R . . B 1
C313 C 0.8145(4) 0.1273(3) 0.2978(2) 0.0367(9) Uani 0.6808 1 d . U P B 1
H31H H 0.893465 0.110793 0.261661 0.044 Uiso 1 1 calc R . . B 1
H31I H 0.765435 0.070156 0.307994 0.044 Uiso 1 1 calc R . . B 1
C314 C 0.7608(5) 0.2387(5) 0.2447(4) 0.0273(5) Uani 0.6808 1 d . U P B 1
H31J H 0.767097 0.237120 0.185603 0.033 Uiso 0.6808 1 calc R . P B 1
H31K H 0.808809 0.295824 0.236113 0.033 Uiso 0.6808 1 calc R . P B 1
C315 C 0.6299(10) 0.2729(13) 0.2862(6) 0.0382(19) Uani 0.6808 1 d . U P B 1
H31L H 0.580382 0.218808 0.292901 0.057 Uiso 0.6808 1 calc GR . P B 1
H31M H 0.605048 0.344437 0.247597 0.057 Uiso 0.6808 1 calc GR . P B 1
H31N H 0.622186 0.276933 0.344108 0.057 Uiso 0.6808 1 calc GR . P B 1
C316 C 0.7987(3) -0.1686(3) 0.5753(2) 0.0273(5) Uani 0.5457 1 d . U P B 1
H31O H 0.824494 -0.203401 0.529411 0.033 Uiso 1 1 calc R . . B 1
H31P H 0.869269 -0.167867 0.592754 0.033 Uiso 1 1 calc R . . B 1
C317 C 0.7190(11) -0.2398(9) 0.6529(6) 0.0224(14) Uani 0.5457 1 d . U P B 1
H31Q H 0.638892 -0.224390 0.644634 0.027 Uiso 0.5457 1 calc R . P B 1
H31R H 0.715681 -0.224389 0.706239 0.027 Uiso 0.5457 1 calc R . P B 1
C318 C 0.7640(6) -0.3649(5) 0.6658(5) 0.0277(13) Uani 0.5457 1 d . U P B 1
H31S H 0.770410 -0.378393 0.611057 0.033 Uiso 0.5457 1 calc R . P B 1
H31T H 0.843527 -0.379516 0.675108 0.033 Uiso 0.5457 1 calc R . P B 1
C319 C 0.6843(6) -0.4448(5) 0.7433(4) 0.0323(13) Uani 0.5457 1 d . U P B 1
H31U H 0.603598 -0.427743 0.736127 0.039 Uiso 0.5457 1 calc R . P B 1
H31V H 0.681975 -0.435060 0.798790 0.039 Uiso 0.5457 1 calc R . P B 1
C320 C 0.7267(10) -0.5665(7) 0.7507(5) 0.042(2) Uani 0.5457 1 d . U P B 1
H32A H 0.726079 -0.577374 0.696921 0.063 Uiso 0.5457 1 calc GR . P B 1
H32B H 0.673984 -0.614312 0.801692 0.063 Uiso 0.5457 1 calc GR . P B 1
H32C H 0.806517 -0.583943 0.757937 0.063 Uiso 0.5457 1 calc GR . P B 1
V0AA V 0.49125(4) 0.90156(3) 0.92016(3) 0.01166(10) Uani 1 1 d . . . . .
O0AA O 0.63342(19) 0.86689(19) 0.89528(15) 0.0181(5) Uani 1 1 d . . . . .
N101 N 0.4245(2) 0.7927(2) 1.04560(16) 0.0114(5) Uani 1 1 d . . . . .
N102 N 0.4190(2) 0.8110(2) 0.87569(17) 0.0137(5) Uani 1 1 d . . . . .
N103 N 0.4586(2) 1.0338(2) 0.81178(17) 0.0136(5) Uani 1 1 d . . . . .
N104 N 0.4640(2) 1.0146(2) 0.98267(17) 0.0141(5) Uani 1 1 d . . . . .
N105 N 0.3970(2) 0.6389(2) 1.00515(17) 0.0133(5) Uani 1 1 d . . . . .
N106 N 0.4189(2) 0.9371(2) 0.72391(17) 0.0143(5) Uani 1 1 d . . . . .
N107 N 0.4841(2) 1.1871(2) 0.85392(18) 0.0160(5) Uani 1 1 d . . . . .
N108 N 0.4240(2) 0.8976(2) 1.14082(17) 0.0142(5) Uani 1 1 d . . . . .
C101 C 0.4164(3) 0.8043(3) 1.1265(2) 0.0126(6) Uani 1 1 d . U . . .
C102 C 0.3957(3) 0.6995(3) 1.1981(2) 0.0123(6) Uani 1 1 d . U . . .
C103 C 0.3923(3) 0.6220(3) 1.1584(2) 0.0125(6) Uani 1 1 d . U . . .
C104 C 0.4072(3) 0.6836(2) 1.06337(19) 0.0117(6) Uani 1 1 d . U . . .
C105 C 0.3987(3) 0.6999(3) 0.9206(2) 0.0136(6) Uani 1 1 d . U . . .
C106 C 0.3758(3) 0.6544(3) 0.8602(2) 0.0142(6) Uani 1 1 d . U . . .
C107 C 0.3847(3) 0.7411(3) 0.7767(2) 0.0139(6) Uani 1 1 d . U . . .
C108 C 0.4104(3) 0.8395(3) 0.7880(2) 0.0146(6) Uani 1 1 d . U . . .
C109 C 0.4370(3) 1.0287(3) 0.7365(2) 0.0146(6) Uani 1 1 d . U . . .
C110 C 0.4364(3) 1.1384(3) 0.6702(2) 0.0157(6) Uani 1 1 d . U . . .
C111 C 0.4577(3) 1.2109(3) 0.7076(2) 0.0157(6) Uani 1 1 d . U . . .
C112 C 0.4702(3) 1.1437(3) 0.7958(2) 0.0144(6) Uani 1 1 d . U . . .
C113 C 0.4766(3) 1.1282(3) 0.9389(2) 0.0152(6) Uani 1 1 d . U . . .
C114 C 0.4688(3) 1.1796(3) 1.0050(2) 0.0145(6) Uani 1 1 d . U . . .
C115 C 0.4429(3) 1.0966(3) 1.0895(2) 0.0158(6) Uani 1 1 d . U . . .
C116 C 0.4432(3) 0.9937(3) 1.0743(2) 0.0128(6) Uani 1 1 d . U . . .
C117 C 0.3776(3) 0.6673(3) 1.2918(2) 0.0137(6) Uani 1 1 d . U . . .
H117 H 0.377418 0.718536 1.318307 0.016 Uiso 1 1 calc R . . . .
C118 C 0.3598(3) 0.5566(3) 1.3434(2) 0.0157(6) Uani 1 1 d . U . . .
H118 H 0.348997 0.533066 1.405327 0.019 Uiso 1 1 calc R . . . .
C119 C 0.3581(3) 0.4796(3) 1.3030(2) 0.0164(7) Uani 1 1 d . U . . .
H119 H 0.346767 0.405886 1.338832 0.020 Uiso 1 1 calc R . . . .
C120 C 0.3730(3) 0.5113(3) 1.2108(2) 0.0148(6) Uani 1 1 d . U . . .
H120 H 0.370168 0.460301 1.184917 0.018 Uiso 1 1 calc R . . . .
C121 C 0.3479(3) 0.5495(3) 0.8727(2) 0.0179(7) Uani 1 1 d . U . . .
H121 H 0.338901 0.493148 0.928465 0.022 Uiso 1 1 calc R . . . .
C122 C 0.3339(3) 0.5319(3) 0.7994(2) 0.0200(7) Uani 1 1 d . U . . .
H122 H 0.316913 0.462162 0.805908 0.024 Uiso 1 1 calc R . . . .
C123 C 0.3451(3) 0.6182(3) 0.7149(2) 0.0198(7) Uani 1 1 d . U . . .
H123 H 0.335821 0.604054 0.666731 0.024 Uiso 1 1 calc R . . . .
C124 C 0.3697(3) 0.7240(3) 0.7027(2) 0.0182(7) Uani 1 1 d . U . . .
H124 H 0.376012 0.781094 0.647442 0.022 Uiso 1 1 calc R . . . .
C125 C 0.4190(3) 1.1801(3) 0.5824(2) 0.0186(7) Uani 1 1 d . U . . .
H125 H 0.405097 1.132982 0.557079 0.022 Uiso 1 1 calc R . . . .
C126 C 0.4234(3) 1.2924(3) 0.5360(2) 0.0230(7) Uani 1 1 d . U . . .
H126 H 0.412608 1.321288 0.478308 0.028 Uiso 1 1 calc R . . . .
C127 C 0.4440(3) 1.3655(3) 0.5741(2) 0.0226(7) Uani 1 1 d . U . . .
H127 H 0.446250 1.441059 0.540956 0.027 Uiso 1 1 calc R . . . .
C128 C 0.4607(3) 1.3263(3) 0.6595(2) 0.0205(7) Uani 1 1 d . U . . .
H128 H 0.473479 1.374316 0.684551 0.025 Uiso 1 1 calc R . . . .
C129 C 0.4757(3) 1.2894(3) 0.9949(2) 0.0174(7) Uani 1 1 d . U . . .
H129 H 0.494886 1.343652 0.938334 0.021 Uiso 1 1 calc R . . . .
C130 C 0.4527(3) 1.3144(3) 1.0729(2) 0.0207(7) Uani 1 1 d . U . . .
H130 H 0.456707 1.386915 1.068412 0.025 Uiso 1 1 calc R . . . .
C131 C 0.4235(3) 1.2329(3) 1.1583(2) 0.0206(7) Uani 1 1 d . U . . .
H131 H 0.407005 1.252800 1.209217 0.025 Uiso 1 1 calc R . . . .
C132 C 0.4185(3) 1.1216(3) 1.1688(2) 0.0163(6) Uani 1 1 d . U . . .
H132 H 0.400056 1.067175 1.225394 0.020 Uiso 1 1 calc R . . . .
V1AA V 0.05532(4) 0.74893(3) 0.34682(3) 0.01200(10) Uani 1 1 d . . . . .
O1AA O -0.08673(19) 0.78190(19) 0.36796(15) 0.0180(5) Uani 1 1 d . . . . .
N501 N 0.1236(2) 0.8572(2) 0.22254(17) 0.0135(5) Uani 1 1 d . . . . .
N502 N 0.0896(2) 0.6336(2) 0.28470(17) 0.0130(5) Uani 1 1 d . . . . .
N503 N 0.0832(2) 0.6191(2) 0.45717(17) 0.0144(5) Uani 1 1 d . . . . .
N504 N 0.1210(2) 0.8417(2) 0.39376(17) 0.0134(5) Uani 1 1 d . . . . .
N505 N 0.1271(2) 0.7539(2) 0.12621(17) 0.0122(5) Uani 1 1 d . . . . .
N506 N 0.0686(2) 0.4622(2) 0.41640(17) 0.0157(5) Uani 1 1 d . . . . .
N507 N 0.1141(2) 0.7140(2) 0.54843(18) 0.0166(6) Uani 1 1 d . . . . .
N508 N 0.1490(2) 1.0122(2) 0.26090(17) 0.0148(5) Uani 1 1 d . . . . .
C501 C 0.1416(3) 0.9668(3) 0.2046(2) 0.0137(6) Uani 1 1 d . U . . .
C502 C 0.1572(3) 1.0281(3) 0.1083(2) 0.0139(6) Uani 1 1 d . U . . .
C503 C 0.1547(3) 0.9523(3) 0.0684(2) 0.0137(6) Uani 1 1 d . U . . .
C504 C 0.1337(3) 0.8447(3) 0.1408(2) 0.0131(6) Uani 1 1 d . U . . .
C505 C 0.1103(3) 0.6549(3) 0.1929(2) 0.0138(6) Uani 1 1 d . U . . .
C506 C 0.1078(3) 0.5530(3) 0.1787(2) 0.0131(6) Uani 1 1 d . U . . .
C507 C 0.0819(3) 0.4702(3) 0.2646(2) 0.0152(6) Uani 1 1 d . U . . .
C508 C 0.0757(3) 0.5216(3) 0.3290(2) 0.0144(6) Uani 1 1 d . U . . .
C509 C 0.0771(3) 0.5075(3) 0.4724(2) 0.0158(6) Uani 1 1 d . U . . .
C510 C 0.0869(3) 0.4409(3) 0.5637(2) 0.0163(7) Uani 1 1 d . U . . .
C511 C 0.0990(3) 0.5142(3) 0.6031(2) 0.0173(7) Uani 1 1 d . U . . .
C512 C 0.0980(3) 0.6258(3) 0.5349(2) 0.0148(6) Uani 1 1 d . U . . .
C513 C 0.1270(3) 0.8150(3) 0.4812(2) 0.0137(6) Uani 1 1 d . U . . .
C514 C 0.1547(3) 0.9097(3) 0.4926(2) 0.0158(6) Uani 1 1 d . U . . .
C515 C 0.1680(3) 0.9959(3) 0.4085(2) 0.0146(6) Uani 1 1 d . U . . .
C516 C 0.1460(3) 0.9525(3) 0.3477(2) 0.0128(6) Uani 1 1 d . U . . .
C517 C 0.1761(3) 1.1400(3) 0.0562(2) 0.0160(6) Uani 1 1 d . U . . .
H517 H 0.178661 1.190644 0.082513 0.019 Uiso 1 1 calc R . . . .
C518 C 0.1908(3) 1.1719(3) -0.0359(2) 0.0190(7) Uani 1 1 d . U . . .
H518 H 0.202218 1.245585 -0.071840 0.023 Uiso 1 1 calc R . . . .
C519 C 0.1887(3) 1.0946(3) -0.0756(2) 0.0178(7) Uani 1 1 d . U . . .
H519 H 0.198746 1.118310 -0.137459 0.021 Uiso 1 1 calc R . . . .
C520 C 0.1718(3) 0.9835(3) -0.0245(2) 0.0165(7) Uani 1 1 d . U . . .
H520 H 0.172009 0.932244 -0.051040 0.020 Uiso 1 1 calc R . . . .
C521 C 0.1289(3) 0.5258(3) 0.1008(2) 0.0159(6) Uani 1 1 d . U . . .
H521 H 0.149621 0.579181 0.043918 0.019 Uiso 1 1 calc R . . . .
C522 C 0.1182(3) 0.4182(3) 0.1109(2) 0.0196(7) Uani 1 1 d . U . . .
H522 H 0.130659 0.399287 0.060063 0.024 Uiso 1 1 calc R . . . .
C523 C 0.0881(3) 0.3349(3) 0.1980(2) 0.0224(7) Uani 1 1 d . U . . .
H523 H 0.079993 0.263086 0.203117 0.027 Uiso 1 1 calc R . . . .
C524 C 0.0711(3) 0.3603(3) 0.2749(2) 0.0193(7) Uani 1 1 d . U . . .
H524 H 0.053124 0.306224 0.331680 0.023 Uiso 1 1 calc R . . . .
C525 C 0.0900(3) 0.3263(3) 0.6093(2) 0.0205(7) Uani 1 1 d . U . . .
H525 H 0.081676 0.277723 0.583059 0.025 Uiso 1 1 calc R . . . .
C526 C 0.1060(3) 0.2876(3) 0.6957(2) 0.0258(8) Uani 1 1 d . U . . .
H526 H 0.109167 0.211563 0.727611 0.031 Uiso 1 1 calc R . . . .
C527 C 0.1174(3) 0.3609(3) 0.7354(2) 0.0247(8) Uani 1 1 d . U . . .
H527 H 0.127434 0.332750 0.793289 0.030 Uiso 1 1 calc R . . . .
C528 C 0.1140(3) 0.4761(3) 0.6892(2) 0.0203(7) Uani 1 1 d . U . . .
H528 H 0.121583 0.525050 0.715446 0.024 Uiso 1 1 calc R . . . .
C529 C 0.1702(3) 0.9270(3) 0.5669(2) 0.0171(7) Uani 1 1 d . U . . .
H529 H 0.162212 0.870300 0.622395 0.020 Uiso 1 1 calc R . . . .
C530 C 0.1976(3) 1.0314(3) 0.5547(2) 0.0219(7) Uani 1 1 d . U . . .
H530 H 0.206496 1.045024 0.603152 0.026 Uiso 1 1 calc R . . . .
C531 C 0.2124(3) 1.1168(3) 0.4704(2) 0.0219(7) Uani 1 1 d . U . . .
H531 H 0.231838 1.185496 0.464227 0.026 Uiso 1 1 calc R . . . .
C532 C 0.1984(3) 1.1010(3) 0.3959(2) 0.0171(7) Uani 1 1 d . U . . .
H532 H 0.208765 1.157452 0.340175 0.020 Uiso 1 1 calc R . . . .
C321 C 0.7092(14) -0.2245(12) 0.6753(8) 0.0224(14) Uani 0.4543 1 d . U P C 2
H32D H 0.715270 -0.191046 0.716681 0.027 Uiso 0.4543 1 calc R . P C 2
H32E H 0.626974 -0.210669 0.671628 0.027 Uiso 0.4543 1 calc R . P C 2
C322 C 0.7447(7) -0.3503(6) 0.7100(5) 0.0253(15) Uani 0.4543 1 d . U P C 2
H32F H 0.704098 -0.379410 0.773514 0.030 Uiso 0.4543 1 calc R . P C 2
H32G H 0.830084 -0.362525 0.704471 0.030 Uiso 0.4543 1 calc R . P C 2
C323 C 0.7155(8) -0.4173(7) 0.6612(6) 0.0291(18) Uani 0.4543 1 d . U P C 2
H32H H 0.764933 -0.397312 0.599639 0.035 Uiso 0.4543 1 calc R . P C 2
H32I H 0.632301 -0.399095 0.659798 0.035 Uiso 0.4543 1 calc R . P C 2
C324 C 0.7388(12) -0.5441(9) 0.7101(7) 0.044(3) Uani 0.4543 1 d . U P C 2
H32J H 0.820523 -0.561640 0.713282 0.065 Uiso 0.4543 1 calc GR . P C 2
H32K H 0.724014 -0.584527 0.677374 0.065 Uiso 0.4543 1 calc GR . P C 2
H32L H 0.686351 -0.564608 0.769846 0.065 Uiso 0.4543 1 calc GR . P C 2
C325 C 0.7987(3) -0.1686(3) 0.5753(2) 0.0273(5) Uani 0.4543 1 d . U P C 2
C326 C 0.653(2) 0.273(3) 0.2607(17) 0.0382(19) Uani 0.3192 1 d . . P D 2
H32M H 0.623110 0.217086 0.250812 0.057 Uiso 0.3192 1 calc GR . P D 2
H32N H 0.628278 0.345442 0.223206 0.057 Uiso 0.3192 1 calc GR . P D 2
H32O H 0.622068 0.267720 0.322737 0.057 Uiso 0.3192 1 calc GR . P D 2
C327 C 0.7911(10) 0.2555(10) 0.2372(10) 0.0273(5) Uani 0.3192 1 d . U P D 2
H32P H 0.823634 0.304921 0.253631 0.033 Uiso 0.3192 1 calc R . P D 2
H32Q H 0.825383 0.266874 0.173602 0.033 Uiso 0.3192 1 calc R . P D 2
C328 C 0.8145(4) 0.1273(3) 0.2978(2) 0.0367(9) Uani 0.3192 1 d . . P D 2
C221 C 0.755(4) 0.550(3) 0.406(3) 0.0385(13) Uani 0.1612 1 d . U P E 2
H22D H 0.830162 0.582870 0.370998 0.046 Uiso 0.1612 1 calc R . P E 2
H22E H 0.693743 0.609425 0.416420 0.046 Uiso 0.1612 1 calc R . P E 2
C222 C 0.769(3) 0.463(3) 0.496(3) 0.065(2) Uani 0.1612 1 d . U P E 2
H22F H 0.719332 0.487539 0.544240 0.097 Uiso 0.1612 1 calc GR . P E 2
H22G H 0.851473 0.453575 0.497082 0.097 Uiso 0.1612 1 calc GR . P E 2
H22H H 0.746256 0.393946 0.501388 0.097 Uiso 0.1612 1 calc GR . P E 2
C223 C 0.7155(3) 0.4782(3) 0.3535(2) 0.0332(7) Uani 0.1612 1 d . . P E 2


_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
N201 C201 1.538(4) . ?
N201 C206 1.520(3) . ?
N201 C211 1.517(4) . ?
N201 C216 1.526(3) . ?
C201 H20A 0.9700 . ?
C201 H20B 0.9700 . ?
C201 C202 1.520(4) . ?
C202 H20C 0.9700 . ?
C202 H20D 0.9700 . ?
C202 C203 1.542(4) . ?
C203 H20E 0.9700 . ?
C203 H20F 0.9700 . ?
C203 C204 1.479(7) . ?
C204 H20G 0.9700 . ?
C204 H20H 0.9700 . ?
C204 C205 1.557(8) . ?
C205 H20I 0.9600 . ?
C205 H20J 0.9600 . ?
C205 H20K 0.9600 . ?
C206 H20L 0.9700 . ?
C206 H20M 0.9700 . ?
C206 C207 1.530(4) . ?
C207 H20N 0.9700 . ?
C207 H20O 0.9700 . ?
C207 C208 1.541(5) . ?
C208 H20P 0.9700 . ?
C208 H20Q 0.9700 . ?
C208 C209 1.520(5) . ?
C209 H20R 0.9700 . ?
C209 H20S 0.9700 . ?
C209 C210 1.530(5) . ?
C210 H21A 0.9600 . ?
C210 H21B 0.9600 . ?
C210 H21C 0.9600 . ?
C211 H21D 0.9700 . ?
C211 H21E 0.9700 . ?
C211 C212 1.529(4) . ?
C212 H21F 0.9700 . ?
C212 H21G 0.9700 . ?
C212 C213 1.542(4) . ?
C213 H21H 0.9700 . ?
C213 H21I 0.9700 . ?
C213 C214 1.522(5) . ?
C214 H21J 0.9700 . ?
C214 H21K 0.9700 . ?
C214 C215 1.523(4) . ?
C215 H21L 0.9600 . ?
C215 H21M 0.9600 . ?
C215 H21N 0.9600 . ?
C216 H21O 0.9700 . ?
C216 H21P 0.9700 . ?
C216 C217 1.522(4) . ?
C217 H21Q 0.9700 . ?
C217 H21R 0.9700 . ?
C217 C218 1.529(4) . ?
C218 H21S 0.9700 . ?
C218 H21T 0.9700 . ?
C218 C219 1.525(4) . ?
C219 H21U 0.9700 . ?
C219 H21V 0.9700 . ?
C219 C220 1.524(5) . ?
C220 H22A 0.9600 . ?
C220 H22B 0.9600 . ?
C220 H22C 0.9600 . ?
N301 C301 1.520(4) . ?
N301 C306 1.528(3) . ?
N301 C311 1.527(3) . ?
N301 C316 1.531(4) . ?
C301 H30A 0.9700 . ?
C301 H30B 0.9700 . ?
C301 C302 1.521(4) . ?
C302 H30C 0.9700 . ?
C302 H30D 0.9700 . ?
C302 C303 1.528(4) . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C304 1.516(4) . ?
C304 H30G 0.9700 . ?
C304 H30H 0.9700 . ?
C304 C305 1.523(5) . ?
C305 H30I 0.9600 . ?
C305 H30J 0.9600 . ?
C305 H30K 0.9600 . ?
C306 H30L 0.9700 . ?
C306 H30M 0.9700 . ?
C306 C307 1.526(4) . ?
C307 H30N 0.9700 . ?
C307 H30O 0.9700 . ?
C307 C308 1.540(5) . ?
C308 H30P 0.9700 . ?
C308 H30Q 0.9700 . ?
C308 C309 1.544(5) . ?
C309 H30R 0.9700 . ?
C309 H30S 0.9700 . ?
C309 C310 1.532(4) . ?
C310 H31A 0.9600 . ?
C310 H31B 0.9600 . ?
C310 H31C 0.9600 . ?
C311 H31D 0.9700 . ?
C311 H31E 0.9700 . ?
C311 C312 1.533(4) . ?
C312 H31F 0.9700 . ?
C312 H31G 0.9700 . ?
C312 C313 1.531(4) . ?
C313 H31H 0.9700 . ?
C313 H31I 0.9700 . ?
C313 C314 1.516(7) . ?
C314 H31J 0.9700 . ?
C314 H31K 0.9700 . ?
C314 C315 1.532(11) . ?
C315 H31L 0.9600 . ?
C315 H31M 0.9600 . ?
C315 H31N 0.9600 . ?
C316 H31O 0.9700 . ?
C316 H31P 0.9700 . ?
C316 C317 1.448(11) . ?
C317 H31Q 0.9700 . ?
C317 H31R 0.9700 . ?
C317 C318 1.562(12) . ?
C318 H31S 0.9700 . ?
C318 H31T 0.9700 . ?
C318 C319 1.501(8) . ?
C319 H31U 0.9700 . ?
C319 H31V 0.9700 . ?
C319 C320 1.532(11) . ?
C320 H32A 0.9600 . ?
C320 H32B 0.9600 . ?
C320 H32C 0.9600 . ?
V0AA O0AA 1.610(2) . ?
V0AA N101 2.041(3) . ?
V0AA N102 2.038(3) . ?
V0AA N103 2.046(3) . ?
V0AA N104 2.029(3) . ?
N101 C101 1.382(4) . ?
N101 C104 1.384(4) . ?
N102 C105 1.387(4) . ?
N102 C108 1.396(4) . ?
N103 C109 1.384(4) . ?
N103 C112 1.383(4) . ?
N104 C113 1.397(4) . ?
N104 C116 1.391(4) . ?
N105 C104 1.352(4) . ?
N105 C105 1.324(4) . ?
N106 C108 1.311(4) . ?
N106 C109 1.357(4) . ?
N107 C112 1.356(4) . ?
N107 C113 1.313(4) . ?
N108 C101 1.352(4) . ?
N108 C116 1.324(4) . ?
C101 C102 1.437(4) . ?
C102 C103 1.416(4) . ?
C102 C117 1.407(4) . ?
C103 C104 1.448(4) . ?
C103 C120 1.397(4) . ?
C105 C106 1.458(4) . ?
C106 C107 1.408(4) . ?
C106 C121 1.397(4) . ?
C107 C108 1.468(4) . ?
C107 C124 1.402(4) . ?
C109 C110 1.438(4) . ?
C110 C111 1.411(4) . ?
C110 C125 1.420(5) . ?
C111 C112 1.432(4) . ?
C111 C128 1.414(4) . ?
C113 C114 1.463(4) . ?
C114 C115 1.398(4) . ?
C114 C129 1.393(4) . ?
C115 C116 1.456(4) . ?
C115 C132 1.407(4) . ?
C117 H117 0.9300 . ?
C117 C118 1.392(4) . ?
C118 H118 0.9300 . ?
C118 C119 1.412(4) . ?
C119 H119 0.9300 . ?
C119 C120 1.390(4) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.388(4) . ?
C122 H122 0.9300 . ?
C122 C123 1.416(5) . ?
C123 H123 0.9300 . ?
C123 C124 1.395(4) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.376(5) . ?
C126 H126 0.9300 . ?
C126 C127 1.423(5) . ?
C127 H127 0.9300 . ?
C127 C128 1.380(5) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.388(5) . ?
C130 H130 0.9300 . ?
C130 C131 1.401(5) . ?
C131 H131 0.9300 . ?
C131 C132 1.406(4) . ?
C132 H132 0.9300 . ?
V1AA O1AA 1.605(2) . ?
