# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_S15MDJ30
_database_code_depnum_ccdc_archive 'CCDC 1534472'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H68 N2 O4 Ti'
_chemical_formula_weight         712.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   23.0224(3)
_cell_length_b                   14.30120(10)
_cell_length_c                   28.4630(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.744(2)
_cell_angle_gamma                90
_cell_volume                     8578.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16685
_cell_measurement_theta_min      4.9310
_cell_measurement_theta_max      71.8850

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_F_000             3104
_exptl_transmission_factor_min   0.692
_exptl_transmission_factor_max   0.755
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.985
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150.0(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            34998
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         4.444
_diffrn_reflns_theta_max         72.065
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8360
_reflns_number_gt                7530
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0596P)²+7.6708P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8360
_refine_ls_number_parameters     473
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.1137
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
Ti1 Ti 0.52202(2) 0.42246(2) 0.31579(2) 0.01585(9) Uani 1 1 d . . . . .
O1 O 0.54148(5) 0.29739(8) 0.32218(4) 0.0231(2) Uani 1 1 d . . . . .
N1 N 0.51419(6) 0.57542(9) 0.30582(5) 0.0198(3) Uani 1 1 d . . . . .
C1 C 0.58798(9) 0.24388(12) 0.36120(7) 0.0304(4) Uani 1 1 d . . . . .
H1 H 0.6227 0.2863 0.3834 0.037 Uiso 1 1 calc R U . . .
O2 O 0.59457(6) 0.45301(8) 0.37289(4) 0.0241(2) Uani 1 1 d . . . . .
N2 N 0.57534(6) 0.45616(9) 0.26429(5) 0.0168(3) Uani 1 1 d . . . . .
C2 C 0.61542(9) 0.17209(13) 0.33674(10) 0.0416(5) Uani 1 1 d . . . . .
H2A H 0.5816 0.1305 0.3147 0.062 Uiso 1 1 calc R U . . .
H2B H 0.6479 0.1353 0.3636 0.062 Uiso 1 1 calc R U . . .
H2C H 0.6346 0.2040 0.3160 0.062 Uiso 1 1 calc R U . . .
O3 O 0.46537(6) 0.44122(8) 0.34790(4) 0.0232(2) Uani 1 1 d . . . . .
C3 C 0.55769(13) 0.19717(19) 0.39361(10) 0.0586(7) Uani 1 1 d . . . . .
H3A H 0.5398 0.2450 0.4086 0.088 Uiso 1 1 calc R U . . .
H3B H 0.5899 0.1612 0.4212 0.088 Uiso 1 1 calc R U . . .
H3C H 0.5239 0.1551 0.3720 0.088 Uiso 1 1 calc R U . . .
O4 O 0.45305(5) 0.40491(8) 0.24983(4) 0.0209(2) Uani 1 1 d . . . . .
C4 C 0.6123(2) 0.5066(5) 0.4194(2) 0.032(2) Uani 0.6 1 d D . P A 1
H4 H 0.5772 0.5510 0.4157 0.038 Uiso 0.6 1 calc R U P A 1
C5 C 0.6198(3) 0.4383(4) 0.46179(13) 0.0736(18) Uani 0.6 1 d D . P A 1
H5A H 0.5802 0.4033 0.4531 0.110 Uiso 0.6 1 calc R U P A 1
H5B H 0.6297 0.4725 0.4940 0.110 Uiso 0.6 1 calc R U P A 1
H5C H 0.6544 0.3947 0.4659 0.110 Uiso 0.6 1 calc R U P A 1
C6 C 0.6716(2) 0.5618(3) 0.42885(15) 0.0430(9) Uani 0.6 1 d D . P A 1
H6A H 0.7062 0.5189 0.4321 0.064 Uiso 0.6 1 calc R U P A 1
H6B H 0.6833 0.5980 0.4606 0.064 Uiso 0.6 1 calc R U P A 1
H6C H 0.6640 0.6044 0.4000 0.064 Uiso 0.6 1 calc R U P A 1
C7 C 0.43036(7) 0.50832(11) 0.35577(6) 0.0203(3) Uani 1 1 d . . . . .
C8 C 0.43869(8) 0.60258(11) 0.34453(6) 0.0216(3) Uani 1 1 d . . . . .
C9 C 0.40399(8) 0.67373(12) 0.35512(7) 0.0260(3) Uani 1 1 d . . . . .
H9 H 0.4107 0.7367 0.3479 0.031 Uiso 1 1 calc R U . . .
C10 C 0.36026(8) 0.65502(12) 0.37576(7) 0.0265(4) Uani 1 1 d . . . . .
C11 C 0.35177(8) 0.56144(12) 0.38534(6) 0.0248(3) Uani 1 1 d . . . . .
H11 H 0.3215 0.5475 0.3992 0.030 Uiso 1 1 calc R U . . .
C12 C 0.38477(8) 0.48709(12) 0.37600(6) 0.0222(3) Uani 1 1 d . . . . .
C13 C 0.32272(10) 0.73529(14) 0.38610(10) 0.0407(5) Uani 1 1 d . . . . .
C14 C 0.27703(10) 0.70164(16) 0.40911(9) 0.0442(5) Uani 1 1 d . . . . .
H14A H 0.3011 0.6725 0.4425 0.066 Uiso 1 1 calc R U . . .
H14B H 0.2477 0.6558 0.3861 0.066 Uiso 1 1 calc R U . . .
H14C H 0.2530 0.7550 0.4136 0.066 Uiso 1 1 calc R U . . .
C15 C 0.36791(16) 0.8055(3) 0.4213(2) 0.120(2) Uani 1 1 d . . . . .
H15A H 0.3936 0.7755 0.4541 0.179 Uiso 1 1 calc R U . . .
H15B H 0.3438 0.8574 0.4272 0.179 Uiso 1 1 calc R U . . .
H15C H 0.3958 0.8295 0.4056 0.179 Uiso 1 1 calc R U . . .
C16 C 0.28137(15) 0.7816(2) 0.33399(14) 0.0736(10) Uani 1 1 d . . . . .
H16A H 0.2579 0.8344 0.3399 0.110 Uiso 1 1 calc R U . . .
H16B H 0.2513 0.7356 0.3117 0.110 Uiso 1 1 calc R U . . .
H16C H 0.3087 0.8042 0.3175 0.110 Uiso 1 1 calc R U . . .
C17 C 0.37310(9) 0.38570(12) 0.38810(7) 0.0293(4) Uani 1 1 d . . . . .
C18 C 0.31678(10) 0.37822(14) 0.40380(8) 0.0352(4) Uani 1 1 d . . . . .
H18A H 0.3087 0.3123 0.4084 0.053 Uiso 1 1 calc R U . . .
H18B H 0.2790 0.4057 0.3769 0.053 Uiso 1 1 calc R U . . .
H18C H 0.3267 0.4119 0.4361 0.053 Uiso 1 1 calc R U . . .
C19 C 0.43270(11) 0.34913(17) 0.43228(9) 0.0474(6) Uani 1 1 d . . . . .
H19A H 0.4689 0.3522 0.4225 0.071 Uiso 1 1 calc R U . . .
H19B H 0.4259 0.2842 0.4398 0.071 Uiso 1 1 calc R U . . .
H19C H 0.4415 0.3877 0.4629 0.071 Uiso 1 1 calc R U . . .
C20 C 0.35664(12) 0.32329(14) 0.34039(9) 0.0436(5) Uani 1 1 d . . . . .
H20A H 0.3925 0.3223 0.3301 0.065 Uiso 1 1 calc R U . . .
H20B H 0.3191 0.3483 0.3122 0.065 Uiso 1 1 calc R U . . .
H20C H 0.3479 0.2596 0.3484 0.065 Uiso 1 1 calc R U . . .
C21 C 0.48231(8) 0.63054(11) 0.32195(6) 0.0221(3) Uani 1 1 d . . . . .
H21 H 0.4878 0.6958 0.3188 0.027 Uiso 1 1 calc R U . . .
C22 C 0.55726(8) 0.61736(11) 0.28527(6) 0.0218(3) Uani 1 1 d . . . . .
H22A H 0.6004 0.6235 0.3127 0.026 Uiso 1 1 calc R U . . .
H22B H 0.5420 0.6803 0.2713 0.026 Uiso 1 1 calc R U . . .
C23 C 0.55850(7) 0.55342(11) 0.24301(6) 0.0195(3) Uani 1 1 d . . . . .
H23 H 0.5141 0.5506 0.2162 0.023 Uiso 1 1 calc R U . . .
C24 C 0.60014(8) 0.58983(12) 0.21645(7) 0.0250(3) Uani 1 1 d . . . . .
H24A H 0.5897 0.5552 0.1840 0.030 Uiso 1 1 calc R U . . .
H24B H 0.5904 0.6567 0.2078 0.030 Uiso 1 1 calc R U . . .
C25 C 0.67094(8) 0.57952(12) 0.24962(8) 0.0284(4) Uani 1 1 d . . . . .
H25A H 0.6957 0.5992 0.2298 0.034 Uiso 1 1 calc R U . . .
H25B H 0.6829 0.6204 0.2802 0.034 Uiso 1 1 calc R U . . .
C26 C 0.68637(8) 0.47831(12) 0.26655(7) 0.0255(3) Uani 1 1 d . . . . .
H26A H 0.7318 0.4728 0.2897 0.031 Uiso 1 1 calc R U . . .
H26B H 0.6783 0.4382 0.2362 0.031 Uiso 1 1 calc R U . . .
C27 C 0.64539(7) 0.44561(11) 0.29440(6) 0.0211(3) Uani 1 1 d . . . . .
H27A H 0.6548 0.3789 0.3036 0.025 Uiso 1 1 calc R U . . .
H27B H 0.6577 0.4814 0.3267 0.025 Uiso 1 1 calc R U . . .
C28 C 0.55485(7) 0.38509(11) 0.22193(6) 0.0197(3) Uani 1 1 d . . . . .
H28A H 0.5593 0.3220 0.2373 0.024 Uiso 1 1 calc R U . . .
H28B H 0.5839 0.3886 0.2041 0.024 Uiso 1 1 calc R U . . .
C29 C 0.48781(7) 0.39637(11) 0.18279(6) 0.0198(3) Uani 1 1 d . . . . .
C30 C 0.47515(8) 0.39681(12) 0.13063(6) 0.0235(3) Uani 1 1 d . . . . .
H30 H 0.5094 0.3934 0.1201 0.028 Uiso 1 1 calc R U . . .
C31 C 0.41315(8) 0.40223(13) 0.09362(6) 0.0268(4) Uani 1 1 d . . . . .
C32 C 0.36483(8) 0.40860(12) 0.11133(6) 0.0248(3) Uani 1 1 d . . . . .
H32 H 0.3223 0.4125 0.0865 0.030 Uiso 1 1 calc R U . . .
C33 C 0.37472(7) 0.40967(10) 0.16285(6) 0.0201(3) Uani 1 1 d . . . . .
C34 C 0.43843(7) 0.40380(10) 0.19959(6) 0.0183(3) Uani 1 1 d . . . . .
C35 C 0.39678(10) 0.39816(16) 0.03582(7) 0.0374(4) Uani 1 1 d . . . . .
C36 C 0.35596(17) 0.48208(19) 0.00876(9) 0.0693(9) Uani 1 1 d . . . . .
H36A H 0.3802 0.5398 0.0213 0.104 Uiso 1 1 calc R U . . .
H36B H 0.3178 0.4836 0.0159 0.104 Uiso 1 1 calc R U . . .
H36C H 0.3437 0.4767 -0.0283 0.104 Uiso 1 1 calc R U . . .
C37 C 0.35758(14) 0.30977(18) 0.01333(9) 0.0572(7) Uani 1 1 d . . . . .
H37A H 0.3469 0.3069 -0.0236 0.086 Uiso 1 1 calc R U . . .
H37B H 0.3184 0.3116 0.0192 0.086 Uiso 1 1 calc R U . . .
H37C H 0.3823 0.2544 0.0301 0.086 Uiso 1 1 calc R U . . .
C38 C 0.45574(14) 0.3919(3) 0.02417(10) 0.0853(12) Uani 1 1 d . . . . .
H38A H 0.4800 0.4501 0.0346 0.128 Uiso 1 1 calc R U . . .
H38B H 0.4430 0.3822 -0.0127 0.128 Uiso 1 1 calc R U . . .
H38C H 0.4821 0.3393 0.0431 0.128 Uiso 1 1 calc R U . . .
C39 C 0.31896(7) 0.40971(11) 0.17947(7) 0.0224(3) Uani 1 1 d . . . . .
C40 C 0.25519(8) 0.42595(15) 0.13413(8) 0.0346(4) Uani 1 1 d . . . . .
H40A H 0.2567 0.4849 0.1171 0.052 Uiso 1 1 calc R U . . .
H40B H 0.2213 0.4290 0.1466 0.052 Uiso 1 1 calc R U . . .
H40C H 0.2467 0.3743 0.1096 0.052 Uiso 1 1 calc R U . . .
C41 C 0.32617(8) 0.48554(12) 0.21973(7) 0.0259(3) Uani 1 1 d . . . . .
H41A H 0.3650 0.4741 0.2505 0.039 Uiso 1 1 calc R U . . .
H41B H 0.2894 0.4837 0.2288 0.039 Uiso 1 1 calc R U . . .
H41C H 0.3287 0.5471 0.2056 0.039 Uiso 1 1 calc R U . . .
C42 C 0.31694(8) 0.31232(12) 0.20172(8) 0.0299(4) Uani 1 1 d . . . . .
H42A H 0.3108 0.2647 0.1754 0.045 Uiso 1 1 calc R U . . .
H42B H 0.2817 0.3096 0.2127 0.045 Uiso 1 1 calc R U . . .
H42C H 0.3570 0.3006 0.2312 0.045 Uiso 1 1 calc R U . . .
C5A C 0.5909(5) 0.4886(7) 0.4554(3) 0.076(2) Uiso 0.4 1 d D . P A 2
H5A1 H 0.5447 0.4950 0.4425 0.114 Uiso 0.4 1 calc R U P A 2
H5A2 H 0.6112 0.5323 0.4838 0.114 Uiso 0.4 1 calc R U P A 2
H5A3 H 0.6031 0.4245 0.4674 0.114 Uiso 0.4 1 calc R U P A 2
C6A C 0.6820(4) 0.5250(6) 0.4377(4) 0.062(3) Uiso 0.4 1 d D . P A 2
H6A1 H 0.6920 0.5723 0.4648 0.094 Uiso 0.4 1 calc R U P A 2
H6A2 H 0.6969 0.5466 0.4118 0.094 Uiso 0.4 1 calc R U P A 2
H6A3 H 0.7032 0.4661 0.4526 0.094 Uiso 0.4 1 calc R U P A 2
C4A C 0.6119(4) 0.5100(10) 0.4132(4) 0.038(4) Uiso 0.4 1 d D . P A 2
H4A H 0.5930 0.5722 0.3993 0.045 Uiso 0.4 1 calc R U 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
Ti1 O1 1.8351(11) . ?
Ti1 O2 1.8537(12) . ?
Ti1 O3 1.8890(12) . ?
Ti1 O4 1.9257(11) . ?
Ti1 N1 2.2038(13) . ?
Ti1 N2 2.3101(13) . ?
O1 C1 1.417(2) . ?
N1 C21 1.282(2) . ?
N1 C22 1.467(2) . ?
C1 C2 1.514(3) . ?
C1 C3 1.517(3) . ?
O2 C4A 1.330(13) . ?
O2 C4 1.440(7) . ?
N2 C27 1.4983(19) . ?
N2 C28 1.5005(19) . ?
N2 C23 1.5042(19) . ?
O3 C7 1.3290(19) . ?
O4 C34 1.3308(19) . ?
C4 C6 1.505(4) . ?
C4 C5 1.506(4) . ?
C7 C8 1.416(2) . ?
C7 C12 1.419(2) . ?
C8 C9 1.399(2) . ?
C8 C21 1.450(2) . ?
C9 C10 1.381(2) . ?
C10 C11 1.395(2) . ?
C10 C13 1.535(2) . ?
C11 C12 1.393(2) . ?
C12 C17 1.539(2) . ?
C13 C15 1.502(4) . ?
C13 C14 1.524(3) . ?
C13 C16 1.552(4) . ?
C17 C19 1.532(3) . ?
C17 C18 1.536(2) . ?
C17 C20 1.539(3) . ?
C22 C23 1.520(2) . ?
C23 C24 1.531(2) . ?
C24 C25 1.527(2) . ?
C25 C26 1.522(2) . ?
C26 C27 1.530(2) . ?
C28 C29 1.505(2) . ?
C29 C30 1.393(2) . ?
C29 C34 1.404(2) . ?
C30 C31 1.394(2) . ?
C31 C32 1.397(3) . ?
C31 C35 1.534(2) . ?
C32 C33 1.391(2) . ?
C33 C34 1.420(2) . ?
C33 C39 1.536(2) . ?
C35 C38 1.524(3) . ?
C35 C36 1.528(3) . ?
C35 C37 1.535(3) . ?
C39 C40 1.533(2) . ?
C39 C41 1.537(2) . ?
C39 C42 1.538(2) . ?
C5A C4A 1.495(5) . ?
C6A C4A 1.495(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O2 92.57(5) . . ?
O1 Ti1 O3 106.21(5) . . ?
O2 Ti1 O3 95.52(5) . . ?
O1 Ti1 O4 92.42(5) . . ?
O2 Ti1 O4 169.64(5) . . ?
O3 Ti1 O4 91.79(5) . . ?
O1 Ti1 N1 169.83(5) . . ?
O2 Ti1 N1 82.94(5) . . ?
O3 Ti1 N1 83.38(5) . . ?
O4 Ti1 N1 90.64(5) . . ?
O1 Ti1 N2 95.47(5) . . ?
O2 Ti1 N2 89.18(5) . . ?
O3 Ti1 N2 157.54(5) . . ?
O4 Ti1 N2 81.30(5) . . ?
N1 Ti1 N2 75.41(5) . . ?
C1 O1 Ti1 132.96(11) . . ?
C21 N1 C22 117.90(13) . . ?
C21 N1 Ti1 126.40(11) . . ?
C22 N1 Ti1 115.07(9) . . ?
O1 C1 C2 109.23(16) . . ?
O1 C1 C3 109.11(16) . . ?
C2 C1 C3 111.11(18) . . ?
C4A O2 Ti1 138.7(5) . . ?
C4 O2 Ti1 138.9(3) . . ?
C27 N2 C28 108.00(11) . . ?
C27 N2 C23 111.53(12) . . ?
C28 N2 C23 110.86(12) . . ?
C27 N2 Ti1 109.91(9) . . ?
C28 N2 Ti1 107.05(9) . . ?
C23 N2 Ti1 109.38(9) . . ?
C7 O3 Ti1 140.17(10) . . ?
C34 O4 Ti1 143.29(10) . . ?
O2 C4 C6 110.1(4) . . ?
O2 C4 C5 106.9(5) . . ?
C6 C4 C5 113.2(4) . . ?
O3 C7 C8 120.18(14) . . ?
O3 C7 C12 120.80(14) . . ?
C8 C7 C12 119.02(14) . . ?
C9 C8 C7 120.17(15) . . ?
C9 C8 C21 116.90(15) . . ?
C7 C8 C21 122.93(14) . . ?
C10 C9 C8 121.87(16) . . ?
C9 C10 C11 116.91(15) . . ?
C9 C10 C13 119.99(16) . . ?
C11 C10 C13 123.08(16) . . ?
C12 C11 C10 124.38(16) . . ?
C11 C12 C7 117.61(15) . . ?
C11 C12 C17 121.25(15) . . ?
C7 C12 C17 121.13(14) . . ?
C15 C13 C14 109.7(2) . . ?
C15 C13 C10 109.64(19) . . ?
C14 C13 C10 112.68(17) . . ?
C15 C13 C16 110.2(3) . . ?
C14 C13 C16 106.36(19) . . ?
C10 C13 C16 108.20(19) . . ?
C19 C17 C18 108.62(15) . . ?
C19 C17 C12 109.02(16) . . ?
C18 C17 C12 112.00(15) . . ?
C19 C17 C20 110.31(18) . . ?
C18 C17 C20 106.23(16) . . ?
C12 C17 C20 110.61(15) . . ?
N1 C21 C8 126.03(15) . . ?
N1 C22 C23 107.48(13) . . ?
N2 C23 C22 108.75(12) . . ?
N2 C23 C24 113.71(13) . . ?
C22 C23 C24 113.63(13) . . ?
C25 C24 C23 112.74(14) . . ?
C26 C25 C24 110.04(14) . . ?
C25 C26 C27 109.93(13) . . ?
N2 C27 C26 114.79(13) . . ?
N2 C28 C29 114.78(12) . . ?
C30 C29 C34 120.81(15) . . ?
C30 C29 C28 120.10(14) . . ?
C34 C29 C28 119.07(14) . . ?
C29 C30 C31 121.13(16) . . ?
C30 C31 C32 116.93(15) . . ?
C30 C31 C35 122.91(17) . . ?
C32 C31 C35 120.13(16) . . ?
C33 C32 C31 124.42(15) . . ?
C32 C33 C34 117.24(15) . . ?
C32 C33 C39 121.49(14) . . ?
C34 C33 C39 121.11(14) . . ?
O4 C34 C29 118.55(14) . . ?
O4 C34 C33 121.99(14) . . ?
C29 C34 C33 119.46(14) . . ?
C38 C35 C36 110.9(2) . . ?
C38 C35 C31 112.32(17) . . ?
C36 C35 C31 110.29(18) . . ?
C38 C35 C37 106.6(2) . . ?
C36 C35 C37 107.3(2) . . ?
C31 C35 C37 109.14(18) . . ?
C40 C39 C33 112.12(14) . . ?
C40 C39 C41 107.46(14) . . ?
C33 C39 C41 112.15(13) . . ?
C40 C39 C42 107.83(14) . . ?
C33 C39 C42 107.09(13) . . ?
C41 C39 C42 110.11(14) . . ?
O2 C4A C6A 112.5(9) . . ?
O2 C4A C5A 119.1(9) . . ?
C6A C4A C5A 107.0(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ti1 O1 C1 9.91(16) . . . . ?
O3 Ti1 O1 C1 -86.60(16) . . . . ?
O4 Ti1 O1 C1 -179.17(15) . . . . ?