V1AA N501 2.030(3) . ?
V1AA N502 2.040(3) . ?
V1AA N503 2.036(3) . ?
V1AA N504 2.042(3) . ?
N501 C501 1.392(4) . ?
N501 C504 1.396(4) . ?
N502 C505 1.394(4) . ?
N502 C508 1.381(4) . ?
N503 C509 1.392(4) . ?
N503 C512 1.396(4) . ?
N504 C513 1.384(4) . ?
N504 C516 1.398(4) . ?
N505 C504 1.318(4) . ?
N505 C505 1.348(4) . ?
N506 C508 1.348(4) . ?
N506 C509 1.315(4) . ?
N507 C512 1.314(4) . ?
N507 C513 1.365(4) . ?
N508 C501 1.316(4) . ?
N508 C516 1.349(4) . ?
C501 C502 1.464(4) . ?
C502 C503 1.394(4) . ?
C502 C517 1.408(4) . ?
C503 C504 1.466(4) . ?
C503 C520 1.400(4) . ?
C505 C506 1.444(4) . ?
C506 C507 1.412(4) . ?
C506 C521 1.405(4) . ?
C507 C508 1.442(4) . ?
C507 C524 1.405(4) . ?
C509 C510 1.466(5) . ?
C510 C511 1.398(4) . ?
C510 C525 1.395(5) . ?
C511 C512 1.468(4) . ?
C511 C528 1.386(5) . ?
C513 C514 1.433(4) . ?
C514 C515 1.410(4) . ?
C514 C529 1.409(4) . ?
C515 C516 1.442(4) . ?
C515 C532 1.409(4) . ?
C517 H517 0.9300 . ?
C517 C518 1.390(4) . ?
C518 H518 0.9300 . ?
C518 C519 1.408(5) . ?
C519 H519 0.9300 . ?
C519 C520 1.392(5) . ?
C520 H520 0.9300 . ?
C521 H521 0.9300 . ?
C521 C522 1.376(4) . ?
C522 H522 0.9300 . ?
C522 C523 1.430(5) . ?
C523 H523 0.9300 . ?
C523 C524 1.386(5) . ?
C524 H524 0.9300 . ?
C525 H525 0.9300 . ?
C525 C526 1.394(5) . ?
C526 H526 0.9300 . ?
C526 C527 1.398(5) . ?
C527 H527 0.9300 . ?
C527 C528 1.403(5) . ?
C528 H528 0.9300 . ?
C529 H529 0.9300 . ?
C529 C530 1.389(4) . ?
C530 H530 0.9300 . ?
C530 C531 1.407(5) . ?
C531 H531 0.9300 . ?
C531 C532 1.395(4) . ?
C532 H532 0.9300 . ?
C321 H32D 0.9700 . ?
C321 H32E 0.9700 . ?
C321 C322 1.534(16) . ?
C321 C325 1.644(13) . ?
C322 H32F 0.9700 . ?
C322 H32G 0.9700 . ?
C322 C323 1.543(10) . ?
C323 H32H 0.9700 . ?
C323 H32I 0.9700 . ?
C323 C324 1.551(13) . ?
C324 H32J 0.9600 . ?
C324 H32K 0.9600 . ?
C324 H32L 0.9600 . ?
C326 H32M 0.9600 . ?
C326 H32N 0.9600 . ?
C326 H32O 0.9600 . ?
C326 C327 1.54(3) . ?
C327 H32P 0.9700 . ?
C327 H32Q 0.9700 . ?
C327 C328 1.611(13) . ?
C221 H22D 0.9700 . ?
C221 H22E 0.9700 . ?
C221 C222 1.52(5) . ?
C221 C223 1.72(4) . ?
C222 H22F 0.9600 . ?
C222 H22G 0.9600 . ?
C222 H22H 0.9600 . ?

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
C206 N201 C201 107.4(2) . . ?
C206 N201 C216 109.8(2) . . ?
C211 N201 C201 111.0(2) . . ?
C211 N201 C206 110.7(2) . . ?
C211 N201 C216 107.8(2) . . ?
C216 N201 C201 110.2(2) . . ?
N201 C201 H20A 108.5 . . ?
N201 C201 H20B 108.5 . . ?
H20A C201 H20B 107.5 . . ?
C202 C201 N201 115.1(2) . . ?
C202 C201 H20A 108.5 . . ?
C202 C201 H20B 108.5 . . ?
C201 C202 H20C 109.4 . . ?
C201 C202 H20D 109.4 . . ?
C201 C202 C203 111.2(3) . . ?
H20C C202 H20D 108.0 . . ?
C203 C202 H20C 109.4 . . ?
C203 C202 H20D 109.4 . . ?
C202 C203 H20E 108.1 . . ?
C202 C203 H20F 108.1 . . ?
H20E C203 H20F 107.3 . . ?
C204 C203 C202 116.9(3) . . ?
C204 C203 H20E 108.1 . . ?
C204 C203 H20F 108.1 . . ?
C203 C204 H20G 109.2 . . ?
C203 C204 H20H 109.2 . . ?
C203 C204 C205 112.2(4) . . ?
H20G C204 H20H 107.9 . . ?
C205 C204 H20G 109.2 . . ?
C205 C204 H20H 109.2 . . ?
C204 C205 H20I 109.5 . . ?
C204 C205 H20J 109.5 . . ?
C204 C205 H20K 109.5 . . ?
H20I C205 H20J 109.5 . . ?
H20I C205 H20K 109.5 . . ?
H20J C205 H20K 109.5 . . ?
N201 C206 H20L 108.2 . . ?
N201 C206 H20M 108.2 . . ?
N201 C206 C207 116.4(2) . . ?
H20L C206 H20M 107.3 . . ?
C207 C206 H20L 108.2 . . ?
C207 C206 H20M 108.2 . . ?
C206 C207 H20N 109.8 . . ?
C206 C207 H20O 109.8 . . ?
C206 C207 C208 109.5(3) . . ?
H20N C207 H20O 108.2 . . ?
C208 C207 H20N 109.8 . . ?
C208 C207 H20O 109.8 . . ?
C207 C208 H20P 108.6 . . ?
C207 C208 H20Q 108.6 . . ?
H20P C208 H20Q 107.6 . . ?
C209 C208 C207 114.5(3) . . ?
C209 C208 H20P 108.6 . . ?
C209 C208 H20Q 108.6 . . ?
C208 C209 H20R 108.6 . . ?
C208 C209 H20S 108.6 . . ?
C208 C209 C210 114.6(3) . . ?
H20R C209 H20S 107.6 . . ?
C210 C209 H20R 108.6 . . ?
C210 C209 H20S 108.6 . . ?
C209 C210 H21A 109.5 . . ?
C209 C210 H21B 109.5 . . ?
C209 C210 H21C 109.5 . . ?
H21A C210 H21B 109.5 . . ?
H21A C210 H21C 109.5 . . ?
H21B C210 H21C 109.5 . . ?
N201 C211 H21D 108.6 . . ?
N201 C211 H21E 108.6 . . ?
N201 C211 C212 114.8(2) . . ?
H21D C211 H21E 107.5 . . ?
C212 C211 H21D 108.6 . . ?
C212 C211 H21E 108.6 . . ?
C211 C212 H21F 109.6 . . ?
C211 C212 H21G 109.6 . . ?
C211 C212 C213 110.1(2) . . ?
H21F C212 H21G 108.2 . . ?
C213 C212 H21F 109.6 . . ?
C213 C212 H21G 109.6 . . ?
C212 C213 H21H 108.4 . . ?
C212 C213 H21I 108.4 . . ?
H21H C213 H21I 107.5 . . ?
C214 C213 C212 115.4(3) . . ?
C214 C213 H21H 108.4 . . ?
C214 C213 H21I 108.4 . . ?
C213 C214 H21J 108.7 . . ?
C213 C214 H21K 108.7 . . ?
C213 C214 C215 114.1(3) . . ?
H21J C214 H21K 107.6 . . ?
C215 C214 H21J 108.7 . . ?
C215 C214 H21K 108.7 . . ?
C214 C215 H21L 109.5 . . ?
C214 C215 H21M 109.5 . . ?
C214 C215 H21N 109.5 . . ?
H21L C215 H21M 109.5 . . ?
H21L C215 H21N 109.5 . . ?
H21M C215 H21N 109.5 . . ?
N201 C216 H21O 108.4 . . ?
N201 C216 H21P 108.4 . . ?
H21O C216 H21P 107.5 . . ?
C217 C216 N201 115.3(2) . . ?
C217 C216 H21O 108.4 . . ?
C217 C216 H21P 108.4 . . ?
C216 C217 H21Q 109.4 . . ?
C216 C217 H21R 109.4 . . ?
C216 C217 C218 111.1(2) . . ?
H21Q C217 H21R 108.0 . . ?
C218 C217 H21Q 109.4 . . ?
C218 C217 H21R 109.4 . . ?
C217 C218 H21S 108.9 . . ?
C217 C218 H21T 108.9 . . ?
H21S C218 H21T 107.7 . . ?
C219 C218 C217 113.4(3) . . ?
C219 C218 H21S 108.9 . . ?
C219 C218 H21T 108.9 . . ?
C218 C219 H21U 108.8 . . ?
C218 C219 H21V 108.8 . . ?
H21U C219 H21V 107.7 . . ?
C220 C219 C218 113.8(3) . . ?
C220 C219 H21U 108.8 . . ?
C220 C219 H21V 108.8 . . ?
C219 C220 H22A 109.5 . . ?
C219 C220 H22B 109.5 . . ?
C219 C220 H22C 109.5 . . ?
H22A C220 H22B 109.5 . . ?
H22A C220 H22C 109.5 . . ?
H22B C220 H22C 109.5 . . ?
C301 N301 C306 106.2(2) . . ?
C301 N301 C311 111.2(2) . . ?
C301 N301 C316 111.4(2) . . ?
C306 N301 C316 110.9(2) . . ?
C311 N301 C306 111.6(2) . . ?
C311 N301 C316 105.7(2) . . ?
N301 C301 H30A 108.1 . . ?
N301 C301 H30B 108.1 . . ?
N301 C301 C302 116.8(2) . . ?
H30A C301 H30B 107.3 . . ?
C302 C301 H30A 108.1 . . ?
C302 C301 H30B 108.1 . . ?
C301 C302 H30C 110.0 . . ?
C301 C302 H30D 110.0 . . ?
C301 C302 C303 108.5(3) . . ?
H30C C302 H30D 108.4 . . ?
C303 C302 H30C 110.0 . . ?
C303 C302 H30D 110.0 . . ?
C302 C303 H30E 108.6 . . ?
C302 C303 H30F 108.6 . . ?
H30E C303 H30F 107.6 . . ?
C304 C303 C302 114.5(3) . . ?
C304 C303 H30E 108.6 . . ?
C304 C303 H30F 108.6 . . ?
C303 C304 H30G 109.1 . . ?
C303 C304 H30H 109.1 . . ?
C303 C304 C305 112.6(3) . . ?
H30G C304 H30H 107.8 . . ?
C305 C304 H30G 109.1 . . ?
C305 C304 H30H 109.1 . . ?
C304 C305 H30I 109.5 . . ?
C304 C305 H30J 109.5 . . ?
C304 C305 H30K 109.5 . . ?
H30I C305 H30J 109.5 . . ?
H30I C305 H30K 109.5 . . ?
H30J C305 H30K 109.5 . . ?
N301 C306 H30L 108.2 . . ?
N301 C306 H30M 108.2 . . ?
H30L C306 H30M 107.3 . . ?
C307 C306 N301 116.4(2) . . ?
C307 C306 H30L 108.2 . . ?
C307 C306 H30M 108.2 . . ?
C306 C307 H30N 109.9 . . ?
C306 C307 H30O 109.9 . . ?
C306 C307 C308 109.1(3) . . ?
H30N C307 H30O 108.3 . . ?
C308 C307 H30N 109.9 . . ?
C308 C307 H30O 109.9 . . ?
C307 C308 H30P 109.1 . . ?
C307 C308 H30Q 109.1 . . ?
C307 C308 C309 112.3(3) . . ?
H30P C308 H30Q 107.9 . . ?
C309 C308 H30P 109.1 . . ?
C309 C308 H30Q 109.1 . . ?
C308 C309 H30R 109.0 . . ?
C308 C309 H30S 109.0 . . ?
H30R C309 H30S 107.8 . . ?
C310 C309 C308 112.9(3) . . ?
C310 C309 H30R 109.0 . . ?
C310 C309 H30S 109.0 . . ?
C309 C310 H31A 109.5 . . ?
C309 C310 H31B 109.5 . . ?
C309 C310 H31C 109.5 . . ?
H31A C310 H31B 109.5 . . ?
H31A C310 H31C 109.5 . . ?
H31B C310 H31C 109.5 . . ?
N301 C311 H31D 108.3 . . ?
N301 C311 H31E 108.3 . . ?
N301 C311 C312 116.0(2) . . ?
H31D C311 H31E 107.4 . . ?
C312 C311 H31D 108.3 . . ?
C312 C311 H31E 108.3 . . ?
C311 C312 H31F 109.3 . . ?
C311 C312 H31G 109.3 . . ?
H31F C312 H31G 107.9 . . ?
C313 C312 C311 111.7(3) . . ?
C313 C312 H31F 109.3 . . ?
C313 C312 H31G 109.3 . . ?
C312 C313 H31H 108.5 . . ?
C312 C313 H31I 108.5 . . ?
H31H C313 H31I 107.5 . . ?
C314 C313 C312 114.9(4) . . ?
C314 C313 H31H 108.5 . . ?
C314 C313 H31I 108.5 . . ?
C313 C314 H31J 108.2 . . ?
C313 C314 H31K 108.2 . . ?
C313 C314 C315 116.2(6) . . ?
H31J C314 H31K 107.4 . . ?
C315 C314 H31J 108.2 . . ?
C315 C314 H31K 108.2 . . ?
C314 C315 H31L 109.5 . . ?
C314 C315 H31M 109.5 . . ?
C314 C315 H31N 109.5 . . ?
H31L C315 H31M 109.5 . . ?
H31L C315 H31N 109.5 . . ?
H31M C315 H31N 109.5 . . ?
N301 C316 H31O 107.6 . . ?
N301 C316 H31P 107.6 . . ?
H31O C316 H31P 107.0 . . ?
C317 C316 N301 118.9(5) . . ?
C317 C316 H31O 107.6 . . ?
C317 C316 H31P 107.6 . . ?
C316 C317 H31Q 109.6 . . ?
C316 C317 H31R 109.6 . . ?
C316 C317 C318 110.3(6) . . ?
H31Q C317 H31R 108.1 . . ?
C318 C317 H31Q 109.6 . . ?
C318 C317 H31R 109.6 . . ?
C317 C318 H31S 108.8 . . ?
C317 C318 H31T 108.8 . . ?
H31S C318 H31T 107.7 . . ?
C319 C318 C317 113.9(6) . . ?
C319 C318 H31S 108.8 . . ?
C319 C318 H31T 108.8 . . ?
C318 C319 H31U 109.1 . . ?
C318 C319 H31V 109.1 . . ?
C318 C319 C320 112.6(6) . . ?
H31U C319 H31V 107.8 . . ?
C320 C319 H31U 109.1 . . ?
C320 C319 H31V 109.1 . . ?
C319 C320 H32A 109.5 . . ?
C319 C320 H32B 109.5 . . ?
C319 C320 H32C 109.5 . . ?
H32A C320 H32B 109.5 . . ?
H32A C320 H32C 109.5 . . ?
H32B C320 H32C 109.5 . . ?
O0AA V0AA N101 105.65(11) . . ?
O0AA V0AA N102 105.83(11) . . ?
O0AA V0AA N103 106.26(11) . . ?
O0AA V0AA N104 106.24(11) . . ?
N101 V0AA N103 148.09(10) . . ?
N102 V0AA N101 85.49(10) . . ?
N102 V0AA N103 85.53(10) . . ?
N104 V0AA N101 85.50(10) . . ?
N104 V0AA N102 147.92(11) . . ?
N104 V0AA N103 86.06(10) . . ?
C101 N101 V0AA 126.4(2) . . ?
C101 N101 C104 107.7(2) . . ?
C104 N101 V0AA 124.3(2) . . ?
C105 N102 V0AA 124.5(2) . . ?
C105 N102 C108 108.0(3) . . ?
C108 N102 V0AA 125.6(2) . . ?
C109 N103 V0AA 126.6(2) . . ?
C112 N103 V0AA 125.2(2) . . ?
C112 N103 C109 107.7(3) . . ?
C113 N104 V0AA 125.0(2) . . ?
C116 N104 V0AA 127.5(2) . . ?
C116 N104 C113 107.2(3) . . ?
C105 N105 C104 121.8(3) . . ?
C108 N106 C109 122.3(3) . . ?
C113 N107 C112 122.3(3) . . ?
C116 N108 C101 122.0(3) . . ?
N101 C101 C102 109.8(3) . . ?
N108 C101 N101 127.7(3) . . ?
N108 C101 C102 122.5(3) . . ?
C103 C102 C101 106.7(3) . . ?
C117 C102 C101 132.5(3) . . ?
C117 C102 C103 120.7(3) . . ?
C102 C103 C104 106.2(3) . . ?
C120 C103 C102 120.9(3) . . ?
C120 C103 C104 132.9(3) . . ?
N101 C104 C103 109.6(3) . . ?
N105 C104 N101 127.4(3) . . ?
N105 C104 C103 122.9(3) . . ?
N102 C105 C106 109.6(3) . . ?
N105 C105 N102 128.5(3) . . ?
N105 C105 C106 121.9(3) . . ?
C107 C106 C105 106.7(3) . . ?
C121 C106 C105 132.3(3) . . ?
C121 C106 C107 121.0(3) . . ?
C106 C107 C108 106.8(3) . . ?
C124 C107 C106 121.2(3) . . ?
C124 C107 C108 132.0(3) . . ?
N102 C108 C107 108.8(3) . . ?
N106 C108 N102 128.3(3) . . ?
N106 C108 C107 122.9(3) . . ?
N103 C109 C110 109.2(3) . . ?
N106 C109 N103 127.3(3) . . ?
N106 C109 C110 123.5(3) . . ?
C111 C110 C109 106.9(3) . . ?
C111 C110 C125 120.4(3) . . ?
C125 C110 C109 132.7(3) . . ?
C110 C111 C112 106.5(3) . . ?
C110 C111 C128 121.1(3) . . ?
C128 C111 C112 132.4(3) . . ?
N103 C112 C111 109.7(3) . . ?
N107 C112 N103 127.4(3) . . ?
N107 C112 C111 122.8(3) . . ?
N104 C113 C114 109.3(3) . . ?
N107 C113 N104 128.4(3) . . ?
N107 C113 C114 122.1(3) . . ?
C115 C114 C113 106.7(3) . . ?
C129 C114 C113 131.1(3) . . ?
C129 C114 C115 122.1(3) . . ?
C114 C115 C116 106.9(3) . . ?
C114 C115 C132 120.9(3) . . ?
C132 C115 C116 132.1(3) . . ?
N104 C116 C115 109.7(3) . . ?
N108 C116 N104 127.8(3) . . ?
N108 C116 C115 122.5(3) . . ?
C102 C117 H117 121.0 . . ?
C118 C117 C102 118.0(3) . . ?
C118 C117 H117 121.0 . . ?
C117 C118 H118 119.6 . . ?
C117 C118 C119 120.8(3) . . ?
C119 C118 H118 119.6 . . ?
C118 C119 H119 119.2 . . ?
C120 C119 C118 121.6(3) . . ?
C120 C119 H119 119.2 . . ?
C103 C120 H120 121.0 . . ?
C119 C120 C103 118.0(3) . . ?
C119 C120 H120 121.0 . . ?
C106 C121 H121 121.0 . . ?
C122 C121 C106 118.0(3) . . ?
C122 C121 H121 121.0 . . ?
C121 C122 H122 119.4 . . ?
C121 C122 C123 121.1(3) . . ?
C123 C122 H122 119.4 . . ?
C122 C123 H123 119.4 . . ?
C124 C123 C122 121.1(3) . . ?
C124 C123 H123 119.4 . . ?
C107 C124 H124 121.3 . . ?
C123 C124 C107 117.5(3) . . ?
C123 C124 H124 121.3 . . ?
C110 C125 H125 121.1 . . ?
C126 C125 C110 117.9(3) . . ?
C126 C125 H125 121.1 . . ?
C125 C126 H126 119.2 . . ?
C125 C126 C127 121.6(3) . . ?
C127 C126 H126 119.2 . . ?
C126 C127 H127 119.4 . . ?
C128 C127 C126 121.2(3) . . ?
C128 C127 H127 119.4 . . ?
C111 C128 H128 121.1 . . ?
C127 C128 C111 117.8(3) . . ?
C127 C128 H128 121.1 . . ?
C114 C129 H129 121.4 . . ?
C130 C129 C114 117.2(3) . . ?
C130 C129 H129 121.4 . . ?
C129 C130 H130 119.2 . . ?
C129 C130 C131 121.5(3) . . ?
C131 C130 H130 119.2 . . ?
C130 C131 H131 119.3 . . ?
C130 C131 C132 121.5(3) . . ?
C132 C131 H131 119.3 . . ?
C115 C132 H132 121.6 . . ?
C131 C132 C115 116.8(3) . . ?
C131 C132 H132 121.6 . . ?
O1AA V1AA N501 105.17(11) . . ?
O1AA V1AA N502 106.14(11) . . ?
O1AA V1AA N503 105.79(11) . . ?
O1AA V1AA N504 105.94(11) . . ?
N501 V1AA N502 85.75(10) . . ?
N501 V1AA N503 149.04(11) . . ?
N501 V1AA N504 85.77(10) . . ?
N502 V1AA N504 147.91(11) . . ?
N503 V1AA N502 86.10(10) . . ?
N503 V1AA N504 85.45(10) . . ?
C501 N501 V1AA 124.7(2) . . ?
C501 N501 C504 107.8(3) . . ?
C504 N501 V1AA 125.9(2) . . ?
C505 N502 V1AA 126.6(2) . . ?
C508 N502 V1AA 124.5(2) . . ?
C508 N502 C505 108.0(3) . . ?
C509 N503 V1AA 125.4(2) . . ?
C509 N503 C512 107.6(3) . . ?
C512 N503 V1AA 126.7(2) . . ?
C513 N504 V1AA 126.3(2) . . ?
C513 N504 C516 107.5(3) . . ?
C516 N504 V1AA 125.1(2) . . ?
C504 N505 C505 122.4(3) . . ?
C509 N506 C508 121.9(3) . . ?
C512 N507 C513 121.8(3) . . ?
C501 N508 C516 122.3(3) . . ?
N501 C501 C502 109.0(3) . . ?
N508 C501 N501 128.2(3) . . ?
N508 C501 C502 122.7(3) . . ?
C503 C502 C501 107.1(3) . . ?
C503 C502 C517 121.0(3) . . ?
C517 C502 C501 131.8(3) . . ?
C502 C503 C504 106.9(3) . . ?
C502 C503 C520 121.7(3) . . ?
C520 C503 C504 131.4(3) . . ?
N501 C504 C503 109.0(3) . . ?
N505 C504 N501 128.2(3) . . ?
N505 C504 C503 122.8(3) . . ?
N502 C505 C506 109.1(3) . . ?
N505 C505 N502 127.1(3) . . ?
N505 C505 C506 123.8(3) . . ?
C507 C506 C505 106.5(3) . . ?
C521 C506 C505 133.0(3) . . ?
C521 C506 C507 120.5(3) . . ?
C506 C507 C508 107.0(3) . . ?
C524 C507 C506 121.1(3) . . ?
C524 C507 C508 131.8(3) . . ?
N502 C508 C507 109.2(3) . . ?
N506 C508 N502 128.2(3) . . ?
N506 C508 C507 122.3(3) . . ?
N503 C509 C510 109.2(3) . . ?
N506 C509 N503 128.5(3) . . ?
N506 C509 C510 122.3(3) . . ?
C511 C510 C509 107.3(3) . . ?
C525 C510 C509 131.2(3) . . ?
C525 C510 C511 121.5(3) . . ?
C510 C511 C512 106.5(3) . . ?
C528 C511 C510 121.4(3) . . ?
C528 C511 C512 132.0(3) . . ?
N503 C512 C511 109.4(3) . . ?
N507 C512 N503 128.2(3) . . ?
N507 C512 C511 122.3(3) . . ?
N504 C513 C514 109.9(3) . . ?
N507 C513 N504 127.4(3) . . ?
N507 C513 C514 122.6(3) . . ?
C515 C514 C513 106.7(3) . . ?
C529 C514 C513 132.8(3) . . ?
C529 C514 C515 120.6(3) . . ?
C514 C515 C516 107.0(3) . . ?
C532 C515 C514 121.3(3) . . ?
C532 C515 C516 131.7(3) . . ?
N504 C516 C515 108.9(3) . . ?
N508 C516 N504 127.2(3) . . ?
N508 C516 C515 123.9(3) . . ?
C502 C517 H517 121.2 . . ?
C518 C517 C502 117.5(3) . . ?
C518 C517 H517 121.2 . . ?
C517 C518 H518 119.5 . . ?
C517 C518 C519 121.1(3) . . ?
C519 C518 H518 119.5 . . ?
C518 C519 H519 119.2 . . ?
C520 C519 C518 121.5(3) . . ?
C520 C519 H519 119.2 . . ?
C503 C520 H520 121.4 . . ?
C519 C520 C503 117.2(3) . . ?
C519 C520 H520 121.4 . . ?
C506 C521 H521 120.8 . . ?
C522 C521 C506 118.3(3) . . ?
C522 C521 H521 120.8 . . ?
C521 C522 H522 119.3 . . ?
C521 C522 C523 121.4(3) . . ?
C523 C522 H522 119.3 . . ?
C522 C523 H523 119.8 . . ?
C524 C523 C522 120.5(3) . . ?
C524 C523 H523 119.8 . . ?
C507 C524 H524 120.9 . . ?
C523 C524 C507 118.1(3) . . ?
C523 C524 H524 120.9 . . ?
C510 C525 H525 121.4 . . ?
C526 C525 C510 117.3(3) . . ?
C526 C525 H525 121.4 . . ?
C525 C526 H526 119.4 . . ?
C525 C526 C527 121.3(3) . . ?
C527 C526 H526 119.4 . . ?
C526 C527 H527 119.4 . . ?
C526 C527 C528 121.1(3) . . ?
C528 C527 H527 119.4 . . ?
C511 C528 C527 117.4(3) . . ?
C511 C528 H528 121.3 . . ?
C527 C528 H528 121.3 . . ?
C514 C529 H529 121.0 . . ?
C530 C529 C514 118.0(3) . . ?
C530 C529 H529 121.0 . . ?
C529 C530 H530 119.3 . . ?
C529 C530 C531 121.3(3) . . ?
C531 C530 H530 119.3 . . ?
C530 C531 H531 119.3 . . ?
C532 C531 C530 121.5(3) . . ?
C532 C531 H531 119.3 . . ?
C515 C532 H532 121.3 . . ?
C531 C532 C515 117.3(3) . . ?
C531 C532 H532 121.3 . . ?
H32D C321 H32E 108.2 . . ?
C322 C321 H32D 109.8 . . ?
C322 C321 H32E 109.8 . . ?
C322 C321 C325 109.4(8) . . ?
C325 C321 H32D 109.8 . . ?
C325 C321 H32E 109.8 . . ?
C321 C322 H32F 108.5 . . ?
C321 C322 H32G 108.5 . . ?
C321 C322 C323 115.1(7) . . ?
H32F C322 H32G 107.5 . . ?
C323 C322 H32F 108.5 . . ?
C323 C322 H32G 108.5 . . ?
C322 C323 H32H 109.6 . . ?
C322 C323 H32I 109.6 . . ?
C322 C323 C324 110.5(7) . . ?
H32H C323 H32I 108.1 . . ?
C324 C323 H32H 109.6 . . ?
C324 C323 H32I 109.6 . . ?
C323 C324 H32J 109.5 . . ?
C323 C324 H32K 109.5 . . ?
C323 C324 H32L 109.5 . . ?
H32J C324 H32K 109.5 . . ?
H32J C324 H32L 109.5 . . ?
H32K C324 H32L 109.5 . . ?
H32M C326 H32N 109.5 . . ?
H32M C326 H32O 109.5 . . ?
H32N C326 H32O 109.5 . . ?
C327 C326 H32M 109.5 . . ?
C327 C326 H32N 109.5 . . ?
C327 C326 H32O 109.5 . . ?
C326 C327 H32P 111.4 . . ?
C326 C327 H32Q 111.4 . . ?
C326 C327 C328 102.0(14) . . ?
H32P C327 H32Q 109.2 . . ?
C328 C327 H32P 111.4 . . ?
C328 C327 H32Q 111.4 . . ?
H22D C221 H22E 108.9 . . ?
C222 C221 H22D 110.9 . . ?
C222 C221 H22E 110.9 . . ?
C222 C221 C223 104(3) . . ?
C223 C221 H22D 110.9 . . ?
C223 C221 H22E 110.9 . . ?
C221 C222 H22F 109.5 . . ?
C221 C222 H22G 109.5 . . ?
C221 C222 H22H 109.5 . . ?
H22F C222 H22G 109.5 . . ?
H22F C222 H22H 109.5 . . ?
H22G C222 H22H 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.926(15)
2 0.074(15)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/0-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_TIOPc2MDABCOI
_database_code_depnum_ccdc_archive 'CCDC 1581414'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-03-23
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.03.22 svn.r3403 for OlexSys, GUI svn.r5332)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of titanyl phthalocyanine with two N-methyldiazabicyclooctanium cations and iodine anion'
_chemical_formula_moiety         'C32 H16 N8 O Ti, 2(C7 H15 N2), I'
_chemical_formula_sum            'C46 H46 I N12 O Ti'
_chemical_formula_weight         957.75
_chemical_melting_point          'not measured'
_chemical_oxdiff_formula         'C209 H190 N19 Ti19 O19 I1'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.5787(7)
_cell_length_b                   13.0731(5)
_cell_length_c                   25.4452(17)
_cell_angle_alpha                90
_cell_angle_beta                 91.733(5)
_cell_angle_gamma                90
_cell_volume                     4182.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18294
_cell_measurement_temperature    130.00(14)
_cell_measurement_theta_max      29.0490
_cell_measurement_theta_min      1.6320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0493
0 0 -1 0.0362
0 -1 0 0.1209
0 1 0 0.0833
-1 0 0 0.1022
1 0 0 0.1022

_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.085
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0005 -0.0002 0.9967 -0.0242 -0.0134 0.0020
-0.0005 0.0002 -0.9967 0.0242 0.0134 -0.0020
-0.0005 -0.9985 -0.0006 -0.0024 0.0121 0.0528
0.0005 0.9985 0.0006 0.0024 -0.0121 -0.0528
-0.9979 -0.0003 0.0001 0.0290 -0.0467 0.0121
0.9979 0.0003 -0.0001 -0.0290 0.0467 -0.0121

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            50066
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         1.601
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  29.00   1.00   50.00    --  -12.20  37.00  60.00   66
  2  ω    -33.00  -7.00   1.00   50.00    --  -12.20 -37.00 -90.00   26
  3  ω    -61.00  12.00   1.00   50.00    --  -12.20 -37.00  30.00   73
  4  ω    -14.00  13.00   1.00   50.00    --  -12.20 -57.00 -30.00   27
  5  ω     -3.00  23.00   1.00   50.00    --   11.89 -37.00-150.00   26
  6  ω    -27.00  -1.00   1.00   50.00    --  -12.20 -57.00   0.00   26
  7  ω     35.00  69.00   1.00   50.00    --  -12.20  19.00 -30.00   34
  8  ω    -40.00  10.00   1.00   50.00    --  -12.20 -57.00 120.00   50
  9  ω    -80.00 -54.00   1.00   50.00    --  -12.20 -37.00-150.00   26
 10  ω     34.00  61.00   1.00   50.00    --  -12.20  19.00 120.00   27
 11  ω    -85.00   9.00   1.00   50.00    --  -12.20 -57.00-120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0290920000
_diffrn_orient_matrix_UB_12      0.0024691000
_diffrn_orient_matrix_UB_13      -0.0243004000
_diffrn_orient_matrix_UB_21      0.0467852000
_diffrn_orient_matrix_UB_22      -0.0121765000
_diffrn_orient_matrix_UB_23      -0.0135124000
_diffrn_orient_matrix_UB_31      -0.0121176000
_diffrn_orient_matrix_UB_32      -0.0528522000
_diffrn_orient_matrix_UB_33      0.0019681000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8487
_reflns_number_total             10563
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.102
_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)+(0.0287P)²+7.5995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1006
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,H30H), C305(H30I,
 H30J), C306(H30K,H30L), C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F),
 C204(H20G,H20H), C205(H20I,H20J), C206(H20K,H20L)
2.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132)
2.c Idealised Me refined as rotating group:
 C307(H30M,H30N,H30O), C207(H20M,H20N,H20O)
;
_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 0.53917(4) 0.00054(4) 0.59169(2) 0.01526(10) Uani 1 1 d . . . . .
O O 0.51835(16) -0.02650(16) 0.65386(8) 0.0234(4) Uani 1 1 d . . . . .
N101 N 0.68380(17) 0.07338(17) 0.59211(9) 0.0168(5) Uani 1 1 d . . . . .
N102 N 0.47411(18) 0.14309(17) 0.57685(9) 0.0169(5) Uani 1 1 d . . . . .
N103 N 0.40947(17) -0.05493(17) 0.54907(9) 0.0170(5) Uani 1 1 d . . . . .
N104 N 0.62012(17) -0.12405(17) 0.56328(9) 0.0160(5) Uani 1 1 d . . . . .
N105 N 0.62795(18) 0.25075(17) 0.60199(9) 0.0188(5) Uani 1 1 d . . . . .
N106 N 0.29064(18) 0.09219(18) 0.55329(9) 0.0180(5) Uani 1 1 d . . . . .
N107 N 0.46594(18) -0.23254(17) 0.53950(9) 0.0179(5) Uani 1 1 d . . . . .
N108 N 0.80322(18) -0.07362(17) 0.58726(9) 0.0178(5) Uani 1 1 d . . . . .
C101 C 0.7819(2) 0.0240(2) 0.59497(11) 0.0174(5) Uani 1 1 d . . . . .
C102 C 0.8641(2) 0.1005(2) 0.60752(11) 0.0186(6) Uani 1 1 d . . . . .
C103 C 0.8135(2) 0.1955(2) 0.61135(11) 0.0185(6) Uani 1 1 d . . . . .
C104 C 0.6994(2) 0.1775(2) 0.60153(10) 0.0173(5) Uani 1 1 d . . . . .
C105 C 0.5233(2) 0.2348(2) 0.58979(11) 0.0181(6) Uani 1 1 d . . . . .
C106 C 0.4451(2) 0.3153(2) 0.58820(11) 0.0190(6) Uani 1 1 d . . . . .
C107 C 0.3470(2) 0.2696(2) 0.57313(11) 0.0181(5) Uani 1 1 d . . . . .
C108 C 0.3671(2) 0.1617(2) 0.56615(11) 0.0182(6) Uani 1 1 d . . . . .
C109 C 0.3112(2) -0.0058(2) 0.54533(11) 0.0170(5) Uani 1 1 d . . . . .
C110 C 0.2293(2) -0.0822(2) 0.53250(10) 0.0176(5) Uani 1 1 d . . . . .
C111 C 0.2807(2) -0.1771(2) 0.52832(11) 0.0182(6) Uani 1 1 d . . . . .
C112 C 0.3944(2) -0.1588(2) 0.53863(11) 0.0172(5) Uani 1 1 d . . . . .
C113 C 0.5709(2) -0.2157(2) 0.55040(11) 0.0175(5) Uani 1 1 d . . . . .
C114 C 0.6484(2) -0.2963(2) 0.55292(11) 0.0179(5) Uani 1 1 d . . . . .
C115 C 0.7473(2) -0.2509(2) 0.56661(11) 0.0183(6) Uani 1 1 d . . . . .
C116 C 0.7276(2) -0.1425(2) 0.57244(10) 0.0170(5) Uani 1 1 d . . . . .
C117 C 0.9742(2) 0.0921(2) 0.61251(11) 0.0227(6) Uani 1 1 d . . . . .
H117 H 1.007782 0.028895 0.610502 0.027 Uiso 1 1 calc R . . . .
C118 C 1.0323(2) 0.1812(2) 0.62059(12) 0.0258(6) Uani 1 1 d . . . . .
H118 H 1.106083 0.177552 0.623406 0.031 Uiso 1 1 calc R . . . .
C119 C 0.9825(2) 0.2764(2) 0.62459(12) 0.0248(6) Uani 1 1 d . . . . .
H119 H 1.023584 0.334808 0.630197 0.030 Uiso 1 1 calc R . . . .
C120 C 0.8722(2) 0.2849(2) 0.62027(11) 0.0213(6) Uani 1 1 d . . . . .
H120 H 0.838718 0.347959 0.623238 0.026 Uiso 1 1 calc R . . . .
C121 C 0.4525(2) 0.4208(2) 0.59824(12) 0.0241(6) Uani 1 1 d . . . . .
H121 H 0.517084 0.450747 0.608152 0.029 Uiso 1 1 calc R . . . .
C122 C 0.3605(3) 0.4788(2) 0.59292(12) 0.0287(7) Uani 1 1 d . . . . .
H122 H 0.363420 0.548780 0.599424 0.034 Uiso 1 1 calc R . . . .
C123 C 0.2624(2) 0.4334(2) 0.57778(12) 0.0280(7) Uani 1 1 d . . . . .
H123 H 0.201793 0.473976 0.574731 0.034 Uiso 1 1 calc R . . . .
C124 C 0.2545(2) 0.3294(2) 0.56737(11) 0.0234(6) Uani 1 1 d . . . . .
H124 H 0.189887 0.300151 0.556877 0.028 Uiso 1 1 calc R . . . .
C125 C 0.1189(2) -0.0750(2) 0.52608(11) 0.0211(6) Uani 1 1 d . . . . .
H125 H 0.084634 -0.012139 0.527976 0.025 Uiso 1 1 calc R . . . .
C126 C 0.0618(2) -0.1645(2) 0.51677(11) 0.0245(6) Uani 1 1 d . . . . .
H126 H -0.011913 -0.161647 0.513168 0.029 Uiso 1 1 calc R . . . .
C127 C 0.1137(2) -0.2595(2) 0.51270(12) 0.0247(6) Uani 1 1 d . . . . .
H127 H 0.073658 -0.318244 0.506397 0.030 Uiso 1 1 calc R . . . .
C128 C 0.2239(2) -0.2668(2) 0.51796(11) 0.0215(6) Uani 1 1 d . . . . .
H128 H 0.258399 -0.329290 0.514683 0.026 Uiso 1 1 calc R . . . .
C129 C 0.6392(2) -0.4029(2) 0.54686(11) 0.0217(6) Uani 1 1 d . . . . .
H129 H 0.574616 -0.432840 0.536916 0.026 Uiso 1 1 calc R . . . .
C130 C 0.7292(2) -0.4618(2) 0.55615(12) 0.0253(6) Uani 1 1 d . . . . .
H130 H 0.724448 -0.532633 0.553363 0.030 Uiso 1 1 calc R . . . .
C131 C 0.8279(2) -0.4166(2) 0.56974(12) 0.0263(7) Uani 1 1 d . . . . .
H131 H 0.887154 -0.458066 0.575498 0.032 Uiso 1 1 calc R . . . .
C132 C 0.8384(2) -0.3116(2) 0.57470(12) 0.0223(6) Uani 1 1 d . . . . .
H132 H 0.903933 -0.282130 0.583160 0.027 Uiso 1 1 calc R . . . .
N301 N 0.6686(2) 0.2032(2) 0.28081(12) 0.0320(6) Uani 1 1 d . . . . .
N302 N 0.8645(2) 0.18434(19) 0.30945(10) 0.0240(5) Uani 1 1 d . . . . .
C301 C 0.6949(3) 0.0954(3) 0.28967(18) 0.0452(10) Uani 1 1 d . . . . .
H30A H 0.688966 0.058728 0.256568 0.054 Uiso 1 1 calc R . . . .
H30B H 0.644461 0.065764 0.313406 0.054 Uiso 1 1 calc R . . . .
C302 C 0.8087(3) 0.0827(2) 0.31328(14) 0.0314(7) Uani 1 1 d . . . . .
H30C H 0.805989 0.061465 0.349742 0.038 Uiso 1 1 calc R . . . .
H30D H 0.846750 0.030975 0.294007 0.038 Uiso 1 1 calc R . . . .
C303 C 0.6912(3) 0.2610(3) 0.32870(14) 0.0400(9) Uani 1 1 d . . . . .
H30E H 0.650868 0.232269 0.357040 0.048 Uiso 1 1 calc R . . . .
H30F H 0.668324 0.331227 0.323549 0.048 Uiso 1 1 calc R . . . .
C304 C 0.8099(3) 0.2597(3) 0.34448(13) 0.0341(8) Uani 1 1 d . . . . .
H30G H 0.840218 0.327372 0.340304 0.041 Uiso 1 1 calc R . . . .
H30H H 0.819378 0.239526 0.381008 0.041 Uiso 1 1 calc R . . . .
C305 C 0.7367(3) 0.2424(3) 0.23960(13) 0.0332(7) Uani 1 1 d . . . . .
H30I H 0.725924 0.315533 0.235791 0.040 Uiso 1 1 calc R . . . .
H30J H 0.717036 0.210199 0.206370 0.040 Uiso 1 1 calc R . . . .
C306 C 0.8545(2) 0.2210(2) 0.25293(11) 0.0227(6) Uani 1 1 d . . . . .
H30K H 0.881298 0.169167 0.229487 0.027 Uiso 1 1 calc R . . . .
H30L H 0.896003 0.282857 0.248607 0.027 Uiso 1 1 calc R . . . .
C307 C 0.9789(3) 0.1742(3) 0.32559(14) 0.0345(8) Uani 1 1 d . . . . .
H30M H 0.984627 0.152029 0.361526 0.052 Uiso 1 1 calc GR . . . .
H30N H 1.013538 0.239196 0.322133 0.052 Uiso 1 1 calc GR . . . .
H30O H 1.012218 0.124893 0.303496 0.052 Uiso 1 1 calc GR . . . .
N201 N 0.6665(3) 0.8560(2) 0.24775(11) 0.0362(7) Uani 1 1 d . . . . .
N202 N 0.6827(2) 0.66104(19) 0.25062(10) 0.0250(5) Uani 1 1 d . . . . .
C201 C 0.5650(3) 0.8101(3) 0.26118(18) 0.0456(10) Uani 1 1 d . . . . .
H20A H 0.510972 0.830019 0.235184 0.055 Uiso 1 1 calc R . . . .
H20B H 0.543968 0.835839 0.295058 0.055 Uiso 1 1 calc R . . . .
C202 C 0.5717(3) 0.6923(3) 0.26343(15) 0.0340(8) Uani 1 1 d . . . . .
H20C H 0.554660 0.668357 0.298262 0.041 Uiso 1 1 calc R . . . .
H20D H 0.521142 0.662502 0.238260 0.041 Uiso 1 1 calc R . . . .
C203 C 0.7465(3) 0.8256(3) 0.28732(14) 0.0382(8) Uani 1 1 d . . . . .
H20E H 0.726043 0.850784 0.321422 0.046 Uiso 1 1 calc R . . . .
H20F H 0.814066 0.856533 0.279146 0.046 Uiso 1 1 calc R . . . .
C204 C 0.7597(3) 0.7086(3) 0.28998(14) 0.0365(8) Uani 1 1 d . . . . .
H20G H 0.832006 0.689876 0.281889 0.044 Uiso 1 1 calc R . . . .
H20H H 0.745268 0.684332 0.325069 0.044 Uiso 1 1 calc R . . . .
C205 C 0.6978(4) 0.8174(3) 0.19657(14) 0.0456(10) Uani 1 1 d . . . . .
H20I H 0.766020 0.846372 0.187893 0.055 Uiso 1 1 calc R . . . .
H20J H 0.645869 0.838727 0.169818 0.055 Uiso 1 1 calc R . . . .
C206 C 0.7058(3) 0.6998(3) 0.19674(13) 0.0329(7) Uani 1 1 d . . . . .
H20K H 0.655183 0.671233 0.171256 0.039 Uiso 1 1 calc R . . . .
H20L H 0.776690 0.678961 0.187164 0.039 Uiso 1 1 calc R . . . .
C207 C 0.6916(3) 0.5472(2) 0.25235(16) 0.0391(9) Uani 1 1 d . . . . .
H20M H 0.674527 0.523251 0.286748 0.059 Uiso 1 1 calc GR . . . .
H20N H 0.762942 0.527304 0.244678 0.059 Uiso 1 1 calc GR . . . .
H20O H 0.643022 0.517821 0.226732 0.059 Uiso 1 1 calc GR . . . .
I3A I 0.99687(2) 0.47326(2) 0.29271(2) 0.03335(7) Uani 1 1 d . . . A 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 O 1.650(2) . ?
Ti1 N101 2.053(2) . ?
Ti1 N102 2.065(2) . ?
Ti1 N103 2.063(2) . ?
Ti1 N104 2.063(2) . ?
N101 C101 1.392(3) . ?
N101 C104 1.395(3) . ?
N102 C105 1.385(4) . ?
N102 C108 1.387(4) . ?
N103 C109 1.394(3) . ?
N103 C112 1.395(3) . ?
N104 C113 1.384(3) . ?
N104 C116 1.386(3) . ?
N105 C104 1.314(4) . ?
N105 C105 1.359(4) . ?
N106 C108 1.356(4) . ?
N106 C109 1.323(4) . ?
N107 C112 1.319(4) . ?
N107 C113 1.358(4) . ?
N108 C101 1.320(3) . ?
N108 C116 1.355(4) . ?
C101 C102 1.467(4) . ?
C102 C103 1.401(4) . ?
C102 C117 1.392(4) . ?
C103 C104 1.468(4) . ?
C103 C120 1.397(4) . ?
C105 C106 1.440(4) . ?
C106 C107 1.413(4) . ?
C106 C121 1.405(4) . ?
C107 C108 1.444(4) . ?
C107 C124 1.406(4) . ?
C109 C110 1.466(4) . ?
C110 C111 1.404(4) . ?
C110 C125 1.396(4) . ?
C111 C112 1.466(4) . ?
C111 C128 1.394(4) . ?
C113 C114 1.436(4) . ?
C114 C115 1.412(4) . ?
C114 C129 1.406(4) . ?
C115 C116 1.447(4) . ?
C115 C132 1.404(4) . ?
C117 H117 0.9300 . ?
C117 C118 1.387(4) . ?
C118 H118 0.9300 . ?
C118 C119 1.398(4) . ?
C119 H119 0.9300 . ?
C119 C120 1.394(4) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.387(4) . ?
C122 H122 0.9300 . ?
C122 C123 1.413(5) . ?
C123 H123 0.9300 . ?
C123 C124 1.388(4) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.390(4) . ?
C126 H126 0.9300 . ?
C126 C127 1.407(4) . ?
C127 H127 0.9300 . ?
C127 C128 1.392(4) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.384(4) . ?
C130 H130 0.9300 . ?
C130 C131 1.409(4) . ?
C131 H131 0.9300 . ?
C131 C132 1.384(4) . ?
C132 H132 0.9300 . ?
N301 C301 1.464(4) . ?
N301 C303 1.454(5) . ?
N301 C305 1.467(4) . ?
N302 C302 1.507(4) . ?
N302 C304 1.508(4) . ?
N302 C306 1.517(4) . ?
N302 C307 1.491(4) . ?
C301 H30A 0.9700 . ?
C301 H30B 0.9700 . ?
C301 C302 1.544(5) . ?
C302 H30C 0.9700 . ?
C302 H30D 0.9700 . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C304 1.535(5) . ?
C304 H30G 0.9700 . ?
C304 H30H 0.9700 . ?
C305 H30I 0.9700 . ?
C305 H30J 0.9700 . ?
C305 C306 1.536(4) . ?
C306 H30K 0.9700 . ?
C306 H30L 0.9700 . ?
C307 H30M 0.9600 . ?
C307 H30N 0.9600 . ?
C307 H30O 0.9600 . ?
N201 C201 1.460(5) . ?
N201 C203 1.457(5) . ?
N201 C205 1.462(5) . ?
N202 C202 1.501(4) . ?
N202 C204 1.506(4) . ?
N202 C206 1.498(4) . ?
N202 C207 1.493(4) . ?
C201 H20A 0.9700 . ?
C201 H20B 0.9700 . ?
C201 C202 1.543(5) . ?
C202 H20C 0.9700 . ?
C202 H20D 0.9700 . ?
C203 H20E 0.9700 . ?
C203 H20F 0.9700 . ?
C203 C204 1.539(5) . ?
C204 H20G 0.9700 . ?
C204 H20H 0.9700 . ?
C205 H20I 0.9700 . ?
C205 H20J 0.9700 . ?
C205 C206 1.541(5) . ?
C206 H20K 0.9700 . ?
C206 H20L 0.9700 . ?
C207 H20M 0.9600 . ?
C207 H20N 0.9600 . ?
C207 H20O 0.9600 . ?

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
O Ti1 N101 105.12(10) . . ?
O Ti1 N102 107.17(10) . . ?
O Ti1 N103 106.43(10) . . ?
O Ti1 N104 105.14(10) . . ?
N101 Ti1 N102 85.91(9) . . ?
N101 Ti1 N103 148.45(9) . . ?
N101 Ti1 N104 85.48(9) . . ?
N103 Ti1 N102 85.32(9) . . ?
N103 Ti1 N104 85.93(9) . . ?
N104 Ti1 N102 147.69(9) . . ?
C101 N101 Ti1 124.67(18) . . ?
C101 N101 C104 108.9(2) . . ?
C104 N101 Ti1 124.99(18) . . ?
C105 N102 Ti1 124.48(18) . . ?
C105 N102 C108 108.6(2) . . ?
C108 N102 Ti1 124.84(18) . . ?
C109 N103 Ti1 124.01(18) . . ?
C109 N103 C112 108.7(2) . . ?
C112 N103 Ti1 122.89(18) . . ?
C113 N104 Ti1 122.97(18) . . ?
C113 N104 C116 108.5(2) . . ?
C116 N104 Ti1 124.58(18) . . ?
C104 N105 C105 123.0(2) . . ?
C109 N106 C108 123.0(2) . . ?
C112 N107 C113 122.9(2) . . ?
C101 N108 C116 122.6(2) . . ?
N101 C101 C102 108.3(2) . . ?
N108 C101 N101 128.6(2) . . ?
N108 C101 C102 123.1(2) . . ?
C103 C102 C101 107.5(2) . . ?
C117 C102 C101 131.3(3) . . ?
C117 C102 C103 121.1(3) . . ?
C102 C103 C104 106.8(2) . . ?
C120 C103 C102 120.9(3) . . ?
C120 C103 C104 132.2(3) . . ?
N101 C104 C103 108.5(2) . . ?
N105 C104 N101 128.3(2) . . ?
N105 C104 C103 123.2(2) . . ?
N102 C105 C106 109.0(2) . . ?
N105 C105 N102 127.6(2) . . ?
N105 C105 C106 123.4(2) . . ?
C107 C106 C105 106.8(2) . . ?
C121 C106 C105 132.0(3) . . ?
C121 C106 C107 121.1(3) . . ?
C106 C107 C108 106.9(2) . . ?
C124 C107 C106 120.4(3) . . ?
C124 C107 C108 132.7(3) . . ?
N102 C108 C107 108.6(2) . . ?
N106 C108 N102 127.3(2) . . ?
N106 C108 C107 124.0(2) . . ?
N103 C109 C110 108.5(2) . . ?
N106 C109 N103 127.8(2) . . ?
N106 C109 C110 123.7(2) . . ?
C111 C110 C109 107.3(2) . . ?
C125 C110 C109 132.1(3) . . ?
C125 C110 C111 120.6(3) . . ?
C110 C111 C112 106.9(2) . . ?
C128 C111 C110 121.5(3) . . ?
C128 C111 C112 131.5(3) . . ?
N103 C112 C111 108.6(2) . . ?
N107 C112 N103 128.3(2) . . ?
N107 C112 C111 123.0(2) . . ?
N104 C113 C114 109.0(2) . . ?
N107 C113 N104 127.9(2) . . ?
N107 C113 C114 123.0(2) . . ?
C115 C114 C113 107.2(2) . . ?
C129 C114 C113 132.0(3) . . ?
C129 C114 C115 120.8(3) . . ?
C114 C115 C116 106.5(2) . . ?
C132 C115 C114 120.5(3) . . ?
C132 C115 C116 132.9(3) . . ?
N104 C116 C115 108.8(2) . . ?
N108 C116 N104 127.2(2) . . ?
N108 C116 C115 123.9(2) . . ?
C102 C117 H117 121.1 . . ?
C118 C117 C102 117.8(3) . . ?
C118 C117 H117 121.1 . . ?
C117 C118 H118 119.2 . . ?
C117 C118 C119 121.6(3) . . ?
C119 C118 H118 119.2 . . ?
C118 C119 H119 119.6 . . ?
C120 C119 C118 120.8(3) . . ?
C120 C119 H119 119.6 . . ?
C103 C120 H120 121.1 . . ?
C119 C120 C103 117.8(3) . . ?
C119 C120 H120 121.1 . . ?
C106 C121 H121 121.0 . . ?
C122 C121 C106 117.9(3) . . ?
C122 C121 H121 121.0 . . ?
C121 C122 H122 119.5 . . ?
C121 C122 C123 121.1(3) . . ?
C123 C122 H122 119.5 . . ?
C122 C123 H123 119.3 . . ?
C124 C123 C122 121.4(3) . . ?
C124 C123 H123 119.3 . . ?
C107 C124 H124 121.0 . . ?
C123 C124 C107 118.1(3) . . ?
C123 C124 H124 121.0 . . ?
C110 C125 H125 121.0 . . ?
C126 C125 C110 118.0(3) . . ?
C126 C125 H125 121.0 . . ?
C125 C126 H126 119.4 . . ?
C125 C126 C127 121.1(3) . . ?
C127 C126 H126 119.4 . . ?
C126 C127 H127 119.5 . . ?
C128 C127 C126 121.1(3) . . ?
C128 C127 H127 119.5 . . ?
C111 C128 H128 121.2 . . ?
C127 C128 C111 117.6(3) . . ?
C127 C128 H128 121.2 . . ?
C114 C129 H129 121.0 . . ?
C130 C129 C114 118.0(3) . . ?
C130 C129 H129 121.0 . . ?
C129 C130 H130 119.4 . . ?
C129 C130 C131 121.2(3) . . ?
C131 C130 H130 119.4 . . ?
C130 C131 H131 119.3 . . ?
C132 C131 C130 121.3(3) . . ?