N1 Ti1 O1 C1 73.4(4) . . . . ?
N2 Ti1 O1 C1 99.34(15) . . . . ?
Ti1 O1 C1 C2 -138.98(14) . . . . ?
Ti1 O1 C1 C3 99.4(2) . . . . ?
O1 Ti1 O2 C4A -139.5(7) . . . . ?
O3 Ti1 O2 C4A -32.9(7) . . . . ?
O4 Ti1 O2 C4A 101.8(7) . . . . ?
N1 Ti1 O2 C4A 49.7(7) . . . . ?
N2 Ti1 O2 C4A 125.1(7) . . . . ?
O1 Ti1 O2 C4 -130.4(3) . . . . ?
O3 Ti1 O2 C4 -23.9(3) . . . . ?
O4 Ti1 O2 C4 110.8(4) . . . . ?
N1 Ti1 O2 C4 58.7(3) . . . . ?
N2 Ti1 O2 C4 134.1(3) . . . . ?
O1 Ti1 O3 C7 -175.54(16) . . . . ?
O2 Ti1 O3 C7 90.16(17) . . . . ?
O4 Ti1 O3 C7 -82.49(17) . . . . ?
N1 Ti1 O3 C7 7.95(17) . . . . ?
N2 Ti1 O3 C7 -11.2(3) . . . . ?
Ti1 O2 C4 C6 -137.3(3) . . . . ?
Ti1 O2 C4 C5 99.4(5) . . . . ?
Ti1 O3 C7 C8 -11.4(3) . . . . ?
Ti1 O3 C7 C12 169.33(12) . . . . ?
O3 C7 C8 C9 -176.93(15) . . . . ?
C12 C7 C8 C9 2.4(2) . . . . ?
O3 C7 C8 C21 3.2(2) . . . . ?
C12 C7 C8 C21 -177.55(15) . . . . ?
C7 C8 C9 C10 -1.1(3) . . . . ?
C21 C8 C9 C10 178.81(16) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C13 -179.24(18) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C13 C10 C11 C12 179.50(18) . . . . ?
C10 C11 C12 C7 0.5(3) . . . . ?
C10 C11 C12 C17 179.43(17) . . . . ?
O3 C7 C12 C11 177.24(15) . . . . ?
C8 C7 C12 C11 -2.0(2) . . . . ?
O3 C7 C12 C17 -1.7(2) . . . . ?
C8 C7 C12 C17 179.05(15) . . . . ?
C9 C10 C13 C15 -57.3(3) . . . . ?
C11 C10 C13 C15 124.0(3) . . . . ?
C9 C10 C13 C14 -179.70(18) . . . . ?
C11 C10 C13 C14 1.6(3) . . . . ?
C9 C10 C13 C16 63.0(2) . . . . ?
C11 C10 C13 C16 -115.7(2) . . . . ?
C11 C12 C17 C19 -112.67(19) . . . . ?
C7 C12 C17 C19 66.2(2) . . . . ?
C11 C12 C17 C18 7.6(2) . . . . ?
C7 C12 C17 C18 -173.57(16) . . . . ?
C11 C12 C17 C20 125.86(18) . . . . ?
C7 C12 C17 C20 -55.3(2) . . . . ?
C22 N1 C21 C8 -178.48(15) . . . . ?
Ti1 N1 C21 C8 -8.1(2) . . . . ?
C9 C8 C21 N1 -174.01(16) . . . . ?
C7 C8 C21 N1 5.9(3) . . . . ?
C21 N1 C22 C23 -147.23(15) . . . . ?
Ti1 N1 C22 C23 41.30(15) . . . . ?
C27 N2 C23 C22 -80.12(15) . . . . ?
C28 N2 C23 C22 159.49(12) . . . . ?
Ti1 N2 C23 C22 41.68(13) . . . . ?
C27 N2 C23 C24 47.58(17) . . . . ?
C28 N2 C23 C24 -72.81(16) . . . . ?
Ti1 N2 C23 C24 169.38(11) . . . . ?
N1 C22 C23 N2 -54.13(16) . . . . ?
N1 C22 C23 C24 178.12(13) . . . . ?
N2 C23 C24 C25 -50.98(18) . . . . ?
C22 C23 C24 C25 74.16(18) . . . . ?
C23 C24 C25 C26 54.79(19) . . . . ?
C24 C25 C26 C27 -55.93(19) . . . . ?
C28 N2 C27 C26 71.15(16) . . . . ?
C23 N2 C27 C26 -50.91(17) . . . . ?
Ti1 N2 C27 C26 -172.39(11) . . . . ?
C25 C26 C27 N2 55.76(18) . . . . ?
C27 N2 C28 C29 -170.47(13) . . . . ?
C23 N2 C28 C29 -48.00(17) . . . . ?
Ti1 N2 C28 C29 71.22(14) . . . . ?
N2 C28 C29 C30 130.13(16) . . . . ?
N2 C28 C29 C34 -51.6(2) . . . . ?
C34 C29 C30 C31 -1.6(3) . . . . ?
C28 C29 C30 C31 176.61(15) . . . . ?
C29 C30 C31 C32 1.0(3) . . . . ?
C29 C30 C31 C35 -176.96(17) . . . . ?
C30 C31 C32 C33 -0.1(3) . . . . ?
C35 C31 C32 C33 177.85(17) . . . . ?
C31 C32 C33 C34 0.0(2) . . . . ?
C31 C32 C33 C39 -175.54(16) . . . . ?
Ti1 O4 C34 C29 16.2(2) . . . . ?
Ti1 O4 C34 C33 -163.92(12) . . . . ?
C30 C29 C34 O4 -178.68(14) . . . . ?
C28 C29 C34 O4 3.0(2) . . . . ?
C30 C29 C34 C33 1.5(2) . . . . ?
C28 C29 C34 C33 -176.82(14) . . . . ?
C32 C33 C34 O4 179.52(14) . . . . ?
C39 C33 C34 O4 -5.0(2) . . . . ?
C32 C33 C34 C29 -0.6(2) . . . . ?
C39 C33 C34 C29 174.90(14) . . . . ?
C30 C31 C35 C38 -2.5(3) . . . . ?
C32 C31 C35 C38 179.7(2) . . . . ?
C30 C31 C35 C36 -126.8(2) . . . . ?
C32 C31 C35 C36 55.4(3) . . . . ?
C30 C31 C35 C37 115.6(2) . . . . ?
C32 C31 C35 C37 -62.3(2) . . . . ?
C32 C33 C39 C40 -10.1(2) . . . . ?
C34 C33 C39 C40 174.54(15) . . . . ?
C32 C33 C39 C41 -131.13(16) . . . . ?
C34 C33 C39 C41 53.53(19) . . . . ?
C32 C33 C39 C42 107.96(17) . . . . ?
C34 C33 C39 C42 -67.37(18) . . . . ?
Ti1 O2 C4A C6A -161.6(5) . . . . ?
Ti1 O2 C4A C5A 72.0(13) . . . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.048

####################################################################### 
# 
# 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_e16mdj31
_database_code_depnum_ccdc_archive 'CCDC 1534471'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H72 N2 O4 Zr, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H79 N2 O4 Zr'
_chemical_formula_weight         827.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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'

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

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

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

_cell_length_a                   24.0620(6)
_cell_length_b                   15.1035(3)
_cell_length_c                   30.6787(8)
_cell_angle_alpha                90
_cell_angle_beta                 117.531(3)
_cell_angle_gamma                90
_cell_volume                     9886.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1112
_cell_measurement_theta_min      4.3330
_cell_measurement_theta_max      28.8770

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_F_000             3576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.261
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_T_min  0.97992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.975
_oxdiff_exptl_absorpt_empirical_full_max 1.018
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 16.1468
_diffrn_reflns_number            41135
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         3.326
_diffrn_reflns_theta_max         29.558
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12003
_reflns_number_gt                9671
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
both O-tBu groups show rotational disorder in the ratio 70:30. 
Atoms therein were refined with bond length and ADP restraints.
Additional disorder in one tBu-group in the ratio 80:20.
Atoms therein were refined with bond length and ADP restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+13.6260P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12003
_refine_ls_number_parameters     617
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0913
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.005
_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
Zr1 Zr 0.31497(2) 0.37175(2) 0.34777(2) 0.02036(6) Uani 1 1 d . . . . .
O1 O 0.33007(7) 0.49782(9) 0.35922(6) 0.0342(3) Uani 1 1 d . . . . .
N1 N 0.29796(7) 0.22142(10) 0.32717(6) 0.0237(3) Uani 1 1 d . . . . .
O2 O 0.39664(6) 0.33259(10) 0.39875(5) 0.0336(3) Uani 1 1 d . . . . .
N2 N 0.35147(7) 0.34240(10) 0.28714(6) 0.0239(3) Uani 1 1 d . . . . .
O3 O 0.26304(6) 0.33456(9) 0.38091(5) 0.0264(3) Uani 1 1 d . . . . .
O4 O 0.23519(6) 0.39109(9) 0.28147(5) 0.0251(3) Uani 1 1 d . . . . .
C1 C 0.3350(3) 0.5916(4) 0.3638(2) 0.0323(10) Uani 0.674(4) 1 d . . P A 1
C2 C 0.3182(2) 0.6332(3) 0.31463(19) 0.0669(14) Uani 0.674(4) 1 d . . P A 1
H2A H 0.3497 0.6170 0.3042 0.100 Uiso 0.674(4) 1 calc R U P A 1
H2B H 0.3171 0.6977 0.3174 0.100 Uiso 0.674(4) 1 calc R U P A 1
H2C H 0.2770 0.6119 0.2903 0.100 Uiso 0.674(4) 1 calc R U P A 1
C3 C 0.2887(2) 0.6202(3) 0.3824(2) 0.0606(14) Uani 0.674(4) 1 d . . P A 1
H3A H 0.2463 0.6017 0.3588 0.091 Uiso 0.674(4) 1 calc R U P A 1
H3B H 0.2900 0.6847 0.3860 0.091 Uiso 0.674(4) 1 calc R U P A 1
H3C H 0.3003 0.5924 0.4143 0.091 Uiso 0.674(4) 1 calc R U P A 1
C4 C 0.4024(4) 0.6124(9) 0.4010(4) 0.073(3) Uani 0.674(4) 1 d . . P A 1
H4A H 0.4108 0.5888 0.4332 0.109 Uiso 0.674(4) 1 calc R U P A 1
H4B H 0.4086 0.6767 0.4033 0.109 Uiso 0.674(4) 1 calc R U P A 1
H4C H 0.4311 0.5851 0.3904 0.109 Uiso 0.674(4) 1 calc R U P A 1
C5 C 0.4482(3) 0.3043(4) 0.4420(2) 0.0442(14) Uani 0.674(4) 1 d . U P A 1
C6 C 0.4672(3) 0.2128(4) 0.4340(3) 0.122(3) Uani 0.674(4) 1 d . U P A 1
H6A H 0.4324 0.1716 0.4258 0.182 Uiso 0.674(4) 1 calc R U P A 1
H6B H 0.5036 0.1930 0.4640 0.182 Uiso 0.674(4) 1 calc R U P A 1
H6C H 0.4781 0.2146 0.4069 0.182 Uiso 0.674(4) 1 calc R U P A 1
C7 C 0.5028(2) 0.3656(4) 0.45207(19) 0.0693(15) Uani 0.674(4) 1 d . U P A 1
H7A H 0.5147 0.3596 0.4257 0.104 Uiso 0.674(4) 1 calc R U P A 1
H7B H 0.5385 0.3497 0.4835 0.104 Uiso 0.674(4) 1 calc R U P A 1
H7C H 0.4905 0.4269 0.4535 0.104 Uiso 0.674(4) 1 calc R U P A 1
C8 C 0.4308(4) 0.3158(8) 0.4829(3) 0.132(3) Uani 0.674(4) 1 d . U P A 1
H8A H 0.4251 0.3789 0.4872 0.197 Uiso 0.674(4) 1 calc R U P A 1
H8B H 0.4643 0.2920 0.5135 0.197 Uiso 0.674(4) 1 calc R U P A 1
H8C H 0.3917 0.2840 0.4748 0.197 Uiso 0.674(4) 1 calc R U P A 1
C1A C 0.3409(6) 0.5806(9) 0.3808(4) 0.037(3) Uani 0.326(4) 1 d D U P A 2
C2A C 0.3448(5) 0.5809(7) 0.4318(3) 0.067(3) Uani 0.326(4) 1 d D U P A 2
H2D H 0.3046 0.5614 0.4295 0.100 Uiso 0.326(4) 1 calc R U P A 2
H2E H 0.3541 0.6410 0.4454 0.100 Uiso 0.326(4) 1 calc R U P A 2
H2F H 0.3780 0.5406 0.4533 0.100 Uiso 0.326(4) 1 calc R U P A 2
C3A C 0.2874(6) 0.6377(9) 0.3486(6) 0.103(5) Uani 0.326(4) 1 d D U P A 2
H3D H 0.2852 0.6412 0.3159 0.154 Uiso 0.326(4) 1 calc R U P A 2
H3E H 0.2934 0.6972 0.3628 0.154 Uiso 0.326(4) 1 calc R U P A 2
H3F H 0.2484 0.6124 0.3458 0.154 Uiso 0.326(4) 1 calc R U P A 2
C4A C 0.4010(10) 0.6162(17) 0.3850(7) 0.057(5) Uani 0.326(4) 1 d D U P A 2
H4D H 0.4353 0.5755 0.4047 0.085 Uiso 0.326(4) 1 calc R U P A 2
H4E H 0.4094 0.6743 0.4009 0.085 Uiso 0.326(4) 1 calc R U P A 2
H4F H 0.3979 0.6220 0.3521 0.085 Uiso 0.326(4) 1 calc R U P A 2
C5A C 0.4448(5) 0.3299(6) 0.4494(4) 0.025(2) Uani 0.326(4) 1 d D U P A 2
C6A C 0.5048(4) 0.2999(9) 0.4488(4) 0.067(3) Uani 0.326(4) 1 d D U P A 2
H6D H 0.4994 0.2394 0.4359 0.101 Uiso 0.326(4) 1 calc R U P A 2
H6E H 0.5395 0.3013 0.4823 0.101 Uiso 0.326(4) 1 calc R U P A 2
H6F H 0.5141 0.3396 0.4277 0.101 Uiso 0.326(4) 1 calc R U P A 2
C7A C 0.4553(6) 0.4186(7) 0.4730(4) 0.081(3) Uani 0.326(4) 1 d D U P A 2
H7D H 0.4610 0.4626 0.4519 0.122 Uiso 0.326(4) 1 calc R U P A 2
H7E H 0.4929 0.4169 0.5049 0.122 Uiso 0.326(4) 1 calc R U P A 2
H7F H 0.4190 0.4348 0.4776 0.122 Uiso 0.326(4) 1 calc R U P A 2
C8A C 0.4253(6) 0.2650(6) 0.4766(4) 0.054(3) Uani 0.326(4) 1 d D U P A 2
H8D H 0.3862 0.2851 0.4760 0.081 Uiso 0.326(4) 1 calc R U P A 2
H8E H 0.4581 0.2606 0.5107 0.081 Uiso 0.326(4) 1 calc R U P A 2
H8F H 0.4187 0.2068 0.4608 0.081 Uiso 0.326(4) 1 calc R U P A 2
C9 C 0.22298(8) 0.27182(13) 0.37865(7) 0.0238(4) Uani 1 1 d . . . . .
C10 C 0.18259(9) 0.28589(14) 0.40028(7) 0.0287(4) Uani 1 1 d . . . . .
C11 C 0.13966(10) 0.21981(14) 0.39449(8) 0.0327(5) Uani 1 1 d . . . . .
H11 H 0.1123 0.2291 0.4086 0.039 Uiso 1 1 calc R U . . .
C12 C 0.13397(9) 0.14039(13) 0.36932(8) 0.0313(4) Uani 1 1 d . . . . .
C13 C 0.17498(9) 0.12698(13) 0.35036(8) 0.0287(4) Uani 1 1 d . . . . .
H13 H 0.1733 0.0729 0.3340 0.034 Uiso 1 1 calc R U . . .
C14 C 0.21957(9) 0.19135(12) 0.35461(7) 0.0248(4) Uani 1 1 d . . . . .
C15 C 0.18569(11) 0.37190(16) 0.42795(9) 0.0404(5) Uani 1 1 d . . . . .
C16 C 0.16794(13) 0.45063(16) 0.39275(11) 0.0515(7) Uani 1 1 d . . . . .
H16A H 0.1700 0.5053 0.4107 0.077 Uiso 1 1 calc R U . . .
H16B H 0.1972 0.4546 0.3788 0.077 Uiso 1 1 calc R U . . .
H16C H 0.1252 0.4425 0.3662 0.077 Uiso 1 1 calc R U . . .
C17 C 0.25200(13) 0.3851(2) 0.47068(9) 0.0538(7) Uani 1 1 d . . . . .
H17A H 0.2630 0.3344 0.4931 0.081 Uiso 1 1 calc R U . . .
H17B H 0.2821 0.3900 0.4576 0.081 Uiso 1 1 calc R U . . .
H17C H 0.2530 0.4394 0.4885 0.081 Uiso 1 1 calc R U . . .
C18 C 0.13949(14) 0.3708(2) 0.44978(12) 0.0650(9) Uani 1 1 d . . . . .
H18A H 0.1494 0.3209 0.4726 0.097 Uiso 1 1 calc R U . . .
H18B H 0.1430 0.4263 0.4674 0.097 Uiso 1 1 calc R U . . .
H18C H 0.0966 0.3643 0.4232 0.097 Uiso 1 1 calc R U . . .
C19 C 0.08289(11) 0.07336(15) 0.36333(10) 0.0423(6) Uani 1 1 d . . . . .
C20 C 0.08590(17) -0.0088(2) 0.33681(18) 0.0993(16) Uani 1 1 d . . . . .
H20A H 0.0816 0.0073 0.3045 0.149 Uiso 1 1 calc R U . . .
H20B H 0.1263 -0.0384 0.3560 0.149 Uiso 1 1 calc R U . . .
H20C H 0.0518 -0.0490 0.3327 0.149 Uiso 1 1 calc R U . . .
C21 C 0.0896(2) 0.0479(3) 0.41307(15) 0.0987(14) Uani 1 1 d . . . . .
H21A H 0.0876 0.1013 0.4305 0.148 Uiso 1 1 calc R U . . .
H21B H 0.0555 0.0077 0.4089 0.148 Uiso 1 1 calc R U . . .
H21C H 0.1299 0.0183 0.4321 0.148 Uiso 1 1 calc R U . . .
C22 C 0.01896(14) 0.1172(2) 0.33364(16) 0.0815(11) Uani 1 1 d . . . . .
H22A H 0.0165 0.1708 0.3506 0.122 Uiso 1 1 calc R U . . .
H22B H 0.0136 0.1328 0.3009 0.122 Uiso 1 1 calc R U . . .
H22C H -0.0142 0.0759 0.3304 0.122 Uiso 1 1 calc R U . . .
C23 C 0.25940(9) 0.16922(12) 0.33224(7) 0.0254(4) Uani 1 1 d . . . . .
H23 H 0.2566 0.1105 0.3202 0.030 Uiso 1 1 calc R U . . .
C24 C 0.33422(9) 0.18753(13) 0.30324(8) 0.0279(4) Uani 1 1 d . . . . .
H24A H 0.3180 0.1289 0.2883 0.033 Uiso 1 1 calc R U . . .
H24B H 0.3789 0.1810 0.3276 0.033 Uiso 1 1 calc R U . . .
C25 C 0.32751(9) 0.25386(12) 0.26366(7) 0.0255(4) Uani 1 1 d . . . . .
H25 H 0.2816 0.2610 0.2415 0.031 Uiso 1 1 calc R U . . .
C26 C 0.35681(10) 0.22288(15) 0.23130(8) 0.0337(5) Uani 1 1 d . . . . .
H26A H 0.3425 0.1618 0.2198 0.040 Uiso 1 1 calc R U . . .
H26B H 0.3420 0.2616 0.2020 0.040 Uiso 1 1 calc R U . . .
C27 C 0.42837(10) 0.22447(16) 0.25836(10) 0.0409(5) Uani 1 1 d . . . . .
H27A H 0.4439 0.1812 0.2857 0.049 Uiso 1 1 calc R U . . .
H27B H 0.4452 0.2078 0.2355 0.049 Uiso 1 1 calc R U . . .
C28 C 0.45072(10) 0.31708(16) 0.27854(9) 0.0381(5) Uani 1 1 d . . . . .
H28A H 0.4386 0.3594 0.2510 0.046 Uiso 1 1 calc R U . . .
H28B H 0.4970 0.3175 0.2978 0.046 Uiso 1 1 calc R U . . .
C29 C 0.42177(9) 0.34567(14) 0.31129(8) 0.0299(4) Uani 1 1 d . . . . .
H29A H 0.4384 0.3071 0.3407 0.036 Uiso 1 1 calc R U . . .
H29B H 0.4354 0.4070 0.3226 0.036 Uiso 1 1 calc R U . . .
C30 C 0.32627(9) 0.41624(13) 0.25035(7) 0.0285(4) Uani 1 1 d . . . . .
H30A H 0.3498 0.4171 0.2311 0.034 Uiso 1 1 calc R U . . .
H30B H 0.3346 0.4730 0.2684 0.034 Uiso 1 1 calc R U . . .
C31 C 0.25748(9) 0.41136(13) 0.21512(7) 0.0277(4) Uani 1 1 d . . . . .
C32 C 0.21389(9) 0.40163(12) 0.23342(7) 0.0254(4) Uani 1 1 d . . . . .
C33 C 0.14891(9) 0.40118(13) 0.19975(8) 0.0304(4) Uani 1 1 d . . . . .
C34 C 0.13230(11) 0.41223(14) 0.14982(8) 0.0372(5) Uani 1 1 d . . . . .
H34 H 0.0889 0.4135 0.1271 0.045 Uiso 1 1 calc R U . . .
C35 C 0.17499(11) 0.42150(14) 0.13135(8) 0.0368(5) Uani 1 1 d . . . . .
C36 C 0.23797(11) 0.41968(13) 0.16494(8) 0.0337(5) Uani 1 1 d . . . . .
H36 H 0.2685 0.4242 0.1535 0.040 Uiso 1 1 calc R U . . .