C132 C131 H131 119.3 . . ?
C115 C132 H132 120.9 . . ?
C131 C132 C115 118.2(3) . . ?
C131 C132 H132 120.9 . . ?
C301 N301 C305 108.2(3) . . ?
C303 N301 C301 109.5(3) . . ?
C303 N301 C305 108.3(3) . . ?
C302 N302 C304 108.5(2) . . ?
C302 N302 C306 108.4(2) . . ?
C304 N302 C306 109.1(2) . . ?
C307 N302 C302 110.6(2) . . ?
C307 N302 C304 110.4(3) . . ?
C307 N302 C306 109.9(2) . . ?
N301 C301 H30A 109.3 . . ?
N301 C301 H30B 109.3 . . ?
N301 C301 C302 111.5(3) . . ?
H30A C301 H30B 108.0 . . ?
C302 C301 H30A 109.3 . . ?
C302 C301 H30B 109.3 . . ?
N302 C302 C301 107.9(3) . . ?
N302 C302 H30C 110.1 . . ?
N302 C302 H30D 110.1 . . ?
C301 C302 H30C 110.1 . . ?
C301 C302 H30D 110.1 . . ?
H30C C302 H30D 108.4 . . ?
N301 C303 H30E 109.2 . . ?
N301 C303 H30F 109.2 . . ?
N301 C303 C304 112.2(3) . . ?
H30E C303 H30F 107.9 . . ?
C304 C303 H30E 109.2 . . ?
C304 C303 H30F 109.2 . . ?
N302 C304 C303 108.0(3) . . ?
N302 C304 H30G 110.1 . . ?
N302 C304 H30H 110.1 . . ?
C303 C304 H30G 110.1 . . ?
C303 C304 H30H 110.1 . . ?
H30G C304 H30H 108.4 . . ?
N301 C305 H30I 109.4 . . ?
N301 C305 H30J 109.4 . . ?
N301 C305 C306 111.1(3) . . ?
H30I C305 H30J 108.0 . . ?
C306 C305 H30I 109.4 . . ?
C306 C305 H30J 109.4 . . ?
N302 C306 C305 108.5(2) . . ?
N302 C306 H30K 110.0 . . ?
N302 C306 H30L 110.0 . . ?
C305 C306 H30K 110.0 . . ?
C305 C306 H30L 110.0 . . ?
H30K C306 H30L 108.4 . . ?
N302 C307 H30M 109.5 . . ?
N302 C307 H30N 109.5 . . ?
N302 C307 H30O 109.5 . . ?
H30M C307 H30N 109.5 . . ?
H30M C307 H30O 109.5 . . ?
H30N C307 H30O 109.5 . . ?
C201 N201 C205 109.1(3) . . ?
C203 N201 C201 108.4(3) . . ?
C203 N201 C205 108.8(3) . . ?
C202 N202 C204 109.1(3) . . ?
C206 N202 C202 108.3(3) . . ?
C206 N202 C204 109.3(3) . . ?
C207 N202 C202 109.5(3) . . ?
C207 N202 C204 110.3(3) . . ?
C207 N202 C206 110.3(3) . . ?
N201 C201 H20A 109.2 . . ?
N201 C201 H20B 109.2 . . ?
N201 C201 C202 111.9(3) . . ?
H20A C201 H20B 107.9 . . ?
C202 C201 H20A 109.2 . . ?
C202 C201 H20B 109.2 . . ?
N202 C202 C201 108.2(3) . . ?
N202 C202 H20C 110.0 . . ?
N202 C202 H20D 110.0 . . ?
C201 C202 H20C 110.0 . . ?
C201 C202 H20D 110.0 . . ?
H20C C202 H20D 108.4 . . ?
N201 C203 H20E 109.2 . . ?
N201 C203 H20F 109.2 . . ?
N201 C203 C204 111.9(3) . . ?
H20E C203 H20F 107.9 . . ?
C204 C203 H20E 109.2 . . ?
C204 C203 H20F 109.2 . . ?
N202 C204 C203 108.3(3) . . ?
N202 C204 H20G 110.0 . . ?
N202 C204 H20H 110.0 . . ?
C203 C204 H20G 110.0 . . ?
C203 C204 H20H 110.0 . . ?
H20G C204 H20H 108.4 . . ?
N201 C205 H20I 109.4 . . ?
N201 C205 H20J 109.4 . . ?
N201 C205 C206 111.2(3) . . ?
H20I C205 H20J 108.0 . . ?
C206 C205 H20I 109.4 . . ?
C206 C205 H20J 109.4 . . ?
N202 C206 C205 109.0(3) . . ?
N202 C206 H20K 109.9 . . ?
N202 C206 H20L 109.9 . . ?
C205 C206 H20K 109.9 . . ?
C205 C206 H20L 109.9 . . ?
H20K C206 H20L 108.3 . . ?
N202 C207 H20M 109.5 . . ?
N202 C207 H20N 109.5 . . ?
N202 C207 H20O 109.5 . . ?
H20M C207 H20N 109.5 . . ?
H20M C207 H20O 109.5 . . ?
H20N C207 H20O 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_VOPc2MDABCOI
_database_code_depnum_ccdc_archive 'CCDC 1581417'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-03-20
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of vanadyl phthalocyanine with two N-methyldiazabicyclooctanium cations and iodine anion'
_chemical_formula_moiety         'C32 H16 N8 O V, 2(C7 H15 N2), I'
_chemical_formula_sum            'C46 H46 I N12 O V'
_chemical_formula_weight         960.79
_chemical_melting_point          'not measured'
_chemical_oxdiff_formula         'C46 H16 N8 O1 V1 Br1'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.5922(3)
_cell_length_b                   13.0726(2)
_cell_length_c                   25.4070(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.730(2)
_cell_angle_gamma                90
_cell_volume                     4180.41(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    28157
_cell_measurement_temperature    129.7(7)
_cell_measurement_theta_max      30.5660
_cell_measurement_theta_min      2.2250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.1255
0 -1 0 0.1255
-1 0 0 0.1752
1 0 0 0.2172
0 0 1 0.0361
0 0 -1 0.0361
1 1 0 0.1474

_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.072
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0014 0.9999 0.0008 0.0167 -0.0348 -0.0382
0.0014 -0.9999 -0.0008 -0.0167 0.0348 0.0382
-0.9986 -0.0001 0.0007 -0.0240 0.0320 -0.0397
0.9986 0.0001 -0.0007 0.0240 -0.0320 0.0397
-0.0003 0.0008 1.0002 0.0241 0.0139 -0.0022
0.0003 -0.0008 -1.0002 -0.0241 -0.0139 0.0022
0.9973 1.0000 0.0001 0.0406 -0.0667 0.0015

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            71075
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.873
_diffrn_reflns_theta_min         1.604
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      129.7(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00 -20.00   1.00   40.00    --  -18.47 -57.00 150.00   67
  2  ω    -26.00  18.00   1.00   40.00    --  -18.47  57.00  90.00   44
  3  ω    -50.00  58.00   1.00   40.00    --  -18.47  37.00 -60.00  108
  4  ω    -27.00  -1.00   1.00   40.00    --  -18.47 -60.00 -75.24   26
  5  ω    -40.00 -13.00   1.00   40.00    --  -18.47 -60.00 170.52   27
  6  ω    -97.00  13.00   1.00   40.00    --  -18.47 -60.00   4.60  110
  7  ω    -75.00  13.00   1.00   40.00    --  -18.47 -59.00  91.57   88
  8  ω     37.00  63.00   1.00   40.00    --  -18.47  19.00  90.00   26
  9  ω    -83.00   3.00   1.00   40.00    --  -18.47 -57.00-150.00   86
 10  ω    -45.00   0.00   1.00   40.00    --  -18.47  57.00 -30.00   45
 11  ω    -43.00 -16.00   1.00   40.00    --  -18.47 -57.00-120.00   27
 12  ω    -53.00 -30.00   1.00   40.00    --  -18.47 -37.00  60.00   23
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0240105000
_diffrn_orient_matrix_UB_12      0.0166788000
_diffrn_orient_matrix_UB_13      0.0241229000
_diffrn_orient_matrix_UB_21      -0.0319900000
_diffrn_orient_matrix_UB_22      -0.0348189000
_diffrn_orient_matrix_UB_23      0.0139009000
_diffrn_orient_matrix_UB_31      0.0397288000
_diffrn_orient_matrix_UB_32      -0.0381089000
_diffrn_orient_matrix_UB_33      -0.0021641000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10408
_reflns_number_total             12334
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         12334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+3.8331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0833
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F),
 C304(H30G,H30H), C305(H30I,H30J), C306(H30K,H30L)
2.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132)
2.c Idealised Me refined as rotating group:
 C207(H20M,H20N,H20O), C307(H30M,H30N,H30O)
;
_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
V1 V 0.96009(2) 0.50140(2) 0.40986(2) 0.01220(6) Uani 1 1 d . . . . .
O1 O 0.98087(11) 0.47643(10) 0.34886(5) 0.0192(3) Uani 1 1 d . . . . .
N101 N 1.08919(12) 0.44559(11) 0.45034(6) 0.0145(3) Uani 1 1 d . . . . .
N102 N 0.88073(12) 0.37709(11) 0.43637(6) 0.0138(3) Uani 1 1 d . . . . .
N103 N 0.81736(12) 0.57268(12) 0.40799(6) 0.0145(3) Uani 1 1 d . . . . .
N104 N 1.02492(12) 0.64175(11) 0.42322(6) 0.0144(3) Uani 1 1 d . . . . .
N105 N 1.03388(12) 0.26760(12) 0.46015(6) 0.0155(3) Uani 1 1 d . . . . .
N106 N 0.69736(12) 0.42633(12) 0.41243(6) 0.0159(3) Uani 1 1 d . . . . .
N107 N 0.87243(12) 0.75029(12) 0.39744(6) 0.0163(3) Uani 1 1 d . . . . .
N108 N 1.20890(12) 0.59193(12) 0.44647(6) 0.0161(3) Uani 1 1 d . . . . .
C101 C 1.18766(14) 0.49435(14) 0.45414(7) 0.0146(3) Uani 1 1 d . . . . .
C102 C 1.26976(14) 0.41818(14) 0.46729(7) 0.0155(3) Uani 1 1 d . . . . .
C103 C 1.21820(14) 0.32341(14) 0.47165(7) 0.0155(3) Uani 1 1 d . . . . .
C104 C 1.10498(14) 0.34182(14) 0.46104(7) 0.0146(3) Uani 1 1 d . . . . .
C105 C 0.92944(14) 0.28473(13) 0.44942(7) 0.0150(3) Uani 1 1 d . . . . .
C106 C 0.85200(14) 0.20416(14) 0.44701(7) 0.0152(3) Uani 1 1 d . . . . .
C107 C 0.75308(14) 0.24993(14) 0.43354(7) 0.0154(3) Uani 1 1 d . . . . .
C108 C 0.77325(14) 0.35788(14) 0.42757(7) 0.0146(3) Uani 1 1 d . . . . .
C109 C 0.71921(14) 0.52365(14) 0.40477(7) 0.0151(3) Uani 1 1 d . . . . .
C110 C 0.63668(14) 0.59994(14) 0.39192(7) 0.0158(3) Uani 1 1 d . . . . .
C111 C 0.68746(14) 0.69453(14) 0.38804(7) 0.0162(3) Uani 1 1 d . . . . .
C112 C 0.80132(14) 0.67671(14) 0.39803(7) 0.0149(3) Uani 1 1 d . . . . .
C113 C 0.97639(14) 0.73374(14) 0.41013(7) 0.0155(3) Uani 1 1 d . . . . .
C114 C 1.05439(15) 0.81413(14) 0.41162(7) 0.0167(3) Uani 1 1 d . . . . .
C115 C 1.15282(15) 0.76847(14) 0.42676(7) 0.0168(3) Uani 1 1 d . . . . .
C116 C 1.13214(14) 0.66097(14) 0.43367(7) 0.0153(3) Uani 1 1 d . . . . .
C117 C 1.38021(14) 0.42550(15) 0.47396(7) 0.0185(4) Uani 1 1 d . . . . .
H117 H 1.414507 0.488327 0.471988 0.022 Uiso 1 1 calc R . . . .
C118 C 1.43716(15) 0.33586(16) 0.48362(8) 0.0219(4) Uani 1 1 d . . . . .
H118 H 1.510791 0.338710 0.487374 0.026 Uiso 1 1 calc R . . . .
C119 C 1.38523(16) 0.24084(16) 0.48783(8) 0.0218(4) Uani 1 1 d . . . . .
H119 H 1.425105 0.182086 0.494388 0.026 Uiso 1 1 calc R . . . .
C120 C 1.27511(15) 0.23359(15) 0.48231(7) 0.0188(4) Uani 1 1 d . . . . .
H120 H 1.240618 0.171113 0.485616 0.023 Uiso 1 1 calc R . . . .
C121 C 0.86127(16) 0.09761(14) 0.45296(7) 0.0189(4) Uani 1 1 d . . . . .
H121 H 0.925851 0.067675 0.462818 0.023 Uiso 1 1 calc R . . . .
C122 C 0.77157(17) 0.03869(15) 0.44373(8) 0.0227(4) Uani 1 1 d . . . . .
H122 H 0.776487 -0.032113 0.446435 0.027 Uiso 1 1 calc R . . . .
C123 C 0.67216(17) 0.08400(16) 0.43021(8) 0.0236(4) Uani 1 1 d . . . . .
H123 H 0.613010 0.042474 0.424351 0.028 Uiso 1 1 calc R . . . .
C124 C 0.66170(15) 0.18921(15) 0.42558(8) 0.0195(4) Uani 1 1 d . . . . .
H124 H 0.596111 0.218853 0.417434 0.023 Uiso 1 1 calc R . . . .
C125 C 0.52669(15) 0.59086(15) 0.38704(7) 0.0194(4) Uani 1 1 d . . . . .
H125 H 0.493469 0.527513 0.389142 0.023 Uiso 1 1 calc R . . . .
C126 C 0.46818(15) 0.68033(16) 0.37888(8) 0.0221(4) Uani 1 1 d . . . . .
H126 H 0.394464 0.676666 0.376108 0.027 Uiso 1 1 calc R . . . .
C127 C 0.51816(16) 0.77562(16) 0.37476(8) 0.0222(4) Uani 1 1 d . . . . .
H127 H 0.477150 0.833977 0.369099 0.027 Uiso 1 1 calc R . . . .
C128 C 0.62867(15) 0.78433(15) 0.37903(8) 0.0193(4) Uani 1 1 d . . . . .
H128 H 0.662076 0.847414 0.376002 0.023 Uiso 1 1 calc R . . . .
C129 C 1.04706(16) 0.91996(14) 0.40159(8) 0.0207(4) Uani 1 1 d . . . . .
H129 H 0.982593 0.950086 0.391694 0.025 Uiso 1 1 calc R . . . .
C130 C 1.13913(18) 0.97770(16) 0.40698(8) 0.0253(4) Uani 1 1 d . . . . .
H130 H 1.136064 1.047699 0.400570 0.030 Uiso 1 1 calc R . . . .
C131 C 1.23766(17) 0.93263(16) 0.42199(8) 0.0250(4) Uani 1 1 d . . . . .
H131 H 1.298062 0.973388 0.425054 0.030 Uiso 1 1 calc R . . . .
C132 C 1.24558(16) 0.82844(15) 0.43224(8) 0.0203(4) Uani 1 1 d . . . . .
H132 H 1.310262 0.799076 0.442426 0.024 Uiso 1 1 calc R . . . .
N201 N 0.16218(17) 0.85637(15) 0.74833(8) 0.0317(4) Uani 1 1 d . . . . .
N202 N 0.18185(14) 0.66153(13) 0.75011(7) 0.0218(3) Uani 1 1 d . . . . .
C201 C 0.0621(2) 0.80867(19) 0.76288(12) 0.0396(6) Uani 1 1 d . . . . .
H20A H 0.006336 0.828760 0.737776 0.048 Uiso 1 1 calc R . . . .
H20B H 0.042677 0.833029 0.797347 0.048 Uiso 1 1 calc R . . . .
C202 C 0.07052(18) 0.69072(18) 0.76398(10) 0.0303(5) Uani 1 1 d . . . . .
H20C H 0.054853 0.665276 0.798761 0.036 Uiso 1 1 calc R . . . .
H20D H 0.019871 0.661085 0.738820 0.036 Uiso 1 1 calc R . . . .
C203 C 0.1924(3) 0.8188(2) 0.69657(9) 0.0416(6) Uani 1 1 d . . . . .
H20E H 0.259511 0.849380 0.687369 0.050 Uiso 1 1 calc R . . . .
H20F H 0.139129 0.839671 0.670335 0.050 Uiso 1 1 calc R . . . .
C204 C 0.20301(19) 0.70161(18) 0.69586(8) 0.0284(5) Uani 1 1 d . . . . .
H20G H 0.152433 0.672585 0.670472 0.034 Uiso 1 1 calc R . . . .
H20H H 0.273982 0.682441 0.685775 0.034 Uiso 1 1 calc R . . . .
C205 C 0.2452(2) 0.82626(18) 0.78719(10) 0.0339(5) Uani 1 1 d . . . . .
H20I H 0.226462 0.850936 0.821692 0.041 Uiso 1 1 calc R . . . .
H20J H 0.311908 0.857952 0.778155 0.041 Uiso 1 1 calc R . . . .
C206 C 0.25964(19) 0.70942(18) 0.78930(9) 0.0315(5) Uani 1 1 d . . . . .
H20K H 0.331770 0.691459 0.780614 0.038 Uiso 1 1 calc R . . . .
H20L H 0.246486 0.684481 0.824469 0.038 Uiso 1 1 calc R . . . .
C207 C 0.1928(2) 0.54766(17) 0.75132(11) 0.0362(6) Uani 1 1 d . . . . .
H20M H 0.264407 0.529141 0.743573 0.054 Uiso 1 1 calc GR . . . .
H20N H 0.144829 0.517938 0.725512 0.054 Uiso 1 1 calc GR . . . .
H20O H 0.176116 0.522800 0.785651 0.054 Uiso 1 1 calc GR . . . .
N301 N 0.16949(14) 0.29873(14) 0.28398(8) 0.0287(4) Uani 1 1 d . . . . .
N302 N 0.36709(13) 0.31576(13) 0.31040(6) 0.0204(3) Uani 1 1 d . . . . .
C301 C 0.19603(19) 0.40516(19) 0.29601(15) 0.0505(8) Uani 1 1 d . . . . .
H30A H 0.149330 0.430160 0.322817 0.061 Uiso 1 1 calc R . . . .
H30B H 0.183998 0.446366 0.264640 0.061 Uiso 1 1 calc R . . . .
C302 C 0.31224(17) 0.41788(16) 0.31552(9) 0.0260(4) Uani 1 1 d . . . . .
H30C H 0.347465 0.468988 0.294564 0.031 Uiso 1 1 calc R . . . .
H30D H 0.314803 0.440000 0.351975 0.031 Uiso 1 1 calc R . . . .
C303 C 0.23516(18) 0.2640(2) 0.24063(9) 0.0354(5) Uani 1 1 d . . . . .
H30E H 0.215525 0.301541 0.208889 0.042 Uiso 1 1 calc R . . . .
H30F H 0.221778 0.191954 0.234013 0.042 Uiso 1 1 calc R . . . .
C304 C 0.35419(15) 0.27990(15) 0.25359(7) 0.0196(4) Uani 1 1 d . . . . .
H30G H 0.392411 0.216281 0.248913 0.024 Uiso 1 1 calc R . . . .
H30H H 0.383026 0.330650 0.230117 0.024 Uiso 1 1 calc R . . . .
C305 C 0.1951(2) 0.2356(2) 0.33002(10) 0.0382(6) Uani 1 1 d . . . . .
H30I H 0.175466 0.165264 0.322439 0.046 Uiso 1 1 calc R . . . .
H30J H 0.153540 0.258655 0.359301 0.046 Uiso 1 1 calc R . . . .
C306 C 0.31354(19) 0.24017(17) 0.34591(9) 0.0301(5) Uani 1 1 d . . . . .
H30K H 0.322167 0.261568 0.382345 0.036 Uiso 1 1 calc R . . . .
H30L H 0.345424 0.173074 0.342344 0.036 Uiso 1 1 calc R . . . .
C307 C 0.48208(18) 0.32512(18) 0.32542(9) 0.0299(5) Uani 1 1 d . . . . .
H30M H 0.516275 0.260160 0.321065 0.045 Uiso 1 1 calc GR . . . .
H30N H 0.489455 0.346203 0.361538 0.045 Uiso 1 1 calc GR . . . .
H30O H 0.514541 0.375018 0.303322 0.045 Uiso 1 1 calc GR . . . .
I1 I 0.50244(2) 0.52688(2) 0.20725(2) 0.02933(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6128(13) . ?
V1 N101 2.0327(16) . ?
V1 N102 2.0331(15) . ?
V1 N103 2.0237(15) . ?
V1 N104 2.0326(15) . ?
N101 C101 1.395(2) . ?
N101 C104 1.397(2) . ?
N102 C105 1.390(2) . ?
N102 C108 1.388(2) . ?
N103 C109 1.392(2) . ?
N103 C112 1.397(2) . ?
N104 C113 1.385(2) . ?
N104 C116 1.391(2) . ?
N105 C104 1.320(2) . ?
N105 C105 1.354(2) . ?
N106 C108 1.356(2) . ?
N106 C109 1.317(2) . ?
N107 C112 1.315(2) . ?
N107 C113 1.356(2) . ?
N108 C101 1.319(2) . ?
N108 C116 1.355(2) . ?
C101 C102 1.467(2) . ?
C102 C103 1.405(3) . ?
C102 C117 1.399(3) . ?
C103 C104 1.463(2) . ?
C103 C120 1.398(3) . ?
C105 C106 1.435(2) . ?
C106 C107 1.415(3) . ?
C106 C121 1.406(3) . ?
C107 C108 1.443(2) . ?
C107 C124 1.407(3) . ?
C109 C110 1.470(2) . ?
C110 C111 1.397(3) . ?
C110 C125 1.392(3) . ?
C111 C112 1.467(3) . ?
C111 C128 1.403(3) . ?
C113 C114 1.438(3) . ?
C114 C115 1.418(3) . ?
C114 C129 1.409(3) . ?
C115 C116 1.441(2) . ?
C115 C132 1.410(3) . ?
C117 H117 0.9300 . ?
C117 C118 1.392(3) . ?
C118 H118 0.9300 . ?
C118 C119 1.409(3) . ?
C119 H119 0.9300 . ?
C119 C120 1.393(3) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.381(3) . ?
C122 H122 0.9300 . ?
C122 C123 1.418(3) . ?
C123 H123 0.9300 . ?
C123 C124 1.386(3) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.394(3) . ?
C126 H126 0.9300 . ?
C126 C127 1.401(3) . ?
C127 H127 0.9300 . ?
C127 C128 1.397(3) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.387(3) . ?
C130 H130 0.9300 . ?
C130 C131 1.416(3) . ?
C131 H131 0.9300 . ?
C131 C132 1.390(3) . ?
C132 H132 0.9300 . ?
N201 C201 1.464(3) . ?
N201 C203 1.465(3) . ?
N201 C205 1.470(3) . ?
N202 C202 1.505(3) . ?
N202 C204 1.506(3) . ?
N202 C206 1.511(3) . ?
N202 C207 1.495(3) . ?
C201 H20A 0.9700 . ?
C201 H20B 0.9700 . ?
C201 C202 1.546(3) . ?
C202 H20C 0.9700 . ?
C202 H20D 0.9700 . ?
C203 H20E 0.9700 . ?
C203 H20F 0.9700 . ?
C203 C204 1.538(3) . ?
C204 H20G 0.9700 . ?
C204 H20H 0.9700 . ?
C205 H20I 0.9700 . ?
C205 H20J 0.9700 . ?
C205 C206 1.539(3) . ?
C206 H20K 0.9700 . ?
C206 H20L 0.9700 . ?
C207 H20M 0.9600 . ?
C207 H20N 0.9600 . ?
C207 H20O 0.9600 . ?
N301 C301 1.461(3) . ?
N301 C303 1.469(3) . ?
N301 C305 1.459(3) . ?
N302 C302 1.510(2) . ?
N302 C304 1.521(2) . ?
N302 C306 1.511(3) . ?
N302 C307 1.491(3) . ?
C301 H30A 0.9700 . ?
C301 H30B 0.9700 . ?
C301 C302 1.540(3) . ?
C302 H30C 0.9700 . ?
C302 H30D 0.9700 . ?
C303 H30E 0.9700 . ?
C303 H30F 0.9700 . ?
C303 C304 1.539(3) . ?
C304 H30G 0.9700 . ?
C304 H30H 0.9700 . ?
C305 H30I 0.9700 . ?
C305 H30J 0.9700 . ?
C305 C306 1.535(4) . ?
C306 H30K 0.9700 . ?
C306 H30L 0.9700 . ?
C307 H30M 0.9600 . ?
C307 H30N 0.9600 . ?
C307 H30O 0.9600 . ?

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
O1 V1 N101 105.25(7) . . ?
O1 V1 N102 104.60(7) . . ?
O1 V1 N103 103.91(7) . . ?
O1 V1 N104 105.50(7) . . ?
N101 V1 N102 86.51(6) . . ?
N103 V1 N101 150.84(6) . . ?
N103 V1 N102 86.03(6) . . ?
N103 V1 N104 86.57(6) . . ?
N104 V1 N101 85.90(6) . . ?
N104 V1 N102 149.90(6) . . ?
C101 N101 V1 124.52(12) . . ?
C101 N101 C104 108.01(15) . . ?
C104 N101 V1 123.66(12) . . ?
C105 N102 V1 123.75(12) . . ?
C108 N102 V1 125.30(12) . . ?
C108 N102 C105 107.60(15) . . ?
C109 N103 V1 125.13(12) . . ?
C109 N103 C112 108.32(15) . . ?
C112 N103 V1 125.17(12) . . ?
C113 N104 V1 124.87(12) . . ?
C113 N104 C116 107.92(15) . . ?
C116 N104 V1 125.27(12) . . ?
C104 N105 C105 122.43(16) . . ?
C109 N106 C108 122.04(16) . . ?
C112 N107 C113 122.24(16) . . ?
C101 N108 C116 122.23(16) . . ?
N101 C101 C102 108.94(15) . . ?
N108 C101 N101 127.98(16) . . ?
N108 C101 C102 123.06(16) . . ?
C103 C102 C101 107.01(15) . . ?
C117 C102 C101 132.25(18) . . ?
C117 C102 C103 120.72(17) . . ?
C102 C103 C104 106.89(16) . . ?
C120 C103 C102 121.38(17) . . ?
C120 C103 C104 131.68(18) . . ?
N101 C104 C103 109.15(15) . . ?
N105 C104 N101 128.18(16) . . ?
N105 C104 C103 122.61(16) . . ?
N102 C105 C106 109.44(15) . . ?
N105 C105 N102 127.65(16) . . ?
N105 C105 C106 122.81(16) . . ?
C107 C106 C105 106.98(16) . . ?
C121 C106 C105 131.95(17) . . ?
C121 C106 C107 120.99(17) . . ?
C106 C107 C108 106.42(16) . . ?
C124 C107 C106 120.42(17) . . ?
C124 C107 C108 133.02(17) . . ?
N102 C108 C107 109.51(15) . . ?
N106 C108 N102 126.98(16) . . ?
N106 C108 C107 123.40(16) . . ?
N103 C109 C110 108.73(15) . . ?