C37 C 0.09945(9) 0.39073(15) 0.21772(8) 0.0368(5) Uani 1 1 d . . . . .
C38 C 0.10864(11) 0.30256(17) 0.24496(10) 0.0453(6) Uani 1 1 d . . . . .
H38A H 0.1510 0.3002 0.2726 0.068 Uiso 1 1 calc R U . . .
H38B H 0.1029 0.2535 0.2224 0.068 Uiso 1 1 calc R U . . .
H38C H 0.0778 0.2976 0.2574 0.068 Uiso 1 1 calc R U . . .
C39 C 0.10513(12) 0.46780(18) 0.25222(11) 0.0512(6) Uani 1 1 d . . . . .
H39A H 0.1476 0.4690 0.2797 0.077 Uiso 1 1 calc R U . . .
H39B H 0.0748 0.4598 0.2648 0.077 Uiso 1 1 calc R U . . .
H39C H 0.0966 0.5238 0.2341 0.077 Uiso 1 1 calc R U . . .
C40 C 0.03238(11) 0.3910(2) 0.17505(11) 0.0583(7) Uani 1 1 d . . . . .
H40A H 0.0024 0.3828 0.1881 0.087 Uiso 1 1 calc R U . . .
H40B H 0.0278 0.3427 0.1523 0.087 Uiso 1 1 calc R U . . .
H40C H 0.0242 0.4477 0.1576 0.087 Uiso 1 1 calc R U . . .
C41 C 0.1539(2) 0.4337(3) 0.07549(19) 0.0382(9) Uani 0.834(5) 1 d . U P B 1
C42 C 0.1144(2) 0.3547(3) 0.04779(14) 0.0670(13) Uani 0.834(5) 1 d . . P B 1
H42A H 0.0782 0.3498 0.0541 0.101 Uiso 0.834(5) 1 calc R U P B 1
H42B H 0.1397 0.3007 0.0589 0.101 Uiso 0.834(5) 1 calc R U P B 1
H42C H 0.0999 0.3627 0.0125 0.101 Uiso 0.834(5) 1 calc R U P B 1
C43 C 0.11473(19) 0.5193(2) 0.05950(12) 0.0599(11) Uani 0.834(5) 1 d . . P B 1
H43A H 0.1410 0.5698 0.0773 0.090 Uiso 0.834(5) 1 calc R U P B 1
H43B H 0.0794 0.5146 0.0670 0.090 Uiso 0.834(5) 1 calc R U P B 1
H43C H 0.0988 0.5279 0.0241 0.090 Uiso 0.834(5) 1 calc R U P B 1
C44 C 0.20827(16) 0.4437(2) 0.06349(11) 0.0515(9) Uani 0.834(5) 1 d . . P B 1
H44A H 0.2339 0.4947 0.0813 0.077 Uiso 0.834(5) 1 calc R U P B 1
H44B H 0.2340 0.3900 0.0734 0.077 Uiso 0.834(5) 1 calc R U P B 1
H44C H 0.1919 0.4530 0.0281 0.077 Uiso 0.834(5) 1 calc R U P B 1
C41A C 0.1383(10) 0.4365(15) 0.0786(13) 0.050(8) Uani 0.166(5) 1 d D U P B 2
C42A C 0.1541(14) 0.3534(18) 0.0559(8) 0.080(7) Uani 0.166(5) 1 d D U P B 2
H42D H 0.1992 0.3418 0.0736 0.120 Uiso 0.166(5) 1 calc R U P B 2
H42E H 0.1416 0.3644 0.0212 0.120 Uiso 0.166(5) 1 calc R U P B 2
H42F H 0.1312 0.3020 0.0589 0.120 Uiso 0.166(5) 1 calc R U P B 2
C43A C 0.0674(8) 0.4504(13) 0.0479(5) 0.057(5) Uani 0.166(5) 1 d D U P B 2
H43D H 0.0453 0.3962 0.0485 0.086 Uiso 0.166(5) 1 calc R U P B 2
H43E H 0.0575 0.4644 0.0139 0.086 Uiso 0.166(5) 1 calc R U P B 2
H43F H 0.0540 0.4995 0.0618 0.086 Uiso 0.166(5) 1 calc R U P B 2
C44A C 0.1713(12) 0.5140(17) 0.0663(7) 0.087(8) Uani 0.166(5) 1 d D U P B 2
H44D H 0.1486 0.5271 0.0310 0.131 Uiso 0.166(5) 1 calc R U P B 2
H44E H 0.1716 0.5666 0.0851 0.131 Uiso 0.166(5) 1 calc R U P B 2
H44F H 0.2145 0.4970 0.0750 0.131 Uiso 0.166(5) 1 calc R U P B 2
C45 C 0.6242(3) 0.2320(4) 0.3985(2) 0.136(2) Uani 1 1 d . . . . .
H45A H 0.6138 0.1712 0.4032 0.204 Uiso 1 1 calc R U . . .
H45B H 0.6462 0.2315 0.3784 0.204 Uiso 1 1 calc R U . . .
H45C H 0.5856 0.2667 0.3818 0.204 Uiso 1 1 calc R U . . .
C46 C 0.6665(3) 0.2737(4) 0.4487(2) 0.127(2) Uani 1 1 d . . . . .
H46A H 0.6726 0.3371 0.4438 0.152 Uiso 1 1 calc R U . . .
H46B H 0.6448 0.2706 0.4693 0.152 Uiso 1 1 calc R U . . .
C47 C 0.7277(2) 0.2317(3) 0.47504(15) 0.1044(17) Uani 1 1 d . . . . .
H47A H 0.7488 0.2349 0.4540 0.125 Uiso 1 1 calc R U . . .
H47B H 0.7209 0.1683 0.4791 0.125 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
Zr1 O1 1.9398(14) . ?
Zr1 O2 1.9535(14) . ?
Zr1 O3 2.0209(12) . ?
Zr1 O4 2.0731(13) . ?
Zr1 N1 2.3417(16) . ?
Zr1 N2 2.4371(15) . ?
O1 C1A 1.382(14) . ?
O1 C1 1.423(6) . ?
N1 C23 1.281(2) . ?
N1 C24 1.468(2) . ?
O2 C5 1.401(7) . ?
O2 C5A 1.447(12) . ?
N2 C30 1.501(3) . ?
N2 C29 1.501(2) . ?
N2 C25 1.502(2) . ?
O3 C9 1.331(2) . ?
O4 C32 1.328(2) . ?
C1 C2 1.506(7) . ?
C1 C4 1.523(9) . ?
C1 C3 1.529(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C8 1.504(9) . ?
C5 C6 1.511(9) . ?
C5 C7 1.519(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C1A C3A 1.483(12) . ?
C1A C4A 1.493(14) . ?
C1A C2A 1.524(11) . ?
C2A H2D 0.9800 . ?
C2A H2E 0.9800 . ?
C2A H2F 0.9800 . ?
C3A H3D 0.9800 . ?
C3A H3E 0.9800 . ?
C3A H3F 0.9800 . ?
C4A H4D 0.9800 . ?
C4A H4E 0.9800 . ?
C4A H4F 0.9800 . ?
C5A C7A 1.488(10) . ?
C5A C8A 1.497(12) . ?
C5A C6A 1.521(11) . ?
C6A H6D 0.9800 . ?
C6A H6E 0.9800 . ?
C6A H6F 0.9800 . ?
C7A H7D 0.9800 . ?
C7A H7E 0.9800 . ?
C7A H7F 0.9800 . ?
C8A H8D 0.9800 . ?
C8A H8E 0.9800 . ?
C8A H8F 0.9800 . ?
C9 C14 1.404(3) . ?
C9 C10 1.423(3) . ?
C10 C11 1.387(3) . ?
C10 C15 1.535(3) . ?
C11 C12 1.399(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(3) . ?
C12 C19 1.536(3) . ?
C13 C14 1.409(3) . ?
C13 H13 0.9500 . ?
C14 C23 1.452(3) . ?
C15 C16 1.528(4) . ?
C15 C17 1.540(3) . ?
C15 C18 1.540(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.504(4) . ?
C19 C21 1.508(4) . ?
C19 C22 1.529(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 0.9500 . ?
C24 C25 1.524(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.533(3) . ?
C25 H25 1.0000 . ?
C26 C27 1.527(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.523(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.526(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.503(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.392(3) . ?
C31 C32 1.407(3) . ?
C32 C33 1.421(3) . ?
C33 C34 1.403(3) . ?
C33 C37 1.534(3) . ?
C34 C35 1.391(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(3) . ?
C35 C41A 1.46(4) . ?
C35 C41 1.557(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.533(3) . ?
C37 C39 1.536(3) . ?
C37 C40 1.538(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.516(6) . ?
C41 C44 1.522(7) . ?
C41 C43 1.540(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C41A C43A 1.54(2) . ?
C41A C44A 1.56(2) . ?
C41A C42A 1.56(2) . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C43A H43D 0.9800 . ?
C43A H43E 0.9800 . ?
C43A H43F 0.9800 . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?
C45 C46 1.534(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.459(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C47 1.511(9) 7_656 ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?

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 Zr1 O2 96.74(7) . . ?
O1 Zr1 O3 106.83(6) . . ?
O2 Zr1 O3 98.07(6) . . ?
O1 Zr1 O4 92.88(6) . . ?
O2 Zr1 O4 163.88(6) . . ?
O3 Zr1 O4 91.45(5) . . ?
O1 Zr1 N1 174.48(6) . . ?
O2 Zr1 N1 84.73(6) . . ?
O3 Zr1 N1 78.16(5) . . ?
O4 Zr1 N1 84.53(5) . . ?
O1 Zr1 N2 102.31(6) . . ?
O2 Zr1 N2 88.38(6) . . ?
O3 Zr1 N2 149.11(5) . . ?
O4 Zr1 N2 76.92(5) . . ?
N1 Zr1 N2 72.37(5) . . ?
C1A O1 Zr1 162.3(4) . . ?
C1 O1 Zr1 174.3(3) . . ?
C23 N1 C24 118.53(16) . . ?
C23 N1 Zr1 127.60(13) . . ?
C24 N1 Zr1 113.77(11) . . ?
C5 O2 Zr1 166.8(3) . . ?
C5A O2 Zr1 151.4(4) . . ?
C30 N2 C29 108.55(14) . . ?
C30 N2 C25 111.65(15) . . ?
C29 N2 C25 111.17(15) . . ?
C30 N2 Zr1 106.02(11) . . ?
C29 N2 Zr1 109.79(11) . . ?
C25 N2 Zr1 109.52(10) . . ?
C9 O3 Zr1 140.65(12) . . ?
C32 O4 Zr1 144.43(12) . . ?
O1 C1 C2 110.2(4) . . ?
O1 C1 C4 106.9(6) . . ?
C2 C1 C4 111.3(5) . . ?
O1 C1 C3 106.0(4) . . ?
C2 C1 C3 110.6(5) . . ?
C4 C1 C3 111.6(6) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C5 C8 106.9(5) . . ?
O2 C5 C6 109.1(5) . . ?
C8 C5 C6 117.7(7) . . ?
O2 C5 C7 108.1(5) . . ?
C8 C5 C7 108.0(6) . . ?
C6 C5 C7 106.9(6) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C1A C3A 107.1(9) . . ?
O1 C1A C4A 109.1(13) . . ?
C3A C1A C4A 110.9(14) . . ?
O1 C1A C2A 113.8(8) . . ?
C3A C1A C2A 107.7(12) . . ?
C4A C1A C2A 108.3(11) . . ?
C1A C2A H2D 109.5 . . ?
C1A C2A H2E 109.5 . . ?
H2D C2A H2E 109.5 . . ?
C1A C2A H2F 109.5 . . ?
H2D C2A H2F 109.5 . . ?
H2E C2A H2F 109.5 . . ?
C1A C3A H3D 109.5 . . ?
C1A C3A H3E 109.5 . . ?
H3D C3A H3E 109.5 . . ?
C1A C3A H3F 109.5 . . ?
H3D C3A H3F 109.5 . . ?
H3E C3A H3F 109.5 . . ?
C1A C4A H4D 109.5 . . ?
C1A C4A H4E 109.5 . . ?
H4D C4A H4E 109.5 . . ?
C1A C4A H4F 109.5 . . ?
H4D C4A H4F 109.5 . . ?
H4E C4A H4F 109.5 . . ?
O2 C5A C7A 111.6(7) . . ?
O2 C5A C8A 108.4(8) . . ?
C7A C5A C8A 110.2(9) . . ?
O2 C5A C6A 106.8(7) . . ?
C7A C5A C6A 109.0(10) . . ?
C8A C5A C6A 110.9(10) . . ?
C5A C6A H6D 109.5 . . ?
C5A C6A H6E 109.5 . . ?
H6D C6A H6E 109.5 . . ?
C5A C6A H6F 109.5 . . ?
H6D C6A H6F 109.5 . . ?
H6E C6A H6F 109.5 . . ?
C5A C7A H7D 109.5 . . ?
C5A C7A H7E 109.5 . . ?
H7D C7A H7E 109.5 . . ?
C5A C7A H7F 109.5 . . ?
H7D C7A H7F 109.5 . . ?
H7E C7A H7F 109.5 . . ?
C5A C8A H8D 109.5 . . ?
C5A C8A H8E 109.5 . . ?
H8D C8A H8E 109.5 . . ?
C5A C8A H8F 109.5 . . ?
H8D C8A H8F 109.5 . . ?
H8E C8A H8F 109.5 . . ?
O3 C9 C14 120.58(16) . . ?
O3 C9 C10 120.25(17) . . ?
C14 C9 C10 119.17(16) . . ?
C11 C10 C9 117.46(18) . . ?
C11 C10 C15 121.53(17) . . ?
C9 C10 C15 121.00(17) . . ?
C10 C11 C12 124.39(18) . . ?
C10 C11 H11 117.8 . . ?
C12 C11 H11 117.8 . . ?
C13 C12 C11 117.02(18) . . ?
C13 C12 C19 122.97(19) . . ?
C11 C12 C19 120.00(18) . . ?
C12 C13 C14 121.68(19) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
C9 C14 C13 120.19(17) . . ?
C9 C14 C23 123.81(16) . . ?
C13 C14 C23 115.99(17) . . ?
C16 C15 C10 109.97(19) . . ?
C16 C15 C17 110.0(2) . . ?
C10 C15 C17 110.3(2) . . ?
C16 C15 C18 107.1(2) . . ?
C10 C15 C18 111.75(18) . . ?
C17 C15 C18 107.7(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 C21 109.1(3) . . ?
C20 C19 C22 108.8(3) . . ?
C21 C19 C22 108.7(3) . . ?
C20 C19 C12 111.88(19) . . ?
C21 C19 C12 110.0(2) . . ?
C22 C19 C12 108.4(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C23 C14 126.09(18) . . ?
N1 C23 H23 117.0 . . ?
C14 C23 H23 117.0 . . ?
N1 C24 C25 107.50(15) . . ?
N1 C24 H24A 110.2 . . ?
C25 C24 H24A 110.2 . . ?
N1 C24 H24B 110.2 . . ?
C25 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
N2 C25 C24 109.12(15) . . ?
N2 C25 C26 113.14(15) . . ?
C24 C25 C26 113.85(16) . . ?
N2 C25 H25 106.8 . . ?
C24 C25 H25 106.8 . . ?
C26 C25 H25 106.8 . . ?
C27 C26 C25 112.56(17) . . ?
C27 C26 H26A 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 109.44(18) . . ?
C28 C27 H27A 109.8 . . ?
C26 C27 H27A 109.8 . . ?
C28 C27 H27B 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
C27 C28 C29 110.15(17) . . ?
C27 C28 H28A 109.6 . . ?
C29 C28 H28A 109.6 . . ?
C27 C28 H28B 109.6 . . ?
C29 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
N2 C29 C28 114.75(17) . . ?
N2 C29 H29A 108.6 . . ?
C28 C29 H29A 108.6 . . ?
N2 C29 H29B 108.6 . . ?
C28 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
N2 C30 C31 115.60(15) . . ?
N2 C30 H30A 108.4 . . ?
C31 C30 H30A 108.4 . . ?
N2 C30 H30B 108.4 . . ?
C31 C30 H30B 108.4 . . ?
H30A C30 H30B 107.4 . . ?
C36 C31 C32 121.21(19) . . ?
C36 C31 C30 119.15(18) . . ?
C32 C31 C30 119.61(17) . . ?
O4 C32 C31 118.63(17) . . ?
O4 C32 C33 122.47(17) . . ?
C31 C32 C33 118.88(18) . . ?
C34 C33 C32 117.09(19) . . ?
C34 C33 C37 121.88(19) . . ?
C32 C33 C37 121.02(18) . . ?
C35 C34 C33 124.5(2) . . ?
C35 C34 H34 117.8 . . ?
C33 C34 H34 117.8 . . ?
C36 C35 C34 117.1(2) . . ?
C36 C35 C41A 136.2(8) . . ?
C34 C35 C41A 106.6(8) . . ?
C36 C35 C41 120.6(3) . . ?
C34 C35 C41 122.3(3) . . ?
C35 C36 C31 121.2(2) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
C38 C37 C33 110.19(18) . . ?
C38 C37 C39 109.8(2) . . ?
C33 C37 C39 109.45(18) . . ?
C38 C37 C40 107.24(19) . . ?
C33 C37 C40 112.2(2) . . ?
C39 C37 C40 108.0(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C44 109.2(4) . . ?
C42 C41 C43 110.4(4) . . ?
C44 C41 C43 107.9(4) . . ?
C42 C41 C35 109.0(4) . . ?
C44 C41 C35 113.5(3) . . ?
C43 C41 C35 106.9(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C35 C41A C43A 129.1(19) . . ?
C35 C41A C44A 105.7(16) . . ?
C43A C41A C44A 107(2) . . ?
C35 C41A C42A 102.8(17) . . ?
C43A C41A C42A 106(2) . . ?
C44A C41A C42A 104(2) . . ?
C41A C42A H42D 109.5 . . ?
C41A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
C41A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
C41A C43A H43D 109.5 . . ?
C41A C43A H43E 109.5 . . ?
H43D C43A H43E 109.5 . . ?
C41A C43A H43F 109.5 . . ?
H43D C43A H43F 109.5 . . ?
H43E C43A H43F 109.5 . . ?
C41A C44A H44D 109.5 . . ?
C41A C44A H44E 109.5 . . ?
H44D C44A H44E 109.5 . . ?
C41A C44A H44F 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C45 114.1(5) . . ?
C47 C46 H46A 108.7 . . ?
C45 C46 H46A 108.7 . . ?
C47 C46 H46B 108.7 . . ?
C45 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
C46 C47 C47 117.7(5) . 7_656 ?
C46 C47 H47A 107.9 . . ?
C47 C47 H47A 107.9 7_656 . ?
C46 C47 H47B 107.9 . . ?
C47 C47 H47B 107.9 7_656 . ?
H47A C47 H47B 107.2 . . ?

_refine_diff_density_max         0.688
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_s15mdj32
_database_code_depnum_ccdc_archive 'CCDC 1534473'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H66 Mg N4 O2, 2(C7 H8)'
_chemical_formula_sum            'C56 H82 Mg N4 O2'
_chemical_formula_weight         867.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 '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                   10.6847(9)
_cell_length_b                   26.0458(7)
_cell_length_c                   19.3381(11)
_cell_angle_alpha                90
_cell_angle_beta                 100.316(7)
_cell_angle_gamma                90
_cell_volume                     5294.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18604
_cell_measurement_theta_min      4.1080
_cell_measurement_theta_max      71.8140

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_F_000             1896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.604
_shelx_estimated_absorpt_T_min   0.889
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_T_min  0.81271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            42079
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.876
_diffrn_reflns_theta_max         72.004
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10345
_reflns_number_gt                9303
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
The asymmetric unit consists of one Mg complex and two toluene solvent molecules.
Disorder in the complex: -one t-Bu group in the ratio 55:45 refined with bond length restraint.
-Atom C19 disordered over two sites in the ratio 88:12.
-diorder in one Cyclohexyl ring in the ratio 52:48
The N-H hydrogen atom was refined with bond legth restraint.
One of the solevnt molecules is disordered over three sites in the ratio 50:30:20. 
All atoms of the minor parts have been anisotropically refined with ADP restraints.
Bond length restraint for all three Methyl-to-Phenylring atoms.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²+3.8275P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10345
_refine_ls_number_parameters     800
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1828
_refine_ls_wR_factor_gt          0.1784
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg1 Mg 0.41024(7) 0.41931(2) 0.80117(3) 0.03280(17) Uani 1 1 d . . . . .
O1 O 0.57328(14) 0.38030(6) 0.81093(7) 0.0373(3) Uani 1 1 d . . . . .
N1 N 0.4580(2) 0.42852(7) 0.91254(9) 0.0424(4) Uani 1 1 d . . . . .
C1 C 0.6662(2) 0.36955(7) 0.86174(10) 0.0335(4) Uani 1 1 d . . . . .
O2 O 0.45053(14) 0.49113(5) 0.78076(7) 0.0349(3) Uani 1 1 d . . . . .
N2 N 0.2257(2) 0.45310(8) 0.83127(10) 0.0468(5) Uani 1 1 d . . . . .
H2 H 0.253(4) 0.4876(15) 0.8253(19) 0.088(11) Uiso 1 1 d . . . . .
C2 C 0.7731(2) 0.33933(8) 0.85025(11) 0.0373(4) Uani 1 1 d . . . . .
C3 C 0.8682(2) 0.32804(9) 0.90675(12) 0.0417(5) Uani 1 1 d . . . . .
H3 H 0.9379 0.3079 0.8980 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8688(2) 0.34428(8) 0.97616(11) 0.0419(5) Uani 1 1 d . . . . .
C5 C 0.7676(2) 0.37331(8) 0.98654(11) 0.0430(5) Uani 1 1 d . . . . .
H5 H 0.7654 0.3854 1.0326 0.052 Uiso 1 1 calc R U . . .
C6 C 0.6663(2) 0.38618(7) 0.93226(10) 0.0379(5) Uani 1 1 d . . . . .
C7 C 0.7778(2) 0.31796(11) 0.77667(12) 0.0483(6) Uani 1 1 d . . . . .
C8 C 0.9025(2) 0.28968(14) 0.77366(15) 0.0653(8) Uani 1 1 d . . . . .