N106 C109 N103 128.67(16) . . ?
N106 C109 C110 122.59(16) . . ?
C111 C110 C109 107.10(16) . . ?
C125 C110 C109 131.06(17) . . ?
C125 C110 C111 121.71(17) . . ?
C110 C111 C112 107.12(16) . . ?
C110 C111 C128 120.78(17) . . ?
C128 C111 C112 132.00(18) . . ?
N103 C112 C111 108.73(15) . . ?
N107 C112 N103 128.29(17) . . ?
N107 C112 C111 122.98(16) . . ?
N104 C113 C114 109.41(16) . . ?
N107 C113 N104 127.69(16) . . ?
N107 C113 C114 122.91(17) . . ?
C115 C114 C113 106.87(16) . . ?
C129 C114 C113 132.19(18) . . ?
C129 C114 C115 120.94(17) . . ?
C114 C115 C116 106.48(16) . . ?
C132 C115 C114 120.49(17) . . ?
C132 C115 C116 133.03(18) . . ?
N104 C116 C115 109.32(16) . . ?
N108 C116 N104 127.37(16) . . ?
N108 C116 C115 123.27(17) . . ?
C102 C117 H117 121.0 . . ?
C118 C117 C102 117.95(18) . . ?
C118 C117 H117 121.0 . . ?
C117 C118 H118 119.4 . . ?
C117 C118 C119 121.18(18) . . ?
C119 C118 H118 119.4 . . ?
C118 C119 H119 119.5 . . ?
C120 C119 C118 121.02(18) . . ?
C120 C119 H119 119.5 . . ?
C103 C120 H120 121.1 . . ?
C119 C120 C103 117.73(18) . . ?
C119 C120 H120 121.1 . . ?
C106 C121 H121 121.0 . . ?
C122 C121 C106 118.00(18) . . ?
C122 C121 H121 121.0 . . ?
C121 C122 H122 119.3 . . ?
C121 C122 C123 121.31(18) . . ?
C123 C122 H122 119.3 . . ?
C122 C123 H123 119.5 . . ?
C124 C123 C122 121.06(18) . . ?
C124 C123 H123 119.5 . . ?
C107 C124 H124 120.9 . . ?
C123 C124 C107 118.18(18) . . ?
C123 C124 H124 120.9 . . ?
C110 C125 H125 121.3 . . ?
C110 C125 C126 117.49(18) . . ?
C126 C125 H125 121.3 . . ?
C125 C126 H126 119.3 . . ?
C125 C126 C127 121.35(18) . . ?
C127 C126 H126 119.3 . . ?
C126 C127 H127 119.5 . . ?
C128 C127 C126 121.02(18) . . ?
C128 C127 H127 119.5 . . ?
C111 C128 H128 121.2 . . ?
C127 C128 C111 117.64(18) . . ?
C127 C128 H128 121.2 . . ?
C114 C129 H129 121.1 . . ?
C130 C129 C114 117.81(19) . . ?
C130 C129 H129 121.1 . . ?
C129 C130 H130 119.2 . . ?
C129 C130 C131 121.56(19) . . ?
C131 C130 H130 119.2 . . ?
C130 C131 H131 119.5 . . ?
C132 C131 C130 121.06(19) . . ?
C132 C131 H131 119.5 . . ?
C115 C132 H132 120.9 . . ?
C131 C132 C115 118.15(19) . . ?
C131 C132 H132 120.9 . . ?
C201 N201 C203 109.4(2) . . ?
C201 N201 C205 108.5(2) . . ?
C203 N201 C205 108.3(2) . . ?
C202 N202 C204 108.54(17) . . ?
C202 N202 C206 109.29(17) . . ?
C204 N202 C206 109.27(17) . . ?
C207 N202 C202 109.48(18) . . ?
C207 N202 C204 110.28(18) . . ?
C207 N202 C206 109.96(17) . . ?
N201 C201 H20A 109.3 . . ?
N201 C201 H20B 109.3 . . ?
N201 C201 C202 111.72(19) . . ?
H20A C201 H20B 107.9 . . ?
C202 C201 H20A 109.3 . . ?
C202 C201 H20B 109.3 . . ?
N202 C202 C201 108.23(18) . . ?
N202 C202 H20C 110.1 . . ?
N202 C202 H20D 110.1 . . ?
C201 C202 H20C 110.1 . . ?
C201 C202 H20D 110.1 . . ?
H20C C202 H20D 108.4 . . ?
N201 C203 H20E 109.3 . . ?
N201 C203 H20F 109.3 . . ?
N201 C203 C204 111.67(19) . . ?
H20E C203 H20F 107.9 . . ?
C204 C203 H20E 109.3 . . ?
C204 C203 H20F 109.3 . . ?
N202 C204 C203 108.54(17) . . ?
N202 C204 H20G 110.0 . . ?
N202 C204 H20H 110.0 . . ?
C203 C204 H20G 110.0 . . ?
C203 C204 H20H 110.0 . . ?
H20G C204 H20H 108.4 . . ?
N201 C205 H20I 109.3 . . ?
N201 C205 H20J 109.3 . . ?
N201 C205 C206 111.71(18) . . ?
H20I C205 H20J 107.9 . . ?
C206 C205 H20I 109.3 . . ?
C206 C205 H20J 109.3 . . ?
N202 C206 C205 108.34(18) . . ?
N202 C206 H20K 110.0 . . ?
N202 C206 H20L 110.0 . . ?
C205 C206 H20K 110.0 . . ?
C205 C206 H20L 110.0 . . ?
H20K C206 H20L 108.4 . . ?
N202 C207 H20M 109.5 . . ?
N202 C207 H20N 109.5 . . ?
N202 C207 H20O 109.5 . . ?
H20M C207 H20N 109.5 . . ?
H20M C207 H20O 109.5 . . ?
H20N C207 H20O 109.5 . . ?
C301 N301 C303 108.7(2) . . ?
C305 N301 C301 109.1(2) . . ?
C305 N301 C303 108.08(19) . . ?
C302 N302 C304 108.54(15) . . ?
C302 N302 C306 108.25(15) . . ?
C306 N302 C304 109.16(16) . . ?
C307 N302 C302 110.39(17) . . ?
C307 N302 C304 110.07(15) . . ?
C307 N302 C306 110.38(17) . . ?
N301 C301 H30A 109.1 . . ?
N301 C301 H30B 109.1 . . ?
N301 C301 C302 112.29(19) . . ?
H30A C301 H30B 107.9 . . ?
C302 C301 H30A 109.1 . . ?
C302 C301 H30B 109.1 . . ?
N302 C302 C301 108.03(18) . . ?
N302 C302 H30C 110.1 . . ?
N302 C302 H30D 110.1 . . ?
C301 C302 H30C 110.1 . . ?
C301 C302 H30D 110.1 . . ?
H30C C302 H30D 108.4 . . ?
N301 C303 H30E 109.4 . . ?
N301 C303 H30F 109.4 . . ?
N301 C303 C304 111.36(19) . . ?
H30E C303 H30F 108.0 . . ?
C304 C303 H30E 109.4 . . ?
C304 C303 H30F 109.4 . . ?
N302 C304 C303 108.67(16) . . ?
N302 C304 H30G 110.0 . . ?
N302 C304 H30H 110.0 . . ?
C303 C304 H30G 110.0 . . ?
C303 C304 H30H 110.0 . . ?
H30G C304 H30H 108.3 . . ?
N301 C305 H30I 109.2 . . ?
N301 C305 H30J 109.2 . . ?
N301 C305 C306 112.21(18) . . ?
H30I C305 H30J 107.9 . . ?
C306 C305 H30I 109.2 . . ?
C306 C305 H30J 109.2 . . ?
N302 C306 C305 108.43(18) . . ?
N302 C306 H30K 110.0 . . ?
N302 C306 H30L 110.0 . . ?
C305 C306 H30K 110.0 . . ?
C305 C306 H30L 110.0 . . ?
H30K C306 H30L 108.4 . . ?
N302 C307 H30M 109.5 . . ?
N302 C307 H30N 109.5 . . ?
N302 C307 H30O 109.5 . . ?
H30M C307 H30N 109.5 . . ?
H30M C307 H30O 109.5 . . ?
H30N C307 H30O 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.883
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane/do-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_diprimvopcc6h4cl2
_database_code_depnum_ccdc_archive 'CCDC 1581408'
_audit_update_record             
;
2017-12-04 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of vanadyl phthalocyanine radical anions with di(i_propyl)inidazolium cations'
_chemical_formula_moiety         'C32 H16 N8 O V, C9 H17 N2'
_chemical_formula_sum            'C41 H33 N10 O V'
_chemical_formula_weight         732.71
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   11.8705(5)
_cell_length_b                   31.689(2)
_cell_length_c                   23.8325(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8964.9(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    13059
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3940
_cell_measurement_theta_min      1.8840
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1251
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46582
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         1.709
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.89 200.89   0.50   80.00    --   28.00  73.42 -25.61  380
  2  ω     10.89 200.89   0.50   80.00    --   28.00  73.42 154.39  380
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5809
_reflns_number_total             8796
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8796
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1678
_refine_ls_R_factor_gt           0.1294
_refine_ls_restrained_S_all      1.040
_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)+(0.1714P)²+60.9685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3366
_refine_ls_wR_factor_ref         0.3624
_refine_special_details          
;The structure contains strongly disordered solvent: six molecules of 
dichlorobenzene were squeezed by standard Olex2 routine.,SQUEEZE
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 C120, C119, C118, C117, C102, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C27B) = Uanis(C27A)
4. Others
 Sof(H20J)=Sof(H20K)=Sof(H20L)=Sof(C27B)=Sof(H27B)=Sof(C29B)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(H20G)=Sof(H20H)=Sof(H20I)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C204(H204), C27A(H27A), C27B(H27B)
5.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C201(H201), C202(H202),
 C203(H203)
5.c Idealised Me refined as rotating group:
 C205(H20A,H20B,H20C), C206(H20D,H20E,H20F), C208(H20G,H20H,H20I), C208(H20J,
 H20K,H20L), C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V11 V 0.22789(9) 0.49092(4) 0.56096(5) 0.0276(3) Uani 1 1 d . . . . .
O11 O 0.1089(4) 0.49696(16) 0.52992(19) 0.0329(11) Uani 1 1 d . . . . .
N101 N 0.1910(4) 0.4605(2) 0.6328(2) 0.0310(14) Uani 1 1 d . . . . .
N102 N 0.2440(4) 0.54350(19) 0.6090(2) 0.0282(13) Uani 1 1 d . . . . .
N103 N 0.3405(4) 0.51851(19) 0.5081(2) 0.0282(13) Uani 1 1 d . . . . .
N104 N 0.2870(4) 0.4347(2) 0.5313(2) 0.0338(14) Uani 1 1 d . . . . .
N105 N 0.1537(5) 0.5194(2) 0.6946(2) 0.0379(16) Uani 1 1 d . . . . .
N106 N 0.3276(4) 0.5917(2) 0.5405(2) 0.0324(14) Uani 1 1 d . . . . .
N107 N 0.3951(4) 0.4582(2) 0.4507(2) 0.0307(14) Uani 1 1 d . . . . .
N108 N 0.2000(5) 0.3860(2) 0.5993(3) 0.0361(15) Uani 1 1 d . . . . .
N201 N 0.1670(5) 0.5185(2) 0.3624(2) 0.0396(16) Uani 1 1 d . . . . .
N202 N 0.1359(5) 0.5800(2) 0.3994(3) 0.0376(15) Uani 1 1 d . . . . .
C101 C 0.1704(6) 0.4168(3) 0.6356(3) 0.0369(18) Uani 1 1 d . . . . .
C102 C 0.1089(6) 0.4081(3) 0.6872(3) 0.0457(19) Uani 1 1 d . U . . .
C103 C 0.0967(6) 0.4475(3) 0.7151(3) 0.0382(17) Uani 1 1 d . U . . .
C104 C 0.1495(6) 0.4791(2) 0.6800(3) 0.0322(16) Uani 1 1 d . . . . .
C105 C 0.1972(5) 0.5493(3) 0.6621(3) 0.0327(17) Uani 1 1 d . . . . .
C106 C 0.1993(6) 0.5933(3) 0.6772(3) 0.0376(18) Uani 1 1 d . . . . .
C107 C 0.2531(6) 0.6150(2) 0.6308(3) 0.0346(18) Uani 1 1 d . . . . .
C108 C 0.2785(5) 0.5824(2) 0.5902(3) 0.0288(15) Uani 1 1 d . . . . .
C109 C 0.3562(5) 0.5611(2) 0.5050(3) 0.0258(15) Uani 1 1 d . . . . .
C110 C 0.4178(6) 0.5712(2) 0.4520(3) 0.0324(17) Uani 1 1 d . . . . .
C111 C 0.4417(5) 0.5322(2) 0.4271(3) 0.0294(16) Uani 1 1 d . . . . .
C112 C 0.3906(5) 0.4993(2) 0.4633(3) 0.0277(15) Uani 1 1 d . . . . .
C113 C 0.3495(5) 0.4291(2) 0.4831(3) 0.0297(16) Uani 1 1 d . . . . .
C114 C 0.3562(6) 0.3831(2) 0.4714(3) 0.0386(18) Uani 1 1 d . . . . .
C115 C 0.2978(6) 0.3623(3) 0.5155(3) 0.0405(19) Uani 1 1 d . . . . .
C116 C 0.2560(5) 0.3956(2) 0.5524(3) 0.0305(16) Uani 1 1 d . . . . .
C117 C 0.0611(7) 0.3687(3) 0.7096(4) 0.059(2) Uani 1 1 d . U . . .
H117 H 0.068558 0.342758 0.691807 0.071 Uiso 1 1 calc R . . . .
C118 C 0.0030(8) 0.3742(4) 0.7604(4) 0.074(3) Uani 1 1 d . U . . .
H118 H -0.033571 0.350979 0.775905 0.089 Uiso 1 1 calc R . . . .
C119 C -0.0026(8) 0.4135(4) 0.7894(4) 0.071(3) Uani 1 1 d . U . . .
H119 H -0.038022 0.414552 0.824207 0.085 Uiso 1 1 calc R . . . .
C120 C 0.0430(6) 0.4503(4) 0.7675(3) 0.054(2) Uani 1 1 d . U . . .
H120 H 0.038191 0.475788 0.786679 0.065 Uiso 1 1 calc R . . . .
C121 C 0.1612(7) 0.6155(3) 0.7229(3) 0.051(2) Uani 1 1 d . . . . .
H121 H 0.125102 0.601554 0.752155 0.061 Uiso 1 1 calc R . . . .
C122 C 0.1770(9) 0.6589(3) 0.7249(4) 0.062(3) Uani 1 1 d . . . . .
H122 H 0.152242 0.674085 0.755906 0.075 Uiso 1 1 calc R . . . .
C123 C 0.2292(8) 0.6795(3) 0.6812(5) 0.066(3) Uani 1 1 d . . . . .
H123 H 0.239999 0.708517 0.683725 0.079 Uiso 1 1 calc R . . . .
C124 C 0.2682(7) 0.6576(3) 0.6310(4) 0.046(2) Uani 1 1 d . . . . .
H124 H 0.301253 0.671749 0.601086 0.055 Uiso 1 1 calc R . . . .
C125 C 0.4534(6) 0.6087(3) 0.4269(3) 0.0379(18) Uani 1 1 d . . . . .
H125 H 0.439250 0.634611 0.443694 0.045 Uiso 1 1 calc R . . . .
C126 C 0.5096(6) 0.6062(3) 0.3769(3) 0.043(2) Uani 1 1 d . . . . .
H126 H 0.531944 0.630835 0.358755 0.052 Uiso 1 1 calc R . . . .
C127 C 0.5336(6) 0.5670(3) 0.3530(3) 0.048(2) Uani 1 1 d . . . . .
H127 H 0.572890 0.566540 0.319244 0.058 Uiso 1 1 calc R . . . .
C128 C 0.5025(6) 0.5287(3) 0.3764(3) 0.0410(19) Uani 1 1 d . . . . .
H128 H 0.520252 0.502851 0.360158 0.049 Uiso 1 1 calc R . . . .
C129 C 0.4086(6) 0.3626(3) 0.4281(4) 0.049(2) Uani 1 1 d . . . . .
H129 H 0.444422 0.377382 0.399463 0.058 Uiso 1 1 calc R . . . .
C130 C 0.4061(8) 0.3189(3) 0.4286(4) 0.056(2) Uani 1 1 d . . . . .
H130 H 0.442375 0.303449 0.400722 0.067 Uiso 1 1 calc R . . . .
C131 C 0.3448(8) 0.2972(3) 0.4742(5) 0.068(3) Uani 1 1 d . . . . .
H131 H 0.341515 0.267879 0.474981 0.082 Uiso 1 1 calc R . . . .
C132 C 0.2929(6) 0.3202(3) 0.5152(4) 0.048(2) Uani 1 1 d . . . . .
H132 H 0.253372 0.306237 0.543329 0.058 Uiso 1 1 calc R . . . .
C201 C 0.1197(6) 0.5401(3) 0.4055(3) 0.0392(18) Uani 1 1 d . . . . .
H201 H 0.081124 0.527809 0.435281 0.047 Uiso 1 1 calc R . . . .
C202 C 0.2130(7) 0.5481(4) 0.3274(3) 0.053(3) Uani 1 1 d . . . . .
H202 H 0.251693 0.542509 0.294339 0.064 Uiso 1 1 calc R . . . .
C203 C 0.1934(7) 0.5860(3) 0.3484(4) 0.047(2) Uani 1 1 d . . . . .
H203 H 0.213691 0.611676 0.332448 0.057 Uiso 1 1 calc R . . . .
C204 C 0.1761(6) 0.4728(3) 0.3552(3) 0.043(2) Uani 1 1 d . . . . .
H204 H 0.255304 0.464953 0.360298 0.051 Uiso 1 1 calc R . . . .
C205 C 0.1075(7) 0.4490(3) 0.3982(3) 0.045(2) Uani 1 1 d . . . . .
H20A H 0.138274 0.453711 0.434895 0.068 Uiso 1 1 calc GR . . . .
H20B H 0.109590 0.419333 0.389804 0.068 Uiso 1 1 calc GR . . . .
H20C H 0.030878 0.458667 0.397185 0.068 Uiso 1 1 calc GR . . . .
C206 C 0.1412(7) 0.4608(3) 0.2943(3) 0.053(2) Uani 1 1 d . . . . .
H20D H 0.067048 0.471392 0.286692 0.080 Uiso 1 1 calc GR . . . .
H20E H 0.141506 0.430625 0.290334 0.080 Uiso 1 1 calc GR . . . .
H20F H 0.193727 0.472908 0.268209 0.080 Uiso 1 1 calc GR . . . .
C208 C 0.0406(7) 0.5979(3) 0.4900(4) 0.048(2) Uani 1 1 d . . . . .
H20G H -0.014229 0.575825 0.486069 0.072 Uiso 0.538(12) 1 calc GR . P A 1
H20H H 0.009238 0.620533 0.511692 0.072 Uiso 0.538(12) 1 calc GR . P A 1
H20I H 0.106219 0.587036 0.508553 0.072 Uiso 0.538(12) 1 calc GR . P A 1
H20J H -0.025355 0.588005 0.470715 0.072 Uiso 0.462(12) 1 calc GR . P A 2
H20K H 0.019270 0.618537 0.517456 0.072 Uiso 0.462(12) 1 calc GR . P A 2
H20L H 0.077098 0.574609 0.508206 0.072 Uiso 0.462(12) 1 calc GR . P A 2
C27A C 0.0743(12) 0.6147(5) 0.4303(7) 0.034(3) Uani 0.538(12) 1 d . . P A 1
H27A H 0.009411 0.625444 0.409251 0.041 Uiso 0.538(12) 1 calc R . P A 1
C29A C 0.1617(11) 0.6484(4) 0.4408(7) 0.042(4) Uani 0.538(12) 1 d . . P A 1
H29A H 0.218735 0.637509 0.465453 0.063 Uiso 0.538(12) 1 calc GR . P A 1
H29B H 0.126520 0.672462 0.457889 0.063 Uiso 0.538(12) 1 calc GR . P A 1
H29C H 0.195355 0.656571 0.405881 0.063 Uiso 0.538(12) 1 calc GR . P A 1
C27B C 0.1232(15) 0.6183(6) 0.4468(8) 0.034(3) Uani 0.462(12) 1 d . . P A 2
H27B H 0.195844 0.625133 0.464134 0.041 Uiso 0.462(12) 1 calc R . P A 2
C29B C 0.0725(16) 0.6547(6) 0.4217(8) 0.051(5) Uani 0.462(12) 1 d . . P A 2
H29D H 0.125841 0.668051 0.397167 0.076 Uiso 0.462(12) 1 calc GR . P A 2
H29E H 0.050302 0.674140 0.450512 0.076 Uiso 0.462(12) 1 calc GR . P A 2
H29F H 0.007491 0.646247 0.400546 0.076 Uiso 0.462(12) 1 calc GR . P A 2


_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
V11 O11 1.606(5) . ?
V11 N101 2.013(5) . ?
V11 N102 2.031(6) . ?
V11 N103 2.035(6) . ?
V11 N104 2.041(6) . ?
N101 C101 1.407(10) . ?
N101 C104 1.363(9) . ?
N102 C105 1.395(8) . ?
N102 C108 1.374(9) . ?
N103 C109 1.365(9) . ?
N103 C112 1.364(8) . ?
N104 C113 1.378(8) . ?
N104 C116 1.389(9) . ?
N105 C104 1.324(10) . ?
N105 C105 1.329(10) . ?
N106 C108 1.353(9) . ?
N106 C109 1.330(9) . ?
N107 C112 1.338(9) . ?
N107 C113 1.319(9) . ?
N108 C101 1.350(10) . ?
N108 C116 1.337(9) . ?
N201 C201 1.357(10) . ?
N201 C202 1.369(10) . ?
N201 C204 1.461(11) . ?
N202 C201 1.288(10) . ?
N202 C203 1.407(10) . ?
N202 C27A 1.514(17) . ?
N202 C27B 1.67(2) . ?
C101 C102 1.456(10) . ?
C102 C103 1.424(12) . ?
C102 C117 1.470(12) . ?
C103 C104 1.446(10) . ?
C103 C120 1.404(10) . ?
C105 C106 1.440(11) . ?
C106 C107 1.450(11) . ?
C106 C121 1.372(11) . ?
C107 C108 1.446(9) . ?
C107 C124 1.361(12) . ?
C109 C110 1.493(9) . ?
C110 C111 1.401(11) . ?
C110 C125 1.395(11) . ?
C111 C112 1.483(10) . ?
C111 C128 1.411(9) . ?
C113 C114 1.486(11) . ?
C114 C115 1.421(11) . ?
C114 C129 1.370(11) . ?
C115 C116 1.458(11) . ?
C115 C132 1.338(12) . ?
C117 H117 0.9300 . ?
C117 C118 1.404(14) . ?
C118 H118 0.9300 . ?
C118 C119 1.428(16) . ?
C119 H119 0.9300 . ?
C119 C120 1.387(14) . ?
C120 H120 0.9300 . ?
C121 H121 0.9300 . ?
C121 C122 1.390(14) . ?
C122 H122 0.9300 . ?
C122 C123 1.377(15) . ?
C123 H123 0.9300 . ?
C123 C124 1.459(13) . ?
C124 H124 0.9300 . ?
C125 H125 0.9300 . ?
C125 C126 1.367(10) . ?
C126 H126 0.9300 . ?
C126 C127 1.398(12) . ?
C127 H127 0.9300 . ?
C127 C128 1.386(12) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C129 C130 1.385(13) . ?
C130 H130 0.9300 . ?
C130 C131 1.478(15) . ?
C131 H131 0.9300 . ?
C131 C132 1.365(13) . ?
C132 H132 0.9300 . ?
C201 H201 0.9300 . ?
C202 H202 0.9300 . ?
C202 C203 1.320(13) . ?
C203 H203 0.9300 . ?
C204 H204 0.9800 . ?
C204 C205 1.511(11) . ?
C204 C206 1.558(10) . ?
C205 H20A 0.9600 . ?
C205 H20B 0.9600 . ?
C205 H20C 0.9600 . ?
C206 H20D 0.9600 . ?
C206 H20E 0.9600 . ?
C206 H20F 0.9600 . ?
C208 H20G 0.9600 . ?
C208 H20H 0.9600 . ?
C208 H20I 0.9600 . ?
C208 H20J 0.9600 . ?
C208 H20K 0.9600 . ?
C208 H20L 0.9600 . ?
C208 C27A 1.570(17) . ?
C208 C27B 1.56(2) . ?
C27A H27A 0.9800 . ?
C27A C29A 1.508(19) . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C27B H27B 0.9800 . ?
C27B C29B 1.43(3) . ?
C29B H29D 0.9600 . ?
C29B H29E 0.9600 . ?
C29B H29F 0.9600 . ?

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
O11 V11 N101 104.9(2) . . ?
O11 V11 N102 104.2(2) . . ?
O11 V11 N103 104.0(2) . . ?
O11 V11 N104 104.3(2) . . ?
N101 V11 N102 86.3(2) . . ?
N101 V11 N103 151.1(2) . . ?
N101 V11 N104 87.2(2) . . ?
N102 V11 N103 86.3(2) . . ?
N102 V11 N104 151.5(2) . . ?
N103 V11 N104 86.2(2) . . ?
C101 N101 V11 123.4(5) . . ?
C104 N101 V11 124.9(5) . . ?
C104 N101 C101 108.9(6) . . ?
C105 N102 V11 125.7(5) . . ?
C108 N102 V11 125.5(4) . . ?
C108 N102 C105 107.2(6) . . ?
C109 N103 V11 123.3(4) . . ?
C112 N103 V11 125.3(5) . . ?
C112 N103 C109 109.9(6) . . ?
C113 N104 V11 125.9(5) . . ?
C113 N104 C116 109.2(6) . . ?
C116 N104 V11 124.2(5) . . ?
C104 N105 C105 123.4(6) . . ?
C109 N106 C108 120.6(6) . . ?
C113 N107 C112 122.1(6) . . ?
C116 N108 C101 120.2(6) . . ?
C201 N201 C202 106.2(7) . . ?
C201 N201 C204 128.2(7) . . ?
C202 N201 C204 125.4(7) . . ?
C201 N202 C203 107.6(7) . . ?
C201 N202 C27A 126.0(8) . . ?
C201 N202 C27B 128.7(8) . . ?
C203 N202 C27A 123.9(8) . . ?
C203 N202 C27B 122.2(9) . . ?
N101 C101 C102 108.3(7) . . ?
N108 C101 N101 129.4(6) . . ?
N108 C101 C102 122.3(7) . . ?
C101 C102 C117 131.4(9) . . ?
C103 C102 C101 106.2(7) . . ?
C103 C102 C117 122.4(8) . . ?
C102 C103 C104 107.1(6) . . ?
C120 C103 C102 121.1(8) . . ?
C120 C103 C104 131.9(8) . . ?
N101 C104 C103 109.5(7) . . ?
N105 C104 N101 128.4(6) . . ?
N105 C104 C103 122.1(7) . . ?
N102 C105 C106 110.4(6) . . ?
N105 C105 N102 126.1(7) . . ?
N105 C105 C106 123.5(6) . . ?
C105 C106 C107 105.9(6) . . ?
C121 C106 C105 133.5(8) . . ?
C121 C106 C107 120.6(8) . . ?
C108 C107 C106 105.3(7) . . ?
C124 C107 C106 121.6(7) . . ?
C124 C107 C108 133.1(8) . . ?