H8A H 0.9745 0.3127 0.7896 0.098 Uiso 1 1 calc R U . . .
H8B H 0.9035 0.2789 0.7252 0.098 Uiso 1 1 calc R U . . .
H8C H 0.9091 0.2594 0.8042 0.098 Uiso 1 1 calc R U . . .
C9 C 0.7672(3) 0.36119(15) 0.72270(14) 0.0709(9) Uani 1 1 d . . . . .
H9A H 0.8387 0.3849 0.7355 0.106 Uiso 1 1 calc R U . . .
H9B H 0.6871 0.3797 0.7218 0.106 Uiso 1 1 calc R U . . .
H9C H 0.7689 0.3467 0.6761 0.106 Uiso 1 1 calc R U . . .
C10 C 0.6698(3) 0.27902(13) 0.75629(17) 0.0698(9) Uani 1 1 d . . . . .
H10A H 0.6723 0.2653 0.7094 0.105 Uiso 1 1 calc R U . . .
H10B H 0.5878 0.2960 0.7561 0.105 Uiso 1 1 calc R U . . .
H10C H 0.6801 0.2508 0.7904 0.105 Uiso 1 1 calc R U . . .
C11 C 0.9749(3) 0.32706(10) 1.03565(12) 0.0527(6) Uani 1 1 d D . . . .
C12 C 0.9641(11) 0.2684(2) 1.0436(5) 0.057(2) Uani 0.55(2) 1 d D . P A 1
H12A H 1.0291 0.2566 1.0827 0.086 Uiso 0.55(2) 1 calc R U P A 1
H12B H 0.9769 0.2516 1.0000 0.086 Uiso 0.55(2) 1 calc R U P A 1
H12C H 0.8795 0.2598 1.0531 0.086 Uiso 0.55(2) 1 calc R U P A 1
C13 C 1.0995(10) 0.3402(9) 1.0164(8) 0.120(7) Uani 0.55(2) 1 d D . P A 1
H13A H 1.1036 0.3261 0.9699 0.180 Uiso 0.55(2) 1 calc R U P A 1
H13B H 1.1682 0.3255 1.0512 0.180 Uiso 0.55(2) 1 calc R U P A 1
H13C H 1.1090 0.3776 1.0155 0.180 Uiso 0.55(2) 1 calc R U P A 1
C14 C 0.9580(15) 0.3480(4) 1.1078(4) 0.092(4) Uani 0.55(2) 1 d D . P A 1
H14A H 0.8748 0.3375 1.1176 0.138 Uiso 0.55(2) 1 calc R U P A 1
H14B H 0.9633 0.3855 1.1076 0.138 Uiso 0.55(2) 1 calc R U P A 1
H14C H 1.0252 0.3342 1.1443 0.138 Uiso 0.55(2) 1 calc R U P A 1
C12A C 0.9374(19) 0.2765(7) 1.0624(13) 0.135(9) Uani 0.45(2) 1 d D . P A 2
H12D H 0.8977 0.2551 1.0228 0.203 Uiso 0.45(2) 1 calc R U P A 2
H12E H 0.8768 0.2821 1.0942 0.203 Uiso 0.45(2) 1 calc R U P A 2
H12F H 1.0131 0.2590 1.0879 0.203 Uiso 0.45(2) 1 calc R U P A 2
C13A C 1.1072(11) 0.3241(8) 1.0160(8) 0.078(4) Uani 0.45(2) 1 d D . P A 2
H13D H 1.1697 0.3147 1.0576 0.117 Uiso 0.45(2) 1 calc R U P A 2
H13E H 1.1295 0.3576 0.9986 0.117 Uiso 0.45(2) 1 calc R U P A 2
H13F H 1.1071 0.2982 0.9793 0.117 Uiso 0.45(2) 1 calc R U P A 2
C14A C 0.998(2) 0.3698(10) 1.0922(11) 0.129(9) Uani 0.45(2) 1 d D . P A 2
H14D H 0.9244 0.3721 1.1159 0.193 Uiso 0.45(2) 1 calc R U P A 2
H14E H 1.0101 0.4027 1.0698 0.193 Uiso 0.45(2) 1 calc R U P A 2
H14F H 1.0742 0.3616 1.1268 0.193 Uiso 0.45(2) 1 calc R U P A 2
C15 C 0.5623(3) 0.41473(8) 0.95201(10) 0.0434(5) Uani 1 1 d . . . . .
H15 H 0.5723 0.4245 1.0000 0.052 Uiso 1 1 calc R U . . .
C16 C 0.3679(3) 0.45940(11) 0.94362(12) 0.0589(7) Uani 1 1 d . . . . .
H16A H 0.3881 0.4963 0.9397 0.071 Uiso 1 1 calc R U . . .
H16B H 0.3761 0.4509 0.9941 0.071 Uiso 1 1 calc R U . . .
C17 C 0.2347(3) 0.44956(10) 0.90732(13) 0.0562(7) Uani 1 1 d . . . . .
H17 H 0.2150 0.4131 0.9178 0.067 Uiso 1 1 calc R U . . .
C18 C 0.1373(3) 0.48276(12) 0.93533(15) 0.0642(8) Uani 1 1 d . . . . .
H18A H 0.1589 0.5194 0.9306 0.077 Uiso 0.883(13) 1 calc R U P B 1
H18B H 0.1414 0.4754 0.9859 0.077 Uiso 0.883(13) 1 calc R U P B 1
H18C H 0.0919 0.4612 0.9650 0.077 Uiso 0.117(13) 1 calc R U P B 2
H18D H 0.1829 0.5100 0.9656 0.077 Uiso 0.117(13) 1 calc R U P B 2
C19 C 0.0021(4) 0.47305(19) 0.8961(2) 0.0738(14) Uani 0.883(13) 1 d . . P B 1
H19A H -0.0252 0.4380 0.9067 0.089 Uiso 0.883(13) 1 calc R U P B 1
H19B H -0.0569 0.4979 0.9118 0.089 Uiso 0.883(13) 1 calc R U P B 1
C19A C 0.044(4) 0.507(2) 0.881(2) 0.101(19) Uani 0.117(13) 1 d . U P B 2
H19C H -0.0301 0.5164 0.9021 0.122 Uiso 0.117(13) 1 calc R U P B 2
H19D H 0.0819 0.5391 0.8670 0.122 Uiso 0.117(13) 1 calc R U P B 2
C20 C -0.0024(3) 0.47862(13) 0.81754(18) 0.0686(8) Uani 1 1 d . . . . .
H20A H 0.0120 0.5150 0.8064 0.082 Uiso 0.883(13) 1 calc R U P B 1
H20B H -0.0878 0.4687 0.7922 0.082 Uiso 0.883(13) 1 calc R U P B 1
H20C H -0.0365 0.5033 0.7799 0.082 Uiso 0.117(13) 1 calc R U P B 2
H20D H -0.0735 0.4564 0.8257 0.082 Uiso 0.117(13) 1 calc R U P B 2
C21 C 0.0975(3) 0.44540(13) 0.79243(17) 0.0670(8) Uani 1 1 d . . . . .
H21A H 0.0740 0.4089 0.7963 0.080 Uiso 1 1 calc R U . . .
H21B H 0.0968 0.4528 0.7421 0.080 Uiso 1 1 calc R U . . .
C22 C 0.45373(18) 0.51803(7) 0.72479(9) 0.0294(4) Uani 1 1 d . . . . .
C23 C 0.50417(19) 0.56933(8) 0.72939(10) 0.0317(4) Uani 1 1 d . . . . .
C24 C 0.5002(2) 0.59717(8) 0.66859(10) 0.0349(4) Uani 1 1 d . . . . .
H24 H 0.5326 0.6312 0.6728 0.042 Uiso 1 1 calc R U . . .
C25 C 0.4514(2) 0.57885(8) 0.60045(10) 0.0359(4) Uani 1 1 d . . . . .
C26 C 0.4068(2) 0.52943(8) 0.59596(10) 0.0364(4) Uani 1 1 d . . . . .
H26 H 0.3748 0.5155 0.5509 0.044 Uiso 1 1 calc R U . . .
C27 C 0.40677(19) 0.49845(8) 0.65601(10) 0.0330(4) Uani 1 1 d . . . . .
C28 C 0.5595(2) 0.59216(8) 0.80158(11) 0.0404(5) Uani 1 1 d . . . . .
C29 C 0.6686(3) 0.55825(10) 0.83921(13) 0.0559(7) Uani 1 1 d . . . . .
H29A H 0.7010 0.5724 0.8859 0.084 Uiso 1 1 calc R U . . .
H29B H 0.7372 0.5574 0.8117 0.084 Uiso 1 1 calc R U . . .
H29C H 0.6370 0.5233 0.8440 0.084 Uiso 1 1 calc R U . . .
C30 C 0.4539(3) 0.59628(10) 0.84589(12) 0.0540(6) Uani 1 1 d . . . . .
H30A H 0.3832 0.6166 0.8204 0.081 Uiso 1 1 calc R U . . .
H30B H 0.4877 0.6130 0.8907 0.081 Uiso 1 1 calc R U . . .
H30C H 0.4234 0.5618 0.8548 0.081 Uiso 1 1 calc R U . . .
C31 C 0.6130(3) 0.64629(10) 0.79565(13) 0.0542(6) Uani 1 1 d . . . . .
H31A H 0.5441 0.6695 0.7751 0.081 Uiso 1 1 calc R U . . .
H31B H 0.6777 0.6453 0.7656 0.081 Uiso 1 1 calc R U . . .
H31C H 0.6515 0.6587 0.8425 0.081 Uiso 1 1 calc R U . . .
C32 C 0.4514(2) 0.61441(9) 0.53737(11) 0.0453(5) Uani 1 1 d . . . . .
C33 C 0.3725(3) 0.66224(11) 0.54618(15) 0.0629(7) Uani 1 1 d . . . . .
H33A H 0.4119 0.6809 0.5885 0.094 Uiso 1 1 calc R U . . .
H33B H 0.2861 0.6519 0.5506 0.094 Uiso 1 1 calc R U . . .
H33C H 0.3689 0.6845 0.5050 0.094 Uiso 1 1 calc R U . . .
C34 C 0.5879(3) 0.63012(11) 0.53320(13) 0.0560(6) Uani 1 1 d . . . . .
H34A H 0.6247 0.6490 0.5758 0.084 Uiso 1 1 calc R U . . .
H34B H 0.5875 0.6521 0.4920 0.084 Uiso 1 1 calc R U . . .
H34C H 0.6388 0.5993 0.5291 0.084 Uiso 1 1 calc R U . . .
C35 C 0.3929(3) 0.58823(12) 0.46824(12) 0.0613(7) Uani 1 1 d . . . . .
H35A H 0.3951 0.6119 0.4290 0.092 Uiso 1 1 calc R U . . .
H35B H 0.3046 0.5788 0.4696 0.092 Uiso 1 1 calc R U . . .
H35C H 0.4417 0.5572 0.4619 0.092 Uiso 1 1 calc R U . . .
C36 C 0.3567(3) 0.44734(9) 0.64379(11) 0.0466(6) Uani 1 1 d . . . . .