N102 C108 C107 111.1(6) . . ?
N106 C108 N102 127.5(6) . . ?
N106 C108 C107 121.4(7) . . ?
N103 C109 C110 108.9(6) . . ?
N106 C109 N103 130.6(6) . . ?
N106 C109 C110 120.5(6) . . ?
C111 C110 C109 105.6(6) . . ?
C125 C110 C109 133.9(7) . . ?
C125 C110 C111 120.5(6) . . ?
C110 C111 C112 106.9(6) . . ?
C110 C111 C128 122.4(7) . . ?
C128 C111 C112 130.7(7) . . ?
N103 C112 C111 108.6(6) . . ?
N107 C112 N103 128.9(6) . . ?
N107 C112 C111 122.5(6) . . ?
N104 C113 C114 108.1(6) . . ?
N107 C113 N104 128.2(7) . . ?
N107 C113 C114 123.6(6) . . ?
C115 C114 C113 106.8(6) . . ?
C129 C114 C113 129.1(8) . . ?
C129 C114 C115 124.0(8) . . ?
C114 C115 C116 106.1(7) . . ?
C132 C115 C114 118.7(8) . . ?
C132 C115 C116 135.3(8) . . ?
N104 C116 C115 109.7(6) . . ?
N108 C116 N104 129.6(7) . . ?
N108 C116 C115 120.7(7) . . ?
C102 C117 H117 123.2 . . ?
C118 C117 C102 113.5(10) . . ?
C118 C117 H117 123.2 . . ?
C117 C118 H118 118.4 . . ?
C117 C118 C119 123.2(9) . . ?
C119 C118 H118 118.4 . . ?
C118 C119 H119 118.9 . . ?
C120 C119 C118 122.2(8) . . ?
C120 C119 H119 118.9 . . ?
C103 C120 H120 121.3 . . ?
C119 C120 C103 117.4(10) . . ?
C119 C120 H120 121.3 . . ?
C106 C121 H121 120.3 . . ?
C106 C121 C122 119.3(9) . . ?
C122 C121 H121 120.3 . . ?
C121 C122 H122 119.9 . . ?
C123 C122 C121 120.3(8) . . ?
C123 C122 H122 119.9 . . ?
C122 C123 H123 118.8 . . ?
C122 C123 C124 122.4(9) . . ?
C124 C123 H123 118.8 . . ?
C107 C124 C123 115.8(9) . . ?
C107 C124 H124 122.1 . . ?
C123 C124 H124 122.1 . . ?
C110 C125 H125 120.9 . . ?
C126 C125 C110 118.3(8) . . ?
C126 C125 H125 120.9 . . ?
C125 C126 H126 119.8 . . ?
C125 C126 C127 120.3(8) . . ?
C127 C126 H126 119.8 . . ?
C126 C127 H127 117.9 . . ?
C128 C127 C126 124.1(7) . . ?
C128 C127 H127 117.9 . . ?
C111 C128 H128 122.8 . . ?
C127 C128 C111 114.3(8) . . ?
C127 C128 H128 122.8 . . ?
C114 C129 H129 121.4 . . ?
C114 C129 C130 117.2(9) . . ?
C130 C129 H129 121.4 . . ?
C129 C130 H130 120.6 . . ?
C129 C130 C131 118.8(8) . . ?
C131 C130 H130 120.6 . . ?
C130 C131 H131 120.0 . . ?
C132 C131 C130 120.1(9) . . ?
C132 C131 H131 120.0 . . ?
C115 C132 C131 121.2(9) . . ?
C115 C132 H132 119.4 . . ?
C131 C132 H132 119.4 . . ?
N201 C201 H201 124.8 . . ?
N202 C201 N201 110.4(7) . . ?
N202 C201 H201 124.8 . . ?
N201 C202 H202 125.5 . . ?
C203 C202 N201 108.9(8) . . ?
C203 C202 H202 125.5 . . ?
N202 C203 H203 126.6 . . ?
C202 C203 N202 106.8(7) . . ?
C202 C203 H203 126.6 . . ?
N201 C204 H204 107.9 . . ?
N201 C204 C205 112.1(6) . . ?
N201 C204 C206 109.3(7) . . ?
C205 C204 H204 107.9 . . ?
C205 C204 C206 111.5(7) . . ?
C206 C204 H204 107.9 . . ?
C204 C205 H20A 109.5 . . ?
C204 C205 H20B 109.5 . . ?
C204 C205 H20C 109.5 . . ?
H20A C205 H20B 109.5 . . ?
H20A C205 H20C 109.5 . . ?
H20B C205 H20C 109.5 . . ?
C204 C206 H20D 109.5 . . ?
C204 C206 H20E 109.5 . . ?
C204 C206 H20F 109.5 . . ?
H20D C206 H20E 109.5 . . ?
H20D C206 H20F 109.5 . . ?
H20E C206 H20F 109.5 . . ?
H20G C208 H20H 109.5 . . ?
H20G C208 H20I 109.5 . . ?
H20H C208 H20I 109.5 . . ?
H20J C208 H20K 109.5 . . ?
H20J C208 H20L 109.5 . . ?
H20K C208 H20L 109.5 . . ?
C27A C208 H20G 109.5 . . ?
C27A C208 H20H 109.5 . . ?
C27A C208 H20I 109.5 . . ?
C27B C208 H20J 109.5 . . ?
C27B C208 H20K 109.5 . . ?
C27B C208 H20L 109.5 . . ?
N202 C27A C208 108.5(10) . . ?
N202 C27A H27A 112.4 . . ?
C208 C27A H27A 112.4 . . ?
C29A C27A N202 105.3(11) . . ?
C29A C27A C208 105.4(12) . . ?
C29A C27A H27A 112.4 . . ?
C27A C29A H29A 109.5 . . ?
C27A C29A H29B 109.5 . . ?
C27A C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
N202 C27B H27B 111.6 . . ?
C208 C27B N202 101.7(11) . . ?
C208 C27B H27B 111.6 . . ?
C29B C27B N202 109.9(14) . . ?
C29B C27B C208 110.2(14) . . ?
C29B C27B H27B 111.6 . . ?
C27B C29B H29D 109.5 . . ?
C27B C29B H29E 109.5 . . ?
C27B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.558 0.250 -0.862 1417.2 257.2 ?
2 -0.198 0.750 -0.638 1417.2 257.3 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: o-dichlorobenzene/hexane'
_chemical_compound_source        no
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_TiOPcHexyl4NC6H4Cl2
_database_code_depnum_ccdc_archive 'CCDC 1583980'
_audit_update_record             
;
2017-11-04 deposited with the CCDC.
2017-12-13 downloaded from the CCDC.
;
_audit_creation_date             2017-10-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            no
_chemical_name_systematic        
'salt of titanyl phthalocyanine with tetrahexylammonium cations, o-dichlorobenzene solate'
_chemical_formula_moiety         'C24 H52 N, C32 H16 N8 O Ti, C6 H4 Cl2'
_chemical_formula_sum            'C62 H72 Cl2 N9 O Ti'
_chemical_formula_weight         1078.08
_chemical_absolute_configuration ?
_chemical_melting_point          'not measured'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# start Validation Reply Form
_vrf_PLAT112_I                   
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem. C 97 %Fit 
RESPONSE: Overall symmetry is closer to C c but local molecular 
arrangement within cation layers does not obey a centrosymmetric rule. 
It is probably due to the high mobility of hexyl chains which 
occupy different positions after nearly fast cooling of the sample 
before diffraction experiment.
;
# end Validation Reply Form

_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           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   23.2181(5)
_cell_length_b                   11.4301(2)
_cell_length_c                   21.4414(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.059(2)
_cell_angle_gamma                90
_cell_volume                     5658.44(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    39581
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3180
_cell_measurement_theta_min      1.8320
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.186
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.276
_diffrn_reflns_theta_min         1.782
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Bruker APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.89 200.89   1.00   80.00    --   28.00  73.42 -25.61  190
  2  ω     10.89 200.89   1.00   80.00    --   28.00  73.42  94.39  190
  3  ω     10.89 200.89   1.00   80.00    --   28.00  73.42 154.39  190
  4  ω     10.89 199.89   1.00   80.00    --   28.00  73.42-145.61  189
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                20292
_reflns_number_total             27307
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1360
_refine_ls_number_reflns         27307
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      1.026
_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)+(0.0587P)²+1.9883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1282
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.57(2)
 0.43(2)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C03V(H03A,H03B), C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C304(H30G,
 H30H), C305(H30I,H30J), C307(H30N,H30O), C308(H30P,H30Q), C309(H30R,H30S),
 C310(H31A,H31B), C312(H31F,H31G), C313(H31H,H31I), C314(H31J,H31K), C315(H31L,
 H31M), C316(H31N,H31O), C318(H31S,H31T), C319(H31U,H31V), C320(H32A,H32B),
 C321(H32C,H32D), C322(H32E,H32F), C401(H40A,H40B), C402(H40C,H40D), C403(H40E,
 H40F), C404(H40G,H40H), C405(H40I,H40J), C407(H40N,H40O), C408(H40P,H40Q),
 C409(H40R,H40S), C410(H41A,H41B), C411(H41C,H41D), C413(H41H,H41I), C414(H41J,
 H41K), C415(H41L,H41M), C416(H41N,H41O), C417(H41P,H41Q), C419(H41U,H41V),
 C420(H42A,H42B), C421(H42C,H42D), C422(H42E,H42F), C423(H42G,H42H)
3.b Aromatic/amide H refined with riding coordinates:
 C117(H117), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C132(H132), C217(H217), C218(H218),
 C219(H219), C220(H220), C221(H221), C222(H222), C223(H223), C224(H224),
 C225(H225), C226(H226), C227(H227), C228(H228), C229(H229), C230(H230),
 C231(H231), C232(H232), C63(H63), C64(H64), C65(H65), C66(H66), C53(H53),
 C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C306(H30K,H30L,H30M), C311(H31C,H31D,H31E), C317(H31P,H31Q,H31R), C323(H32G,
 H32H,H32I), C406(H40K,H40L,H40M), C412(H41E,H41F,H41G), C418(H41R,H41S,H41T),
 C424(H42I,H42J,H42K)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
N301 N 0.74322(16) 0.7367(3) 0.47624(17) 0.0247(8) Uani 1 1 d . . . . .
C03V C 0.70009(19) 0.8073(4) 0.4326(2) 0.0255(9) Uani 1 1 d . . . . .
H03A H 0.664370 0.818261 0.453370 0.031 Uiso 1 1 calc R . . . .
H03B H 0.716766 0.885698 0.426626 0.031 Uiso 1 1 calc R . . . .
C301 C 0.72022(19) 0.6140(4) 0.4869(2) 0.0271(10) Uani 1 1 d . . . . .
H30A H 0.748270 0.573897 0.517741 0.032 Uiso 1 1 calc R . . . .
H30B H 0.719330 0.570301 0.446951 0.032 Uiso 1 1 calc R . . . .
C302 C 0.6602(2) 0.6049(4) 0.5100(2) 0.0357(11) Uani 1 1 d . . . . .
H30C H 0.632528 0.655631 0.484236 0.043 Uiso 1 1 calc R . . . .
H30D H 0.662070 0.631650 0.554117 0.043 Uiso 1 1 calc R . . . .
C303 C 0.6395(2) 0.4776(4) 0.5053(2) 0.0356(12) Uani 1 1 d . . . . .
H30E H 0.642684 0.448511 0.462302 0.043 Uiso 1 1 calc R . . . .
H30F H 0.665105 0.429042 0.534700 0.043 Uiso 1 1 calc R . . . .
C304 C 0.5769(2) 0.4631(4) 0.5203(2) 0.0359(11) Uani 1 1 d . . . . .
H30G H 0.575113 0.479522 0.565373 0.043 Uiso 1 1 calc R . . . .
H30H H 0.552347 0.521519 0.495983 0.043 Uiso 1 1 calc R . . . .
C305 C 0.5525(2) 0.3414(4) 0.5054(2) 0.0342(11) Uani 1 1 d . . . . .
H30I H 0.557854 0.321495 0.461445 0.041 Uiso 1 1 calc R . . . .
H30J H 0.574391 0.283612 0.532947 0.041 Uiso 1 1 calc R . . . .
C306 C 0.4891(2) 0.3326(5) 0.5143(2) 0.0417(13) Uani 1 1 d . . . . .
H30K H 0.467646 0.394118 0.489892 0.063 Uiso 1 1 calc GR . . . .
H30L H 0.484090 0.342178 0.558783 0.063 Uiso 1 1 calc GR . . . .
H30M H 0.474348 0.255836 0.499858 0.063 Uiso 1 1 calc GR . . . .
C307 C 0.6837(2) 0.7528(4) 0.3684(2) 0.0290(10) Uani 1 1 d . . . . .
H30N H 0.679897 0.666978 0.372830 0.035 Uiso 1 1 calc R . . . .
H30O H 0.714692 0.768103 0.341071 0.035 Uiso 1 1 calc R . . . .
C308 C 0.62652(18) 0.8034(4) 0.3380(2) 0.0241(9) Uani 1 1 d . . . . .
H30P H 0.630648 0.889049 0.333193 0.029 Uiso 1 1 calc R . . . .
H30Q H 0.595827 0.789303 0.365857 0.029 Uiso 1 1 calc R . . . .
C309 C 0.60841(18) 0.7488(4) 0.2737(2) 0.0257(9) Uani 1 1 d . . . . .
H30R H 0.638507 0.765713 0.245528 0.031 Uiso 1 1 calc R . . . .
H30S H 0.606153 0.662769 0.278440 0.031 Uiso 1 1 calc R . . . .
C310 C 0.5501(2) 0.7940(5) 0.2435(2) 0.0349(11) Uani 1 1 d . . . . .
H31A H 0.520105 0.779039 0.272039 0.042 Uiso 1 1 calc R . . . .
H31B H 0.552622 0.879644 0.237399 0.042 Uiso 1 1 calc R . . . .
C311 C 0.5321(2) 0.7359(5) 0.1804(2) 0.0441(13) Uani 1 1 d . . . . .
H31C H 0.560000 0.756100 0.150877 0.066 Uiso 1 1 calc GR . . . .
H31D H 0.493516 0.763484 0.164017 0.066 Uiso 1 1 calc GR . . . .
H31E H 0.531309 0.650839 0.185906 0.066 Uiso 1 1 calc GR . . . .
C312 C 0.79993(18) 0.7202(4) 0.4478(2) 0.0257(9) Uani 1 1 d . . . . .
H31F H 0.791734 0.675411 0.408296 0.031 Uiso 1 1 calc R . . . .
H31G H 0.825830 0.671528 0.476848 0.031 Uiso 1 1 calc R . . . .
C313 C 0.8327(2) 0.8310(4) 0.4334(2) 0.0338(11) Uani 1 1 d . . . . .
H31H H 0.844359 0.873745 0.472857 0.041 Uiso 1 1 calc R . . . .
H31I H 0.806982 0.882634 0.405762 0.041 Uiso 1 1 calc R . . . .
C314 C 0.8864(2) 0.8004(4) 0.4012(3) 0.0368(12) Uani 1 1 d . . . . .
H31J H 0.911761 0.748466 0.429035 0.044 Uiso 1 1 calc R . . . .
H31K H 0.874400 0.756855 0.362081 0.044 Uiso 1 1 calc R . . . .
C315 C 0.9208(2) 0.9080(4) 0.3855(2) 0.0365(11) Uani 1 1 d . . . . .
H31L H 0.895987 0.957086 0.355562 0.044 Uiso 1 1 calc R . . . .
H31M H 0.930097 0.954291 0.424259 0.044 Uiso 1 1 calc R . . . .
C316 C 0.9766(2) 0.8817(5) 0.3574(3) 0.0430(13) Uani 1 1 d . . . . .
H31N H 1.000276 0.828077 0.385964 0.052 Uiso 1 1 calc R . . . .
H31O H 0.967120 0.840388 0.317109 0.052 Uiso 1 1 calc R . . . .
C317 C 1.0126(2) 0.9882(5) 0.3460(3) 0.0487(15) Uani 1 1 d . . . . .
H31P H 0.990675 1.039688 0.315649 0.073 Uiso 1 1 calc GR . . . .
H31Q H 1.048484 0.963623 0.329426 0.073 Uiso 1 1 calc GR . . . .
H31R H 1.022129 1.030371 0.385568 0.073 Uiso 1 1 calc GR . . . .
C318 C 0.7524(2) 0.8043(4) 0.5381(2) 0.0281(10) Uani 1 1 d . . . . .
H31S H 0.765487 0.884350 0.528982 0.034 Uiso 1 1 calc R . . . .
H31T H 0.714471 0.811628 0.555033 0.034 Uiso 1 1 calc R . . . .
C319 C 0.7954(2) 0.7519(5) 0.5888(2) 0.0357(12) Uani 1 1 d . . . . .
H31U H 0.835226 0.761492 0.577147 0.043 Uiso 1 1 calc R . . . .
H31V H 0.787667 0.667158 0.592785 0.043 Uiso 1 1 calc R . . . .
C320 C 0.78980(19) 0.8131(4) 0.6515(2) 0.0287(10) Uani 1 1 d . . . . .
H32A H 0.749885 0.802291 0.662746 0.034 Uiso 1 1 calc R . . . .
H32B H 0.796284 0.898006 0.646479 0.034 Uiso 1 1 calc R . . . .
C321 C 0.8327(2) 0.7668(4) 0.7050(2) 0.0308(10) Uani 1 1 d . . . . .
H32C H 0.827968 0.680970 0.708202 0.037 Uiso 1 1 calc R . . . .
H32D H 0.872669 0.782161 0.694956 0.037 Uiso 1 1 calc R . . . .
C322 C 0.82484(19) 0.8218(4) 0.7681(2) 0.0292(10) Uani 1 1 d . . . . .
H32E H 0.785394 0.803962 0.779016 0.035 Uiso 1 1 calc R . . . .
H32F H 0.828224 0.907864 0.764626 0.035 Uiso 1 1 calc R . . . .
C323 C 0.86915(19) 0.7784(4) 0.8208(2) 0.0330(11) Uani 1 1 d . . . . .
H32G H 0.908125 0.801550 0.812030 0.049 Uiso 1 1 calc GR . . . .
H32H H 0.867036 0.692961 0.823528 0.049 Uiso 1 1 calc GR . . . .
H32I H 0.860698 0.812896 0.860703 0.049 Uiso 1 1 calc GR . . . .
N401 N 0.23642(16) 0.2378(3) 0.45186(16) 0.0237(8) Uani 1 1 d . . . . .
C401 C 0.2493(2) 0.3058(4) 0.5131(2) 0.0268(10) Uani 1 1 d . . . . .
H40A H 0.262377 0.385409 0.503152 0.032 Uiso 1 1 calc R . . . .
H40B H 0.212861 0.313924 0.532945 0.032 Uiso 1 1 calc R . . . .
C402 C 0.2949(2) 0.2498(4) 0.5602(2) 0.0342(12) Uani 1 1 d . . . . .
H40C H 0.333646 0.259541 0.545472 0.041 Uiso 1 1 calc R . . . .
H40D H 0.287074 0.164974 0.563117 0.041 Uiso 1 1 calc R . . . .
C403 C 0.2947(2) 0.3057(4) 0.6251(2) 0.0268(10) Uani 1 1 d . . . . .
H40E H 0.303163 0.390323 0.622039 0.032 Uiso 1 1 calc R . . . .
H40F H 0.255625 0.297630 0.639112 0.032 Uiso 1 1 calc R . . . .
C404 C 0.3390(2) 0.2505(4) 0.6740(2) 0.0290(10) Uani 1 1 d . . . . .
H40G H 0.332204 0.165086 0.674913 0.035 Uiso 1 1 calc R . . . .
H40H H 0.378302 0.263395 0.661374 0.035 Uiso 1 1 calc R . . . .
C405 C 0.3364(2) 0.2997(4) 0.7395(2) 0.0305(10) Uani 1 1 d . . . . .
H40I H 0.297248 0.286324 0.752312 0.037 Uiso 1 1 calc R . . . .
H40J H 0.343003 0.385239 0.738590 0.037 Uiso 1 1 calc R . . . .
C406 C 0.3813(2) 0.2445(5) 0.7882(2) 0.0343(11) Uani 1 1 d . . . . .
H40K H 0.420315 0.261713 0.777230 0.052 Uiso 1 1 calc GR . . . .
H40L H 0.375513 0.159543 0.788750 0.052 Uiso 1 1 calc GR . . . .
H40M H 0.376707 0.276734 0.829706 0.052 Uiso 1 1 calc GR . . . .
C407 C 0.21429(19) 0.1152(4) 0.4641(2) 0.0249(9) Uani 1 1 d . . . . .
H40N H 0.245718 0.071771 0.488959 0.030 Uiso 1 1 calc R . . . .
H40O H 0.206490 0.074688 0.423284 0.030 Uiso 1 1 calc R . . . .
C408 C 0.1598(2) 0.1067(4) 0.4983(2) 0.0337(11) Uani 1 1 d . . . . .
H40P H 0.167498 0.140830 0.540793 0.040 Uiso 1 1 calc R . . . .
H40Q H 0.127951 0.151598 0.475051 0.040 Uiso 1 1 calc R . . . .
C409 C 0.1419(2) -0.0208(4) 0.5033(2) 0.0290(10) Uani 1 1 d . . . . .
H40R H 0.172590 -0.063890 0.529417 0.035 Uiso 1 1 calc R . . . .
H40S H 0.137794 -0.056473 0.460956 0.035 Uiso 1 1 calc R . . . .
C410 C 0.0842(2) -0.0330(4) 0.5324(2) 0.0334(11) Uani 1 1 d . . . . .
H41A H 0.089673 -0.003050 0.575932 0.040 Uiso 1 1 calc R . . . .
H41B H 0.054772 0.016853 0.508470 0.040 Uiso 1 1 calc R . . . .
C411 C 0.0612(2) -0.1574(4) 0.5333(3) 0.0463(14) Uani 1 1 d . . . . .
H41C H 0.088599 -0.206602 0.560388 0.056 Uiso 1 1 calc R . . . .
H41D H 0.057970 -0.190233 0.490390 0.056 Uiso 1 1 calc R . . . .
C412 C 0.0019(3) -0.1601(5) 0.5580(4) 0.0590(18) Uani 1 1 d . . . . .
H41E H -0.025325 -0.111726 0.531127 0.089 Uiso 1 1 calc GR . . . .
H41F H 0.005240 -0.129337 0.600949 0.089 Uiso 1 1 calc GR . . . .
H41G H -0.012327 -0.240797 0.557923 0.089 Uiso 1 1 calc GR . . . .
C413 C 0.19099(19) 0.3073(4) 0.41023(19) 0.0232(9) Uani 1 1 d . . . . .
H41H H 0.155399 0.312633 0.431752 0.028 Uiso 1 1 calc R . . . .
H41I H 0.205639 0.387908 0.405703 0.028 Uiso 1 1 calc R . . . .
C414 C 0.1751(2) 0.2566(4) 0.3452(2) 0.0274(10) Uani 1 1 d . . . . .
H41J H 0.168684 0.171317 0.348646 0.033 Uiso 1 1 calc R . . . .
H41K H 0.207676 0.268642 0.319553 0.033 Uiso 1 1 calc R . . . .
C415 C 0.12022(19) 0.3142(4) 0.3124(2) 0.0284(10) Uani 1 1 d . . . . .
H41L H 0.124836 0.400333 0.313388 0.034 Uiso 1 1 calc R . . . .
H41M H 0.086616 0.294091 0.335197 0.034 Uiso 1 1 calc R . . . .
C416 C 0.1089(2) 0.2726(4) 0.2440(2) 0.0304(10) Uani 1 1 d . . . . .
H41N H 0.142752 0.292982 0.221715 0.037 Uiso 1 1 calc R . . . .
H41O H 0.105033 0.186386 0.243546 0.037 Uiso 1 1 calc R . . . .
C417 C 0.0544(2) 0.3263(5) 0.2087(2) 0.0367(12) Uani 1 1 d . . . . .
H41P H 0.054207 0.411569 0.216778 0.044 Uiso 1 1 calc R . . . .
H41Q H 0.055602 0.314688 0.163118 0.044 Uiso 1 1 calc R . . . .
C418 C -0.0008(2) 0.2739(5) 0.2275(3) 0.0417(13) Uani 1 1 d . . . . .
H41R H -0.034128 0.310512 0.203220 0.063 Uiso 1 1 calc GR . . . .
H41S H -0.003026 0.287595 0.272348 0.063 Uiso 1 1 calc GR . . . .
H41T H -0.001140 0.189564 0.219313 0.063 Uiso 1 1 calc GR . . . .
C419 C 0.29113(18) 0.2223(4) 0.41945(19) 0.0227(9) Uani 1 1 d . . . . .
H41U H 0.318982 0.175274 0.447187 0.027 Uiso 1 1 calc R . . . .
H41V H 0.281136 0.176571 0.380617 0.027 Uiso 1 1 calc R . . . .
C420 C 0.32127(19) 0.3334(4) 0.4023(2) 0.0280(10) Uani 1 1 d . . . . .
H42A H 0.333833 0.378099 0.440919 0.034 Uiso 1 1 calc R . . . .
H42B H 0.293762 0.382703 0.375391 0.034 Uiso 1 1 calc R . . . .
C421 C 0.3741(2) 0.3061(4) 0.3675(2) 0.0263(9) Uani 1 1 d . . . . .
H42C H 0.399928 0.251678 0.393148 0.032 Uiso 1 1 calc R . . . .
H42D H 0.360960 0.266412 0.327470 0.032 Uiso 1 1 calc R . . . .
C422 C 0.40792(19) 0.4156(4) 0.3539(2) 0.0273(10) Uani 1 1 d . . . . .
H42E H 0.415062 0.462108 0.392863 0.033 Uiso 1 1 calc R . . . .
H42F H 0.384057 0.463724 0.322646 0.033 Uiso 1 1 calc R . . . .
C423 C 0.4659(2) 0.3896(4) 0.3291(2) 0.0332(11) Uani 1 1 d . . . . .
H42G H 0.487931 0.334584 0.358201 0.040 Uiso 1 1 calc R . . . .
H42H H 0.458350 0.349959 0.287961 0.040 Uiso 1 1 calc R . . . .
C424 C 0.5032(2) 0.4971(5) 0.3212(3) 0.0461(14) Uani 1 1 d . . . . .
H42I H 0.482464 0.551048 0.291235 0.069 Uiso 1 1 calc GR . . . .
H42J H 0.539593 0.473102 0.305501 0.069 Uiso 1 1 calc GR . . . .
H42K H 0.511722 0.536268 0.361781 0.069 Uiso 1 1 calc GR . . . .
Ti01 Ti 0.72829(3) 0.19194(6) 0.45889(3) 0.01172(14) Uani 1 1 d . . . . .
O007 O 0.76685(12) 0.0804(2) 0.43754(12) 0.0196(6) Uani 1 1 d . . . . .
N101 N 0.72424(13) 0.3181(3) 0.38921(14) 0.0139(6) Uani 1 1 d . . . . .
N102 N 0.78376(13) 0.3088(3) 0.50927(14) 0.0147(6) Uani 1 1 d . . . . .
N103 N 0.70260(13) 0.1486(3) 0.54551(14) 0.0157(7) Uani 1 1 d . . . . .
N104 N 0.64341(13) 0.1569(3) 0.42543(14) 0.0149(7) Uani 1 1 d . . . . .
N105 N 0.81224(14) 0.4284(3) 0.42326(14) 0.0148(7) Uani 1 1 d . . . . .
N106 N 0.78203(14) 0.2310(3) 0.61573(14) 0.0172(7) Uani 1 1 d . . . . .
N107 N 0.61507(14) 0.0370(3) 0.51203(14) 0.0168(7) Uani 1 1 d . . . . .
N108 N 0.63539(14) 0.2609(3) 0.32497(14) 0.0149(7) Uani 1 1 d . . . . .
C101 C 0.68425(17) 0.3218(3) 0.33581(16) 0.0148(8) Uani 1 1 d . . . . .
C102 C 0.70399(17) 0.4063(3) 0.29210(17) 0.0160(8) Uani 1 1 d . . . . .
C103 C 0.75616(17) 0.4534(3) 0.32056(17) 0.0158(8) Uani 1 1 d . . . . .
C104 C 0.76772(16) 0.3983(3) 0.38175(17) 0.0152(8) Uani 1 1 d . . . . .
C105 C 0.81880(16) 0.3886(3) 0.48215(17) 0.0153(8) Uani 1 1 d . . . . .
C106 C 0.86364(16) 0.4289(3) 0.52992(17) 0.0158(8) Uani 1 1 d . . . . .
C107 C 0.85396(17) 0.3727(3) 0.58645(17) 0.0169(8) Uani 1 1 d . . . . .
C108 C 0.80357(16) 0.2984(3) 0.57273(17) 0.0152(8) Uani 1 1 d . . . . .
C109 C 0.73581(17) 0.1639(3) 0.60335(17) 0.0169(8) Uani 1 1 d . . . . .
C110 C 0.71145(17) 0.0917(3) 0.65001(17) 0.0169(8) Uani 1 1 d . . . . .
C111 C 0.66294(17) 0.0347(4) 0.61923(17) 0.0181(8) Uani 1 1 d . . . . .
C112 C 0.65774(16) 0.0718(3) 0.55382(17) 0.0155(8) Uani 1 1 d . . . . .
C113 C 0.60767(16) 0.0803(3) 0.45360(17) 0.0147(8) Uani 1 1 d . . . . .
C114 C 0.55679(17) 0.0563(3) 0.41026(17) 0.0166(8) Uani 1 1 d . . . . .
C115 C 0.56254(16) 0.1211(3) 0.35530(17) 0.0148(8) Uani 1 1 d . . . . .
C116 C 0.61660(16) 0.1853(3) 0.36582(17) 0.0156(8) Uani 1 1 d . . . . .
C117 C 0.68003(18) 0.4438(4) 0.23264(19) 0.0223(9) Uani 1 1 d . . . . .
H117 H 0.644699 0.412235 0.213319 0.027 Uiso 1 1 calc R . . . .
C118 C 0.7102(2) 0.5290(4) 0.20324(19) 0.0262(10) Uani 1 1 d . . . . .
H118 H 0.695016 0.556240 0.162973 0.031 Uiso 1 1 calc R . . . .
C119 C 0.76234(19) 0.5760(4) 0.23115(19) 0.0230(9) Uani 1 1 d . . . . .
H119 H 0.781700 0.634189 0.209569 0.028 Uiso 1 1 calc R . . . .
C120 C 0.78617(17) 0.5388(3) 0.28990(18) 0.0188(8) Uani 1 1 d . . . . .
H120 H 0.821700 0.570189 0.308757 0.023 Uiso 1 1 calc R . . . .
C121 C 0.91079(17) 0.5048(4) 0.52699(19) 0.0201(9) Uani 1 1 d . . . . .
H121 H 0.916713 0.544685 0.489326 0.024 Uiso 1 1 calc R . . . .
C122 C 0.94868(19) 0.5196(4) 0.5815(2) 0.0240(9) Uani 1 1 d . . . . .
H122 H 0.981513 0.568951 0.580773 0.029 Uiso 1 1 calc R . . . .
C123 C 0.93870(18) 0.4614(4) 0.63814(19) 0.0238(9) Uani 1 1 d . . . . .
H123 H 0.965120 0.472663 0.674590 0.029 Uiso 1 1 calc R . . . .
C124 C 0.89174(18) 0.3896(4) 0.64115(18) 0.0201(8) Uani 1 1 d . . . . .
H124 H 0.885000 0.352258 0.679299 0.024 Uiso 1 1 calc R . . . .
C125 C 0.72880(18) 0.0727(4) 0.71402(17) 0.0201(9) Uani 1 1 d . . . . .
H125 H 0.761180 0.112143 0.735176 0.024 Uiso 1 1 calc R . . . .
C126 C 0.69626(19) -0.0068(4) 0.74499(18) 0.0239(9) Uani 1 1 d . . . . .
H126 H 0.707029 -0.022328 0.788176 0.029 Uiso 1 1 calc R . . . .
C127 C 0.64815(19) -0.0645(4) 0.7143(2) 0.0259(10) Uani 1 1 d . . . . .
H127 H 0.627221 -0.118419 0.736949 0.031 Uiso 1 1 calc R . . . .
C128 C 0.63052(18) -0.0445(4) 0.65153(19) 0.0225(9) Uani 1 1 d . . . . .
H128 H 0.597578 -0.083018 0.630941 0.027 Uiso 1 1 calc R . . . .
C129 C 0.50781(17) -0.0106(4) 0.41680(19) 0.0205(9) Uani 1 1 d . . . . .
H129 H 0.504299 -0.053280 0.454243 0.025 Uiso 1 1 calc R . . . .
C130 C 0.46408(18) -0.0138(4) 0.36727(19) 0.0242(9) Uani 1 1 d . . . . .
H130 H 0.429932 -0.057848 0.371048 0.029 Uiso 1 1 calc R . . . .
C131 C 0.47013(18) 0.0483(4) 0.31132(18) 0.0216(9) Uani 1 1 d . . . . .
H131 H 0.440277 0.043270 0.277530 0.026 Uiso 1 1 calc R . . . .
C132 C 0.51852(17) 0.1162(4) 0.30451(18) 0.0190(8) Uani 1 1 d . . . . .
H132 H 0.521993 0.158210 0.266854 0.023 Uiso 1 1 calc R . . . .
Ti02 Ti 0.23164(3) 0.69069(6) 0.45997(3) 0.01217(14) Uani 1 1 d . . . . .
O008 O 0.26871(12) 0.5788(2) 0.43652(12) 0.0202(6) Uani 1 1 d . . . . .
N201 N 0.20998(14) 0.6458(3) 0.54805(14) 0.0157(7) Uani 1 1 d . . . . .
N202 N 0.14604(14) 0.6560(3) 0.43015(14) 0.0151(7) Uani 1 1 d . . . . .
N203 N 0.22550(13) 0.8162(3) 0.39012(14) 0.0144(6) Uani 1 1 d . . . . .
N204 N 0.28858(13) 0.8072(3) 0.50817(13) 0.0146(6) Uani 1 1 d . . . . .
N205 N 0.12209(14) 0.5326(3) 0.51738(15) 0.0178(7) Uani 1 1 d . . . . .
N206 N 0.13493(14) 0.7575(3) 0.32924(14) 0.0153(7) Uani 1 1 d . . . . .
N207 N 0.31436(13) 0.9259(3) 0.41997(15) 0.0152(7) Uani 1 1 d . . . . .
N208 N 0.29103(14) 0.7297(3) 0.61502(14) 0.0167(7) Uani 1 1 d . . . . .
C00V C 0.11235(16) 0.5765(3) 0.45926(17) 0.0168(8) Uani 1 1 d . . . . .
C201 C 0.24522(17) 0.6603(3) 0.60421(17) 0.0159(8) Uani 1 1 d . . . . .
C202 C 0.22419(17) 0.5848(4) 0.65154(18) 0.0190(8) Uani 1 1 d . . . . .
C203 C 0.17497(17) 0.5271(4) 0.62298(18) 0.0185(8) Uani 1 1 d . . . . .
C204 C 0.16647(17) 0.5669(4) 0.55797(17) 0.0182(8) Uani 1 1 d . . . . .
C206 C 0.06092(17) 0.5494(4) 0.41715(17) 0.0184(8) Uani 1 1 d . . . . .
C207 C 0.06458(17) 0.6155(3) 0.36205(17) 0.0166(8) Uani 1 1 d . . . . .
C208 C 0.11750(16) 0.6819(3) 0.37114(16) 0.0144(8) Uani 1 1 d . . . . .
C209 C 0.18392(17) 0.8187(3) 0.33798(16) 0.0155(8) Uani 1 1 d . . . . .
C210 C 0.20290(17) 0.8996(3) 0.29190(17) 0.0164(8) Uani 1 1 d . . . . .
C211 C 0.25685(16) 0.9454(3) 0.31768(17) 0.0153(8) Uani 1 1 d . . . . .
C212 C 0.26942(16) 0.8933(3) 0.37959(17) 0.0146(8) Uani 1 1 d . . . . .
C213 C 0.32157(16) 0.8889(3) 0.47969(17) 0.0147(8) Uani 1 1 d . . . . .
C214 C 0.36638(16) 0.9343(3) 0.52624(17) 0.0161(8) Uani 1 1 d . . . . .
C215 C 0.35941(16) 0.8764(3) 0.58324(17) 0.0167(8) Uani 1 1 d . . . . .
C216 C 0.31035(16) 0.7986(3) 0.57093(17) 0.0153(8) Uani 1 1 d . . . . .
C217 C 0.24475(18) 0.5647(4) 0.71482(18) 0.0221(9) Uani 1 1 d . . . . .
H217 H 0.277615 0.604614 0.734630 0.027 Uiso 1 1 calc R . . . .
C218 C 0.2142(2) 0.4828(4) 0.74693(19) 0.0276(10) Uani 1 1 d . . . . .
H218 H 0.227234 0.465407 0.789407 0.033 Uiso 1 1 calc R . . . .
C219 C 0.1650(2) 0.4257(4) 0.7185(2) 0.0270(10) Uani 1 1 d . . . . .
H219 H 0.145230 0.371630 0.742250 0.032 Uiso 1 1 calc R . . . .
C220 C 0.14443(19) 0.4465(4) 0.65589(19) 0.0237(9) Uani 1 1 d . . . . .
H220 H 0.111085 0.407528 0.636510 0.028 Uiso 1 1 calc R . . . .
C221 C 0.01376(18) 0.4773(4) 0.42417(18) 0.0231(9) Uani 1 1 d . . . . .
H221 H 0.011904 0.433145 0.461451 0.028 Uiso 1 1 calc R . . . .
C222 C -0.0302(2) 0.4713(4) 0.3757(2) 0.0317(11) Uani 1 1 d . . . . .
H222 H -0.063080 0.423664 0.379918 0.038 Uiso 1 1 calc R . . . .
C223 C -0.02673(19) 0.5357(4) 0.3198(2) 0.0280(10) Uani 1 1 d . . . . .
H223 H -0.057274 0.529460 0.286833 0.034 Uiso 1 1 calc R . . . .
C224 C 0.02001(17) 0.6075(4) 0.31195(18) 0.0206(9) Uani 1 1 d . . . . .
H224 H 0.022053 0.649843 0.274139 0.025 Uiso 1 1 calc R . . . .
C225 C 0.17806(19) 0.9349(4) 0.23283(19) 0.0237(9) Uani 1 1 d . . . . .
H225 H 0.141879 0.904334 0.215310 0.028 Uiso 1 1 calc R . . . .
C226 C 0.2081(2) 1.0168(4) 0.20026(19) 0.0281(10) Uani 1 1 d . . . . .
H226 H 0.191841 1.042685 0.160118 0.034 Uiso 1 1 calc R . . . .
C227 C 0.26171(19) 1.0613(4) 0.22556(19) 0.0246(9) Uani 1 1 d . . . . .
H227 H 0.281225 1.116525 0.202183 0.030 Uiso 1 1 calc R . . . .
C228 C 0.28683(17) 1.0263(4) 0.28412(18) 0.0191(8) Uani 1 1 d . . . . .
H228 H 0.323327 1.056358 0.301013 0.023 Uiso 1 1 calc R . . . .
C229 C 0.41051(17) 1.0165(4) 0.52246(18) 0.0196(8) Uani 1 1 d . . . . .
H229 H 0.414108 1.058383 0.484782 0.024 Uiso 1 1 calc R . . . .
C230 C 0.44898(18) 1.0348(4) 0.57594(19) 0.0236(9) Uani 1 1 d . . . . .
H230 H 0.480479 1.087337 0.574228 0.028 Uiso 1 1 calc R . . . .
C231 C 0.44181(18) 0.9761(4) 0.63304(19) 0.0238(9) Uani 1 1 d . . . . .
H231 H 0.468001 0.991904 0.669142 0.029 Uiso 1 1 calc R . . . .
C232 C 0.39815(18) 0.8974(4) 0.63715(18) 0.0214(9) Uani 1 1 d . . . . .
H232 H 0.393996 0.857839 0.675383 0.026 Uiso 1 1 calc R . . . .
Cl61 Cl 0.53230(5) 0.68839(11) 0.65500(6) 0.0352(3) Uani 1 1 d . . . . .
Cl62 Cl 0.41826(6) 0.53676(12) 0.65911(6) 0.0417(3) Uani 1 1 d . . . . .
C61 C 0.48299(18) 0.6732(4) 0.5878(2) 0.0249(9) Uani 1 1 d . . . . .
C62 C 0.4330(2) 0.6054(4) 0.5905(2) 0.0272(10) Uani 1 1 d . . . . .
C63 C 0.39448(19) 0.5930(4) 0.5362(2) 0.0256(10) Uani 1 1 d . . . . .
H63 H 0.360403 0.547347 0.537181 0.031 Uiso 1 1 calc R . . . .
C64 C 0.40575(19) 0.6468(4) 0.4812(2) 0.0267(10) Uani 1 1 d . . . . .
H64 H 0.379413 0.637729 0.444506 0.032 Uiso 1 1 calc R . . . .
C65 C 0.4553(2) 0.7142(4) 0.4791(2) 0.0282(10) Uani 1 1 d . . . . .
H65 H 0.462854 0.751206 0.441081 0.034 Uiso 1 1 calc R . . . .
C66 C 0.4940(2) 0.7272(4) 0.5331(2) 0.0280(10) Uani 1 1 d . . . . .
H66 H 0.527834 0.773435 0.532018 0.034 Uiso 1 1 calc R . . . .
Cl51 Cl 1.03080(5) 0.19036(12) 0.67235(6) 0.0440(4) Uani 1 1 d . . . . .
Cl52 Cl 0.91624(7) 0.04611(13) 0.68635(7) 0.0519(4) Uani 1 1 d . . . . .
C51 C 0.97999(19) 0.1668(4) 0.6078(2) 0.0321(11) Uani 1 1 d . . . . .
C52 C 0.9300(2) 0.1023(4) 0.6146(2) 0.0309(11) Uani 1 1 d . . . . .
C53 C 0.88968(19) 0.0838(4) 0.5623(2) 0.0321(11) Uani 1 1 d . . . . .
H53 H 0.855547 0.039814 0.566341 0.039 Uiso 1 1 calc R . . . .
C54 C 0.89964(19) 0.1297(4) 0.5049(2) 0.0300(11) Uani 1 1 d . . . . .
H54 H 0.872449 0.116680 0.469271 0.036 Uiso 1 1 calc R . . . .
C55 C 0.9492(2) 0.1948(4) 0.4990(2) 0.0325(11) Uani 1 1 d . . . . .
H55 H 0.955701 0.226527 0.459384 0.039 Uiso 1 1 calc R . . . .
C56 C 0.9892(2) 0.2136(4) 0.5508(2) 0.0319(11) Uani 1 1 d . . . . .
H56 H 1.022941 0.258837 0.546727 0.038 Uiso 1 1 calc R . . . .


_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
N301 C03V 1.527(5) . ?
N301 C301 1.526(6) . ?
N301 C312 1.520(5) . ?
N301 C318 1.531(5) . ?
C03V H03A 0.9900 . ?
C03V H03B 0.9900 . ?
C03V C307 1.523(6) . ?
C301 H30A 0.9900 . ?
C301 H30B 0.9900 . ?
C301 C302 1.531(6) . ?
C302 H30C 0.9900 . ?
C302 H30D 0.9900 . ?
C302 C303 1.533(7) . ?
C303 H30E 0.9900 . ?
C303 H30F 0.9900 . ?
C303 C304 1.529(7) . ?
C304 H30G 0.9900 . ?
C304 H30H 0.9900 . ?
C304 C305 1.524(7) . ?
C305 H30I 0.9900 . ?
C305 H30J 0.9900 . ?
C305 C306 1.507(7) . ?
C306 H30K 0.9800 . ?
C306 H30L 0.9800 . ?
C306 H30M 0.9800 . ?
C307 H30N 0.9900 . ?
C307 H30O 0.9900 . ?
C307 C308 1.529(6) . ?
C308 H30P 0.9900 . ?
C308 H30Q 0.9900 . ?
C308 C309 1.532(6) . ?
C309 H30R 0.9900 . ?
C309 H30S 0.9900 . ?
C309 C310 1.528(6) . ?
C310 H31A 0.9900 . ?
C310 H31B 0.9900 . ?
C310 C311 1.524(7) . ?
C311 H31C 0.9800 . ?
C311 H31D 0.9800 . ?
C311 H31E 0.9800 . ?
C312 H31F 0.9900 . ?
C312 H31G 0.9900 . ?
C312 C313 1.525(6) . ?
C313 H31H 0.9900 . ?
C313 H31I 0.9900 . ?
C313 C314 1.530(6) . ?
C314 H31J 0.9900 . ?
C314 H31K 0.9900 . ?
C314 C315 1.523(7) . ?
C315 H31L 0.9900 . ?
C315 H31M 0.9900 . ?
C315 C316 1.516(7) . ?
C316 H31N 0.9900 . ?
C316 H31O 0.9900 . ?
C316 C317 1.511(7) . ?
C317 H31P 0.9800 . ?
C317 H31Q 0.9800 . ?
C317 H31R 0.9800 . ?
C318 H31S 0.9900 . ?
C318 H31T 0.9900 . ?
C318 C319 1.519(6) . ?
C319 H31U 0.9900 . ?
C319 H31V 0.9900 . ?
C319 C320 1.533(6) . ?
C320 H32A 0.9900 . ?
C320 H32B 0.9900 . ?
C320 C321 1.534(6) . ?
C321 H32C 0.9900 . ?
C321 H32D 0.9900 . ?
C321 C322 1.520(6) . ?
C322 H32E 0.9900 . ?
C322 H32F 0.9900 . ?
C322 C323 1.528(6) . ?
C323 H32G 0.9800 . ?
C323 H32H 0.9800 . ?
C323 H32I 0.9800 . ?
N401 C401 1.528(5) . ?
N401 C407 1.525(6) . ?
N401 C413 1.531(5) . ?
N401 C419 1.521(5) . ?
C401 H40A 0.9900 . ?
C401 H40B 0.9900 . ?
C401 C402 1.526(6) . ?
C402 H40C 0.9900 . ?
C402 H40D 0.9900 . ?
C402 C403 1.533(6) . ?
C403 H40E 0.9900 . ?
C403 H40F 0.9900 . ?
C403 C404 1.525(6) . ?
C404 H40G 0.9900 . ?
C404 H40H 0.9900 . ?
C404 C405 1.519(6) . ?
C405 H40I 0.9900 . ?
C405 H40J 0.9900 . ?
C405 C406 1.530(6) . ?
C406 H40K 0.9800 . ?
C406 H40L 0.9800 . ?
C406 H40M 0.9800 . ?
C407 H40N 0.9900 . ?
C407 H40O 0.9900 . ?
C407 C408 1.531(6) . ?
C408 H40P 0.9900 . ?
C408 H40Q 0.9900 . ?
C408 C409 1.522(6) . ?
C409 H40R 0.9900 . ?
C409 H40S 0.9900 . ?
C409 C410 1.542(6) . ?
C410 H41A 0.9900 . ?
C410 H41B 0.9900 . ?
C410 C411 1.521(7) . ?
C411 H41C 0.9900 . ?
C411 H41D 0.9900 . ?
C411 C412 1.526(7) . ?
C412 H41E 0.9800 . ?
C412 H41F 0.9800 . ?
C412 H41G 0.9800 . ?
C413 H41H 0.9900 . ?
C413 H41I 0.9900 . ?
C413 C414 1.519(6) . ?
C414 H41J 0.9900 . ?
C414 H41K 0.9900 . ?
C414 C415 1.537(6) . ?
C415 H41L 0.9900 . ?
C415 H41M 0.9900 . ?
C415 C416 1.538(6) . ?
C416 H41N 0.9900 . ?
C416 H41O 0.9900 . ?
C416 C417 1.533(6) . ?
C417 H41P 0.9900 . ?
C417 H41Q 0.9900 . ?
C417 C418 1.507(7) . ?
C418 H41R 0.9800 . ?
C418 H41S 0.9800 . ?
C418 H41T 0.9800 . ?
C419 H41U 0.9900 . ?
C419 H41V 0.9900 . ?
C419 C420 1.514(6) . ?
C420 H42A 0.9900 . ?
C420 H42B 0.9900 . ?
C420 C421 1.533(6) . ?
C421 H42C 0.9900 . ?
C421 H42D 0.9900 . ?
C421 C422 1.523(6) . ?
C422 H42E 0.9900 . ?
C422 H42F 0.9900 . ?
C422 C423 1.528(6) . ?
C423 H42G 0.9900 . ?
C423 H42H 0.9900 . ?
C423 C424 1.524(7) . ?
C424 H42I 0.9800 . ?
C424 H42J 0.9800 . ?
C424 H42K 0.9800 . ?
Ti01 O007 1.650(3) . ?
Ti01 N101 2.071(3) . ?
Ti01 N102 2.078(3) . ?
Ti01 N103 2.070(3) . ?
Ti01 N104 2.064(3) . ?
N101 C101 1.397(5) . ?
N101 C104 1.386(5) . ?
N102 C105 1.390(5) . ?
N102 C108 1.395(5) . ?
N103 C109 1.401(5) . ?
N103 C112 1.388(5) . ?
N104 C113 1.388(5) . ?
N104 C116 1.399(5) . ?
N105 C104 1.336(5) . ?
N105 C105 1.336(5) . ?
N106 C108 1.338(5) . ?
N106 C109 1.323(5) . ?
N107 C112 1.325(5) . ?
N107 C113 1.341(5) . ?
N108 C101 1.331(5) . ?
N108 C116 1.336(5) . ?
C101 C102 1.453(5) . ?
C102 C103 1.405(5) . ?
C102 C117 1.403(5) . ?
C103 C104 1.455(5) . ?
C103 C120 1.402(5) . ?
C105 C106 1.456(5) . ?
C106 C107 1.410(5) . ?
C106 C121 1.403(5) . ?
C107 C108 1.451(5) . ?
C107 C124 1.402(5) . ?
C109 C110 1.457(5) . ?
C110 C111 1.404(6) . ?
C110 C125 1.406(5) . ?
C111 C112 1.458(5) . ?
C111 C128 1.406(5) . ?
C113 C114 1.450(5) . ?
C114 C115 1.410(5) . ?
C114 C129 1.390(5) . ?
C115 C116 1.451(5) . ?
C115 C132 1.414(5) . ?
C117 H117 0.9500 . ?
C117 C118 1.390(6) . ?
C118 H118 0.9500 . ?
C118 C119 1.399(6) . ?
C119 H119 0.9500 . ?
C119 C120 1.388(6) . ?
C120 H120 0.9500 . ?
C121 H121 0.9500 . ?
C121 C122 1.397(6) . ?
C122 H122 0.9500 . ?
C122 C123 1.425(6) . ?
C123 H123 0.9500 . ?
C123 C124 1.372(6) . ?
C124 H124 0.9500 . ?
C125 H125 0.9500 . ?
C125 C126 1.394(6) . ?
C126 H126 0.9500 . ?
C126 C127 1.400(6) . ?
C127 H127 0.9500 . ?
C127 C128 1.383(6) . ?
C128 H128 0.9500 . ?
C129 H129 0.9500 . ?
C129 C130 1.390(6) . ?
C130 H130 0.9500 . ?
C130 C131 1.413(6) . ?
C131 H131 0.9500 . ?
C131 C132 1.386(6) . ?
C132 H132 0.9500 . ?
Ti02 O008 1.650(3) . ?
Ti02 N201 2.070(3) . ?
Ti02 N202 2.061(3) . ?
Ti02 N203 2.068(3) . ?
Ti02 N204 2.074(3) . ?
N201 C201 1.392(5) . ?
N201 C204 1.387(5) . ?
N202 C00V 1.389(5) . ?
N202 C208 1.397(5) . ?
N203 C209 1.398(5) . ?
N203 C212 1.385(5) . ?
N204 C213 1.390(5) . ?
N204 C216 1.390(5) . ?
N205 C00V 1.340(5) . ?
N205 C204 1.336(5) . ?
N206 C208 1.340(5) . ?
N206 C209 1.332(5) . ?
N207 C212 1.336(5) . ?
N207 C213 1.342(5) . ?
N208 C201 1.328(5) . ?
N208 C216 1.343(5) . ?
C00V C206 1.452(5) . ?
C201 C202 1.455(5) . ?
C202 C203 1.403(6) . ?
C202 C217 1.409(5) . ?
C203 C204 1.460(5) . ?
C203 C220 1.398(5) . ?
C206 C207 1.412(5) . ?
C206 C221 1.392(6) . ?
C207 C208 1.439(5) . ?
C207 C224 1.414(5) . ?
C209 C210 1.455(5) . ?
C210 C211 1.415(5) . ?
C210 C225 1.395(5) . ?
C211 C212 1.456(5) . ?
C211 C228 1.401(5) . ?
C213 C214 1.459(5) . ?
C214 C215 1.414(5) . ?
C214 C229 1.399(5) . ?
C215 C216 1.447(5) . ?
C215 C232 1.408(5) . ?
C217 H217 0.9500 . ?
C217 C218 1.399(6) . ?
C218 H218 0.9500 . ?
C218 C219 1.397(7) . ?
C219 H219 0.9500 . ?
C219 C220 1.397(6) . ?
C220 H220 0.9500 . ?
C221 H221 0.9500 . ?
C221 C222 1.379(6) . ?
C222 H222 0.9500 . ?
C222 C223 1.416(6) . ?
C223 H223 0.9500 . ?
C223 C224 1.385(6) . ?
C224 H224 0.9500 . ?
C225 H225 0.9500 . ?
C225 C226 1.397(6) . ?
C226 H226 0.9500 . ?
C226 C227 1.400(6) . ?
C227 H227 0.9500 . ?
C227 C228 1.386(6) . ?
C228 H228 0.9500 . ?
C229 H229 0.9500 . ?
C229 C230 1.393(6) . ?
C230 H230 0.9500 . ?
C230 C231 1.421(6) . ?
C231 H231 0.9500 . ?
C231 C232 1.365(6) . ?
C232 H232 0.9500 . ?
Cl61 C61 1.752(4) . ?
Cl62 C62 1.734(5) . ?
C61 C62 1.401(6) . ?
C61 C66 1.373(6) . ?
C62 C63 1.399(6) . ?
C63 H63 0.9500 . ?
C63 C64 1.379(6) . ?
C64 H64 0.9500 . ?
C64 C65 1.390(6) . ?
C65 H65 0.9500 . ?
C65 C66 1.397(6) . ?
C66 H66 0.9500 . ?
Cl51 C51 1.741(4) . ?
Cl52 C52 1.728(5) . ?
C51 C52 1.396(7) . ?
C51 C56 1.373(7) . ?
C52 C53 1.398(6) . ?
C53 H53 0.9500 . ?
C53 C54 1.381(7) . ?
C54 H54 0.9500 . ?
C54 C55 1.386(7) . ?
C55 H55 0.9500 . ?
C55 C56 1.388(6) . ?
C56 H56 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
C03V N301 C318 106.6(3) . . ?
C301 N301 C03V 111.1(3) . . ?
C301 N301 C318 110.7(3) . . ?
C312 N301 C03V 111.0(3) . . ?
C312 N301 C301 106.1(3) . . ?
C312 N301 C318 111.3(3) . . ?
N301 C03V H03A 108.5 . . ?
N301 C03V H03B 108.5 . . ?
H03A C03V H03B 107.5 . . ?
C307 C03V N301 115.0(3) . . ?
C307 C03V H03A 108.5 . . ?
C307 C03V H03B 108.5 . . ?
N301 C301 H30A 108.0 . . ?
N301 C301 H30B 108.0 . . ?
N301 C301 C302 117.1(4) . . ?
H30A C301 H30B 107.3 . . ?
C302 C301 H30A 108.0 . . ?
C302 C301 H30B 108.0 . . ?
C301 C302 H30C 109.8 . . ?
C301 C302 H30D 109.8 . . ?
C301 C302 C303 109.5(4) . . ?
H30C C302 H30D 108.2 . . ?
C303 C302 H30C 109.8 . . ?
C303 C302 H30D 109.8 . . ?
C302 C303 H30E 109.0 . . ?
C302 C303 H30F 109.0 . . ?
H30E C303 H30F 107.8 . . ?
C304 C303 C302 112.8(4) . . ?
C304 C303 H30E 109.0 . . ?
C304 C303 H30F 109.0 . . ?
C303 C304 H30G 108.9 . . ?
C303 C304 H30H 108.9 . . ?
H30G C304 H30H 107.7 . . ?
C305 C304 C303 113.3(4) . . ?
C305 C304 H30G 108.9 . . ?
C305 C304 H30H 108.9 . . ?
C304 C305 H30I 109.1 . . ?
C304 C305 H30J 109.1 . . ?
H30I C305 H30J 107.9 . . ?
C306 C305 C304 112.4(4) . . ?
C306 C305 H30I 109.1 . . ?
C306 C305 H30J 109.1 . . ?
C305 C306 H30K 109.5 . . ?
C305 C306 H30L 109.5 . . ?
C305 C306 H30M 109.5 . . ?
H30K C306 H30L 109.5 . . ?
H30K C306 H30M 109.5 . . ?
H30L C306 H30M 109.5 . . ?
C03V C307 H30N 109.5 . . ?
C03V C307 H30O 109.5 . . ?
C03V C307 C308 110.7(4) . . ?
H30N C307 H30O 108.1 . . ?
C308 C307 H30N 109.5 . . ?
C308 C307 H30O 109.5 . . ?
C307 C308 H30P 109.2 . . ?
C307 C308 H30Q 109.2 . . ?
C307 C308 C309 111.8(4) . . ?
H30P C308 H30Q 107.9 . . ?
C309 C308 H30P 109.2 . . ?
C309 C308 H30Q 109.2 . . ?
C308 C309 H30R 109.0 . . ?
C308 C309 H30S 109.0 . . ?
H30R C309 H30S 107.8 . . ?
C310 C309 C308 113.0(4) . . ?
C310 C309 H30R 109.0 . . ?
C310 C309 H30S 109.0 . . ?
C309 C310 H31A 109.2 . . ?
C309 C310 H31B 109.2 . . ?
H31A C310 H31B 107.9 . . ?
C311 C310 C309 112.1(4) . . ?
C311 C310 H31A 109.2 . . ?
C311 C310 H31B 109.2 . . ?
C310 C311 H31C 109.5 . . ?
C310 C311 H31D 109.5 . . ?
C310 C311 H31E 109.5 . . ?
H31C C311 H31D 109.5 . . ?
H31C C311 H31E 109.5 . . ?
H31D C311 H31E 109.5 . . ?
N301 C312 H31F 108.1 . . ?
N301 C312 H31G 108.1 . . ?
N301 C312 C313 116.7(3) . . ?
H31F C312 H31G 107.3 . . ?
C313 C312 H31F 108.1 . . ?
C313 C312 H31G 108.1 . . ?
C312 C313 H31H 109.6 . . ?
C312 C313 H31I 109.6 . . ?
C312 C313 C314 110.4(4) . . ?
H31H C313 H31I 108.1 . . ?
C314 C313 H31H 109.6 . . ?
C314 C313 H31I 109.6 . . ?
C313 C314 H31J 109.0 . . ?
C313 C314 H31K 109.0 . . ?
H31J C314 H31K 107.8 . . ?
C315 C314 C313 112.8(4) . . ?
C315 C314 H31J 109.0 . . ?
C315 C314 H31K 109.0 . . ?
C314 C315 H31L 108.6 . . ?
C314 C315 H31M 108.6 . . ?
H31L C315 H31M 107.6 . . ?
C316 C315 C314 114.7(4) . . ?
C316 C315 H31L 108.6 . . ?
C316 C315 H31M 108.6 . . ?
C315 C316 H31N 108.6 . . ?
C315 C316 H31O 108.6 . . ?
H31N C316 H31O 107.6 . . ?
C317 C316 C315 114.6(4) . . ?
C317 C316 H31N 108.6 . . ?
C317 C316 H31O 108.6 . . ?
C316 C317 H31P 109.5 . . ?
C316 C317 H31Q 109.5 . . ?
C316 C317 H31R 109.5 . . ?
H31P C317 H31Q 109.5 . . ?
H31P C317 H31R 109.5 . . ?
H31Q C317 H31R 109.5 . . ?
N301 C318 H31S 108.2 . . ?
N301 C318 H31T 108.2 . . ?
H31S C318 H31T 107.4 . . ?
C319 C318 N301 116.2(4) . . ?
C319 C318 H31S 108.2 . . ?
C319 C318 H31T 108.2 . . ?
C318 C319 H31U 109.7 . . ?
C318 C319 H31V 109.7 . . ?
C318 C319 C320 109.7(4) . . ?
H31U C319 H31V 108.2 . . ?
C320 C319 H31U 109.7 . . ?
C320 C319 H31V 109.7 . . ?
C319 C320 H32A 109.0 . . ?
C319 C320 H32B 109.0 . . ?
C319 C320 C321 113.0(4) . . ?
H32A C320 H32B 107.8 . . ?
C321 C320 H32A 109.0 . . ?
C321 C320 H32B 109.0 . . ?
C320 C321 H32C 108.9 . . ?
C320 C321 H32D 108.9 . . ?
H32C C321 H32D 107.8 . . ?
C322 C321 C320 113.2(4) . . ?
C322 C321 H32C 108.9 . . ?
C322 C321 H32D 108.9 . . ?
C321 C322 H32E 109.0 . . ?
C321 C322 H32F 109.0 . . ?
C321 C322 C323 112.9(4) . . ?
H32E C322 H32F 107.8 . . ?
C323 C322 H32E 109.0 . . ?
C323 C322 H32F 109.0 . . ?
C322 C323 H32G 109.5 . . ?
C322 C323 H32H 109.5 . . ?
C322 C323 H32I 109.5 . . ?
H32G C323 H32H 109.5 . . ?
H32G C323 H32I 109.5 . . ?
H32H C323 H32I 109.5 . . ?
C401 N401 C413 107.3(3) . . ?
C407 N401 C401 111.0(3) . . ?
C407 N401 C413 110.7(3) . . ?
C419 N401 C401 110.8(3) . . ?
C419 N401 C407 106.6(3) . . ?
C419 N401 C413 110.6(3) . . ?
N401 C401 H40A 108.6 . . ?
N401 C401 H40B 108.6 . . ?
H40A C401 H40B 107.6 . . ?
C402 C401 N401 114.5(4) . . ?
C402 C401 H40A 108.6 . . ?
C402 C401 H40B 108.6 . . ?
C401 C402 H40C 109.4 . . ?
C401 C402 H40D 109.4 . . ?
C401 C402 C403 111.0(4) . . ?
H40C C402 H40D 108.0 . . ?
C403 C402 H40C 109.4 . . ?
C403 C402 H40D 109.4 . . ?
C402 C403 H40E 109.1 . . ?
C402 C403 H40F 109.1 . . ?
H40E C403 H40F 107.8 . . ?
C404 C403 C402 112.7(4) . . ?
C404 C403 H40E 109.1 . . ?
C404 C403 H40F 109.1 . . ?
C403 C404 H40G 109.0 . . ?
C403 C404 H40H 109.0 . . ?
H40G C404 H40H 107.8 . . ?
C405 C404 C403 113.1(4) . . ?
C405 C404 H40G 109.0 . . ?
C405 C404 H40H 109.0 . . ?
C404 C405 H40I 109.0 . . ?
C404 C405 H40J 109.0 . . ?
C404 C405 C406 112.8(4) . . ?
H40I C405 H40J 107.8 . . ?
C406 C405 H40I 109.0 . . ?
C406 C405 H40J 109.0 . . ?
C405 C406 H40K 109.5 . . ?
C405 C406 H40L 109.5 . . ?
C405 C406 H40M 109.5 . . ?
H40K C406 H40L 109.5 . . ?
H40K C406 H40M 109.5 . . ?
H40L C406 H40M 109.5 . . ?
N401 C407 H40N 108.1 . . ?
N401 C407 H40O 108.1 . . ?
N401 C407 C408 116.8(3) . . ?
H40N C407 H40O 107.3 . . ?
C408 C407 H40N 108.1 . . ?
C408 C407 H40O 108.1 . . ?
C407 C408 H40P 109.7 . . ?
C407 C408 H40Q 109.7 . . ?
H40P C408 H40Q 108.2 . . ?
C409 C408 C407 109.8(4) . . ?
C409 C408 H40P 109.7 . . ?
C409 C408 H40Q 109.7 . . ?
C408 C409 H40R 109.3 . . ?
C408 C409 H40S 109.3 . . ?
C408 C409 C410 111.7(4) . . ?
H40R C409 H40S 107.9 . . ?
C410 C409 H40R 109.3 . . ?
C410 C409 H40S 109.3 . . ?
C409 C410 H41A 108.7 . . ?
C409 C410 H41B 108.7 . . ?
H41A C410 H41B 107.6 . . ?
C411 C410 C409 114.3(4) . . ?
C411 C410 H41A 108.7 . . ?
C411 C410 H41B 108.7 . . ?
C410 C411 H41C 109.5 . . ?
C410 C411 H41D 109.5 . . ?
C410 C411 C412 110.8(4) . . ?
H41C C411 H41D 108.1 . . ?
C412 C411 H41C 109.5 . . ?
C412 C411 H41D 109.5 . . ?
C411 C412 H41E 109.5 . . ?
C411 C412 H41F 109.5 . . ?
C411 C412 H41G 109.5 . . ?
H41E C412 H41F 109.5 . . ?
H41E C412 H41G 109.5 . . ?
H41F C412 H41G 109.5 . . ?
N401 C413 H41H 108.5 . . ?
N401 C413 H41I 108.5 . . ?
H41H C413 H41I 107.5 . . ?
C414 C413 N401 115.0(3) . . ?
C414 C413 H41H 108.5 . . ?
C414 C413 H41I 108.5 . . ?
C413 C414 H41J 109.4 . . ?
C413 C414 H41K 109.4 . . ?
C413 C414 C415 111.4(4) . . ?
H41J C414 H41K 108.0 . . ?
C415 C414 H41J 109.4 . . ?
C415 C414 H41K 109.4 . . ?
C414 C415 H41L 109.5 . . ?
C414 C415 H41M 109.5 . . ?
C414 C415 C416 110.7(4) . . ?
H41L C415 H41M 108.1 . . ?
C416 C415 H41L 109.5 . . ?
C416 C415 H41M 109.5 . . ?
C415 C416 H41N 108.9 . . ?
C415 C416 H41O 108.9 . . ?
H41N C416 H41O 107.7 . . ?
C417 C416 C415 113.4(4) . . ?
C417 C416 H41N 108.9 . . ?
C417 C416 H41O 108.9 . . ?
C416 C417 H41P 109.0 . . ?
C416 C417 H41Q 109.0 . . ?
H41P C417 H41Q 107.8 . . ?
C418 C417 C416 112.9(4) . . ?
C418 C417 H41P 109.0 . . ?
C418 C417 H41Q 109.0 . . ?
C417 C418 H41R 109.5 . . ?
C417 C418 H41S 109.5 . . ?
C417 C418 H41T 109.5 . . ?
H41R C418 H41S 109.5 . . ?
H41R C418 H41T 109.5 . . ?
H41S C418 H41T 109.5 . . ?
N401 C419 H41U 108.2 . . ?
N401 C419 H41V 108.2 . . ?
H41U C419 H41V 107.4 . . ?
C420 C419 N401 116.3(3) . . ?
C420 C419 H41U 108.2 . . ?
C420 C419 H41V 108.2 . . ?
C419 C420 H42A 109.4 . . ?
C419 C420 H42B 109.4 . . ?
C419 C420 C421 111.2(3) . . ?
H42A C420 H42B 108.0 . . ?
C421 C420 H42A 109.4 . . ?
C421 C420 H42B 109.4 . . ?
C420 C421 H42C 109.1 . . ?
C420 C421 H42D 109.1 . . ?
H42C C421 H42D 107.9 . . ?
C422 C421 C420 112.4(4) . . ?
C422 C421 H42C 109.1 . . ?
C422 C421 H42D 109.1 . . ?
C421 C422 H42E 108.9 . . ?
C421 C422 H42F 108.9 . . ?
C421 C422 C423 113.5(4) . . ?
H42E C422 H42F 107.7 . . ?
C423 C422 H42E 108.9 . . ?
C423 C422 H42F 108.9 . . ?
C422 C423 H42G 108.6 . . ?
C422 C423 H42H 108.6 . . ?
H42G C423 H42H 107.6 . . ?
C424 C423 C422 114.5(4) . . ?
C424 C423 H42G 108.6 . . ?
C424 C423 H42H 108.6 . . ?
C423 C424 H42I 109.5 . . ?
C423 C424 H42J 109.5 . . ?
C423 C424 H42K 109.5 . . ?
H42I C424 H42J 109.5 . . ?
H42I C424 H42K 109.5 . . ?
H42J C424 H42K 109.5 . . ?
O007 Ti01 N101 108.81(13) . . ?
O007 Ti01 N102 108.45(13) . . ?
O007 Ti01 N103 106.25(13) . . ?
O007 Ti01 N104 106.23(13) . . ?
N101 Ti01 N102 84.60(12) . . ?
N103 Ti01 N101 144.94(13) . . ?
N103 Ti01 N102 84.79(12) . . ?
N104 Ti01 N101 85.15(12) . . ?
N104 Ti01 N102 145.31(12) . . ?
N104 Ti01 N103 84.86(12) . . ?
C101 N101 Ti01 126.0(2) . . ?
C104 N101 Ti01 124.5(2) . . ?
C104 N101 C101 108.3(3) . . ?
C105 N102 Ti01 124.2(2) . . ?
C105 N102 C108 108.5(3) . . ?
C108 N102 Ti01 125.1(2) . . ?
C109 N103 Ti01 125.5(2) . . ?
C112 N103 Ti01 123.9(2) . . ?
C112 N103 C109 108.4(3) . . ?
C113 N104 Ti01 124.3(2) . . ?
C113 N104 C116 108.4(3) . . ?
C116 N104 Ti01 126.1(2) . . ?
C105 N105 C104 123.0(3) . . ?
C109 N106 C108 123.3(3) . . ?
C112 N107 C113 122.3(3) . . ?
C101 N108 C116 123.7(3) . . ?
N101 C101 C102 108.8(3) . . ?
N108 C101 N101 127.4(3) . . ?
N108 C101 C102 123.8(3) . . ?
C103 C102 C101 106.9(3) . . ?
C117 C102 C101 131.8(4) . . ?
C117 C102 C103 121.2(4) . . ?
C102 C103 C104 107.1(3) . . ?
C120 C103 C102 120.8(3) . . ?
C120 C103 C104 132.1(4) . . ?
N101 C104 C103 108.9(3) . . ?
N105 C104 N101 128.0(3) . . ?
N105 C104 C103 123.0(3) . . ?
N102 C105 C106 108.7(3) . . ?
N105 C105 N102 127.3(3) . . ?
N105 C105 C106 124.0(3) . . ?
C107 C106 C105 107.1(3) . . ?
C121 C106 C105 131.8(4) . . ?
C121 C106 C107 121.0(4) . . ?
C106 C107 C108 106.9(3) . . ?
C124 C107 C106 120.9(4) . . ?
C124 C107 C108 132.1(4) . . ?
N102 C108 C107 108.9(3) . . ?
N106 C108 N102 127.8(3) . . ?
N106 C108 C107 123.3(3) . . ?
N103 C109 C110 108.6(3) . . ?
N106 C109 N103 127.6(3) . . ?
N106 C109 C110 123.8(3) . . ?
C111 C110 C109 106.9(3) . . ?
C111 C110 C125 121.3(4) . . ?
C125 C110 C109 131.8(4) . . ?
C110 C111 C112 107.4(3) . . ?
C110 C111 C128 120.8(4) . . ?
C128 C111 C112 131.8(4) . . ?
N103 C112 C111 108.7(3) . . ?
N107 C112 N103 128.4(3) . . ?
N107 C112 C111 122.9(3) . . ?
N104 C113 C114 108.9(3) . . ?
N107 C113 N104 128.0(3) . . ?
N107 C113 C114 123.0(3) . . ?
C115 C114 C113 107.1(3) . . ?
C129 C114 C113 131.3(4) . . ?
C129 C114 C115 121.6(4) . . ?
C114 C115 C116 107.0(3) . . ?
C114 C115 C132 119.9(3) . . ?
C132 C115 C116 133.1(3) . . ?
N104 C116 C115 108.6(3) . . ?
N108 C116 N104 127.2(3) . . ?
N108 C116 C115 124.2(3) . . ?
C102 C117 H117 121.5 . . ?
C118 C117 C102 117.1(4) . . ?
C118 C117 H117 121.5 . . ?
C117 C118 H118 119.0 . . ?
C117 C118 C119 122.0(4) . . ?
C119 C118 H118 119.0 . . ?
C118 C119 H119 119.5 . . ?
C120 C119 C118 121.0(4) . . ?
C120 C119 H119 119.5 . . ?
C103 C120 H120 121.0 . . ?
C119 C120 C103 117.9(4) . . ?
C119 C120 H120 121.0 . . ?
C106 C121 H121 121.2 . . ?
C122 C121 C106 117.6(4) . . ?
C122 C121 H121 121.2 . . ?
C121 C122 H122 119.6 . . ?
C121 C122 C123 120.8(4) . . ?
C123 C122 H122 119.6 . . ?
C122 C123 H123 119.3 . . ?
C124 C123 C122 121.4(4) . . ?
C124 C123 H123 119.3 . . ?
C107 C124 H124 120.9 . . ?
C123 C124 C107 118.2(4) . . ?
C123 C124 H124 120.9 . . ?
C110 C125 H125 121.6 . . ?
C126 C125 C110 116.9(4) . . ?
C126 C125 H125 121.6 . . ?
C125 C126 H126 119.1 . . ?
C125 C126 C127 121.9(4) . . ?
C127 C126 H126 119.1 . . ?
C126 C127 H127 119.4 . . ?
C128 C127 C126 121.3(4) . . ?
C128 C127 H127 119.4 . . ?
C111 C128 H128 121.1 . . ?
C127 C128 C111 117.8(4) . . ?
C127 C128 H128 121.1 . . ?
C114 C129 H129 120.8 . . ?
C114 C129 C130 118.5(4) . . ?
C130 C129 H129 120.8 . . ?
C129 C130 H130 119.8 . . ?
C129 C130 C131 120.4(4) . . ?
C131 C130 H130 119.8 . . ?
C130 C131 H131 119.2 . . ?
C132 C131 C130 121.7(4) . . ?
C132 C131 H131 119.2 . . ?
C115 C132 H132 121.0 . . ?
C131 C132 C115 118.0(4) . . ?
C131 C132 H132 121.0 . . ?
O008 Ti02 N201 105.72(13) . . ?
O008 Ti02 N202 105.86(13) . . ?
O008 Ti02 N203 108.39(13) . . ?
O008 Ti02 N204 108.91(13) . . ?
N201 Ti02 N204 84.71(12) . . ?
N202 Ti02 N201 85.19(12) . . ?
N202 Ti02 N203 85.31(12) . . ?
N202 Ti02 N204 145.22(12) . . ?
N203 Ti02 N201 145.89(13) . . ?
N203 Ti02 N204 84.68(12) . . ?
C201 N201 Ti02 125.6(2) . . ?
C204 N201 Ti02 123.5(2) . . ?
C204 N201 C201 108.4(3) . . ?
C00V N202 Ti02 123.8(3) . . ?
C00V N202 C208 108.0(3) . . ?
C208 N202 Ti02 126.2(2) . . ?
C209 N203 Ti02 125.6(2) . . ?
C212 N203 Ti02 124.3(2) . . ?
C212 N203 C209 108.3(3) . . ?
C213 N204 Ti02 124.4(2) . . ?
C213 N204 C216 108.2(3) . . ?
C216 N204 Ti02 125.8(2) . . ?
C204 N205 C00V 122.6(3) . . ?
C209 N206 C208 124.0(3) . . ?
C212 N207 C213 122.7(3) . . ?
C201 N208 C216 123.3(3) . . ?
N202 C00V C206 109.0(3) . . ?
N205 C00V N202 127.9(4) . . ?
N205 C00V C206 123.0(3) . . ?
N201 C201 C202 108.8(3) . . ?
N208 C201 N201 127.5(3) . . ?
N208 C201 C202 123.7(3) . . ?
C203 C202 C201 107.0(3) . . ?
C203 C202 C217 121.4(4) . . ?
C217 C202 C201 131.6(4) . . ?
C202 C203 C204 107.0(3) . . ?
C220 C203 C202 121.5(4) . . ?
C220 C203 C204 131.5(4) . . ?
N201 C204 C203 108.8(3) . . ?
N205 C204 N201 128.0(3) . . ?
N205 C204 C203 123.2(4) . . ?
C207 C206 C00V 106.7(3) . . ?
C221 C206 C00V 131.6(4) . . ?
C221 C206 C207 121.7(4) . . ?
C206 C207 C208 107.1(3) . . ?
C206 C207 C224 119.8(4) . . ?
C224 C207 C208 133.1(4) . . ?
N202 C208 C207 109.1(3) . . ?
N206 C208 N202 126.6(3) . . ?
N206 C208 C207 124.3(3) . . ?
N203 C209 C210 108.9(3) . . ?
N206 C209 N203 127.5(3) . . ?
N206 C209 C210 123.6(3) . . ?
C211 C210 C209 106.8(3) . . ?
C225 C210 C209 132.4(4) . . ?
C225 C210 C211 120.8(4) . . ?
C210 C211 C212 106.8(3) . . ?
C228 C211 C210 120.7(3) . . ?
C228 C211 C212 132.5(4) . . ?
N203 C212 C211 109.2(3) . . ?
N207 C212 N203 127.6(3) . . ?
N207 C212 C211 123.0(3) . . ?
N204 C213 C214 108.9(3) . . ?
N207 C213 N204 127.7(3) . . ?
N207 C213 C214 123.3(3) . . ?
C215 C214 C213 106.7(3) . . ?
C229 C214 C213 132.3(4) . . ?
C229 C214 C215 121.0(3) . . ?
C214 C215 C216 106.8(3) . . ?
C232 C215 C214 120.6(4) . . ?
C232 C215 C216 132.6(4) . . ?
N204 C216 C215 109.4(3) . . ?
N208 C216 N204 127.5(3) . . ?
N208 C216 C215 123.1(3) . . ?
C202 C217 H217 121.8 . . ?
C218 C217 C202 116.4(4) . . ?
C218 C217 H217 121.8 . . ?
C217 C218 H218 119.0 . . ?
C219 C218 C217 122.1(4) . . ?
C219 C218 H218 119.0 . . ?
C218 C219 H219 119.3 . . ?
C218 C219 C220 121.4(4) . . ?
C220 C219 H219 119.3 . . ?
C203 C220 H220 121.4 . . ?
C219 C220 C203 117.2(4) . . ?
C219 C220 H220 121.4 . . ?
C206 C221 H221 120.8 . . ?
C222 C221 C206 118.4(4) . . ?
C222 C221 H221 120.8 . . ?
C221 C222 H222 119.7 . . ?
C221 C222 C223 120.6(4) . . ?
C223 C222 H222 119.7 . . ?
C222 C223 H223 119.1 . . ?
C224 C223 C222 121.7(4) . . ?
C224 C223 H223 119.1 . . ?
C207 C224 H224 121.1 . . ?
C223 C224 C207 117.8(4) . . ?
C223 C224 H224 121.1 . . ?
C210 C225 H225 121.1 . . ?
C210 C225 C226 117.8(4) . . ?
C226 C225 H225 121.1 . . ?
C225 C226 H226 119.3 . . ?
C225 C226 C227 121.3(4) . . ?
C227 C226 H226 119.3 . . ?
C226 C227 H227 119.4 . . ?
C228 C227 C226 121.2(4) . . ?
C228 C227 H227 119.4 . . ?
C211 C228 H228 120.9 . . ?
C227 C228 C211 118.1(4) . . ?
C227 C228 H228 120.9 . . ?
C214 C229 H229 121.2 . . ?
C230 C229 C214 117.6(4) . . ?
C230 C229 H229 121.2 . . ?
C229 C230 H230 119.5 . . ?
C229 C230 C231 121.0(4) . . ?
C231 C230 H230 119.5 . . ?
C230 C231 H231 119.3 . . ?
C232 C231 C230 121.5(4) . . ?
C232 C231 H231 119.3 . . ?
C215 C232 H232 120.9 . . ?
C231 C232 C215 118.3(4) . . ?
C231 C232 H232 120.9 . . ?
C62 C61 Cl61 119.6(3) . . ?
C66 C61 Cl61 119.6(4) . . ?
C66 C61 C62 120.8(4) . . ?
C61 C62 Cl62 121.6(3) . . ?
C63 C62 Cl62 119.6(4) . . ?
C63 C62 C61 118.8(4) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 C62 120.2(4) . . ?
C64 C63 H63 119.9 . . ?
C63 C64 H64 119.7 . . ?
C63 C64 C65 120.6(4) . . ?
C65 C64 H64 119.7 . . ?
C64 C65 H65 120.2 . . ?
C64 C65 C66 119.5(4) . . ?
C66 C65 H65 120.2 . . ?
C61 C66 C65 120.0(4) . . ?
C61 C66 H66 120.0 . . ?
C65 C66 H66 120.0 . . ?
C52 C51 Cl51 120.1(4) . . ?
C56 C51 Cl51 119.4(4) . . ?
C56 C51 C52 120.5(4) . . ?
C51 C52 Cl52 121.5(4) . . ?
C51 C52 C53 119.4(5) . . ?
C53 C52 Cl52 119.1(4) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 C52 119.8(4) . . ?
C54 C53 H53 120.1 . . ?
C53 C54 H54 119.9 . . ?
C53 C54 C55 120.3(4) . . ?
C55 C54 H54 119.9 . . ?
C54 C55 H55 119.9 . . ?
C54 C55 C56 120.1(5) . . ?
C56 C55 H55 119.9 . . ?
C51 C56 C55 119.9(5) . . ?
C51 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.57(2)
2 0.43(2)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane/o-dichlorobenzene'
_chemical_compound_source        no
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