H36 H 0.3119 0.4397 0.5979 0.056 Uiso 1 1 calc R U . C 1
N3 N 0.3677(6) 0.4097(3) 0.6914(5) 0.0320(13) Uani 0.523(7) 1 d . . P D 1
N4 N 0.3408(6) 0.3374(3) 0.7906(4) 0.0336(13) Uani 0.523(7) 1 d D . P D 1
H4 H 0.418(2) 0.3243(16) 0.794(2) 0.031(11) Uiso 0.523(7) 1 d D . P D 1
C37 C 0.3391(5) 0.35708(16) 0.6670(2) 0.0391(13) Uani 0.523(7) 1 d . . P D 1
H37A H 0.4191 0.3391 0.6628 0.047 Uiso 0.523(7) 1 calc R U P D 1
H37B H 0.2840 0.3577 0.6201 0.047 Uiso 0.523(7) 1 calc R U P D 1
C38 C 0.2715(12) 0.3281(8) 0.7190(11) 0.036(3) Uani 0.523(7) 1 d . . P D 1
H38 H 0.1832 0.3419 0.7151 0.043 Uiso 0.523(7) 1 calc R U P D 1
C39 C 0.2636(10) 0.2694(5) 0.7019(8) 0.047(2) Uani 0.523(7) 1 d . . P D 1
H39A H 0.2099 0.2642 0.6552 0.056 Uiso 0.523(7) 1 calc R U P D 1
H39B H 0.3499 0.2564 0.6998 0.056 Uiso 0.523(7) 1 calc R U P D 1
C40 C 0.2106(7) 0.2400(2) 0.7544(4) 0.0615(18) Uani 0.523(7) 1 d . . P D 1
H40A H 0.1193 0.2484 0.7509 0.074 Uiso 0.523(7) 1 calc R U P D 1
H40B H 0.2180 0.2028 0.7454 0.074 Uiso 0.523(7) 1 calc R U P D 1
C41 C 0.2786(13) 0.2523(5) 0.8243(9) 0.063(6) Uani 0.523(7) 1 d . . P D 1
H41A H 0.3665 0.2390 0.8290 0.075 Uiso 0.523(7) 1 calc R U P D 1
H41B H 0.2373 0.2339 0.8590 0.075 Uiso 0.523(7) 1 calc R U P D 1
C42 C 0.2852(8) 0.3091(3) 0.8430(4) 0.0525(17) Uani 0.523(7) 1 d . . P D 1
H42A H 0.1987 0.3223 0.8442 0.063 Uiso 0.523(7) 1 calc R U P D 1
H42B H 0.3379 0.3140 0.8902 0.063 Uiso 0.523(7) 1 calc R U P D 1
N3A N 0.3240(7) 0.4169(4) 0.6888(5) 0.0325(14) Uani 0.477(7) 1 d . . P D 2
N4A N 0.2943(7) 0.3443(3) 0.7870(4) 0.0319(14) Uani 0.477(7) 1 d D . P D 2
H4A H 0.212(2) 0.348(2) 0.785(3) 0.047(16) Uiso 0.477(7) 1 d D . P D 2
C37A C 0.2527(5) 0.37012(18) 0.6654(2) 0.0363(13) Uani 0.477(7) 1 d . . P D 2
H37C H 0.2630 0.3617 0.6168 0.044 Uiso 0.477(7) 1 calc R U P D 2
H37D H 0.1611 0.3757 0.6654 0.044 Uiso 0.477(7) 1 calc R U P D 2
C38A C 0.3009(13) 0.3259(8) 0.7140(10) 0.030(2) Uani 0.477(7) 1 d . . P D 2
H38A H 0.3922 0.3198 0.7111 0.036 Uiso 0.477(7) 1 calc R U P D 2
C39A C 0.2295(12) 0.2782(6) 0.6940(8) 0.047(2) Uani 0.477(7) 1 d . . P D 2
H39C H 0.2422 0.2671 0.6468 0.056 Uiso 0.477(7) 1 calc R U P D 2
H39D H 0.1375 0.2842 0.6922 0.056 Uiso 0.477(7) 1 calc R U P D 2
C40A C 0.2772(8) 0.2353(2) 0.7491(4) 0.0543(17) Uani 0.477(7) 1 d . . P D 2
H40C H 0.3656 0.2260 0.7453 0.065 Uiso 0.477(7) 1 calc R U P D 2
H40D H 0.2237 0.2044 0.7375 0.065 Uiso 0.477(7) 1 calc R U P D 2
C41A C 0.2736(15) 0.2516(4) 0.8270(9) 0.055(6) Uani 0.477(7) 1 d . . P D 2
H41C H 0.1844 0.2543 0.8343 0.066 Uiso 0.477(7) 1 calc R U P D 2
H41D H 0.3177 0.2256 0.8601 0.066 Uiso 0.477(7) 1 calc R U P D 2
C42A C 0.3408(7) 0.3039(3) 0.8399(4) 0.0425(15) Uani 0.477(7) 1 d . . P D 2
H42C H 0.3305 0.3166 0.8868 0.051 Uiso 0.477(7) 1 calc R U P D 2
H42D H 0.4329 0.2988 0.8409 0.051 Uiso 0.477(7) 1 calc R U P D 2
C43 C 0.0188(7) 0.3891(2) 0.5155(4) 0.170(3) Uani 1 1 d . . . . .
H43A H 0.0114 0.4023 0.5621 0.255 Uiso 1 1 calc R U . . .
H43B H -0.0533 0.4013 0.4808 0.255 Uiso 1 1 calc R U . . .
H43C H 0.0984 0.4013 0.5028 0.255 Uiso 1 1 calc R U . . .
C44 C 0.0187(3) 0.33237(13) 0.5169(2) 0.0760(9) Uani 1 1 d . . . . .
C45 C 0.0892(3) 0.3020(2) 0.47415(19) 0.0923(13) Uani 1 1 d . . . . .
H45 H 0.1372 0.3183 0.4435 0.111 Uiso 1 1 calc R U . . .
C46 C 0.0858(4) 0.24885(15) 0.47836(19) 0.0803(10) Uani 1 1 d . . . . .
H46 H 0.1328 0.2282 0.4516 0.096 Uiso 1 1 calc R U . . .
C47 C 0.0161(4) 0.22787(17) 0.5202(2) 0.0904(11) Uani 1 1 d . . . . .
H47 H 0.0132 0.1915 0.5225 0.109 Uiso 1 1 calc R U . . .
C48 C -0.0501(4) 0.2543(2) 0.5593(2) 0.0999(13) Uani 1 1 d . . . . .
H48 H -0.0990 0.2369 0.5886 0.120 Uiso 1 1 calc R U . . .
C49 C -0.0481(4) 0.30552(18) 0.5577(2) 0.0844(10) Uani 1 1 d . . . . .
H49 H -0.0959 0.3239 0.5865 0.101 Uiso 1 1 calc R U . . .
C51 C -0.0911(4) 0.54035(13) 0.6499(2) 0.0544(15) Uani 0.5 1 d DG . P E 1
C52 C -0.1317(3) 0.58420(17) 0.6804(2) 0.0460(13) Uani 0.5 1 d G . P E 1
H52 H -0.2194 0.5888 0.6818 0.055 Uiso 0.5 1 calc R U P E 1
C53 C -0.0440(6) 0.62132(15) 0.7089(3) 0.071(2) Uani 0.5 1 d G . P E 1
H53 H -0.0717 0.6513 0.7297 0.085 Uiso 0.5 1 calc R U P E 1
C54 C 0.0844(5) 0.6146(2) 0.7069(4) 0.083(4) Uani 0.5 1 d G . P E 1
H54 H 0.1444 0.6400 0.7263 0.099 Uiso 0.5 1 calc R U P E 1
C55 C 0.1250(3) 0.5707(2) 0.6764(4) 0.083(3) Uani 0.5 1 d G . P E 1
H55 H 0.2127 0.5662 0.6750 0.100 Uiso 0.5 1 calc R U P E 1
C56 C 0.0373(5) 0.53362(18) 0.6479(3) 0.079(3) Uani 0.5 1 d G . P E 1
H56 H 0.0650 0.5037 0.6270 0.095 Uiso 0.5 1 calc R U P E 1
C57 C -0.1852(14) 0.5014(5) 0.6181(9) 0.172(8) Uani 0.5 1 d D . P E 1
H57A H -0.1484 0.4670 0.6266 0.258 Uiso 0.5 1 calc R U P E 1
H57B H -0.2079 0.5074 0.5674 0.258 Uiso 0.5 1 calc R U P E 1
H57C H -0.2617 0.5040 0.6394 0.258 Uiso 0.5 1 calc R U P E 1
C61 C 0.0323(10) 0.5726(5) 0.6657(6) 0.083(4) Uani 0.3 1 d DG U P F 2
C62 C 0.0256(14) 0.5252(5) 0.6323(8) 0.207(17) Uani 0.3 1 d G U P F 2
H62 H 0.0988 0.5114 0.6175 0.248 Uiso 0.3 1 calc R U P F 2
C63 C -0.0881(18) 0.4979(5) 0.6206(10) 0.161(9) Uani 0.3 1 d G U P F 2
H63 H -0.0927 0.4655 0.5978 0.193 Uiso 0.3 1 calc R U P F 2
C64 C -0.1951(13) 0.5181(7) 0.6423(11) 0.142(10) Uani 0.3 1 d G U P F 2
H64 H -0.2728 0.4995 0.6343 0.170 Uiso 0.3 1 calc R U P F 2
C65 C -0.1884(11) 0.5656(7) 0.6757(10) 0.215(15) Uani 0.3 1 d G U P F 2
H65 H -0.2615 0.5794 0.6906 0.257 Uiso 0.3 1 calc R U P F 2
C66 C -0.0747(14) 0.5928(5) 0.6874(7) 0.089(5) Uani 0.3 1 d G U P F 2
H66 H -0.0701 0.6252 0.7103 0.107 Uiso 0.3 1 calc R U P F 2
C67 C 0.1467(18) 0.6004(8) 0.6902(13) 0.118(7) Uani 0.3 1 d D U P F 2
H67A H 0.1478 0.6117 0.7387 0.177 Uiso 0.3 1 calc R U P F 2
H67B H 0.1506 0.6305 0.6602 0.177 Uiso 0.3 1 calc R U P F 2
H67C H 0.2202 0.5782 0.6887 0.177 Uiso 0.3 1 calc R U P F 2
C71 C 0.0038(17) 0.5730(7) 0.6713(10) 0.32(4) Uani 0.2 1 d DG U P G 3
C72 C 0.0834(13) 0.5527(8) 0.6287(12) 0.098(7) Uani 0.2 1 d G U P G 3
H72 H 0.1719 0.5602 0.6383 0.118 Uiso 0.2 1 calc R U P G 3
C73 C 0.0336(19) 0.5215(8) 0.5721(11) 0.193(17) Uani 0.2 1 d G U P G 3
H73 H 0.0881 0.5077 0.5430 0.231 Uiso 0.2 1 calc R U P G 3
C74 C -0.096(2) 0.5106(7) 0.5581(9) 0.118(8) Uani 0.2 1 d G U P G 3
H74 H -0.1298 0.4893 0.5194 0.141 Uiso 0.2 1 calc R U P G 3
C75 C -0.1754(14) 0.5309(7) 0.6007(9) 0.109(8) Uani 0.2 1 d G U P G 3
H75 H -0.2638 0.5234 0.5911 0.131 Uiso 0.2 1 calc R U P G 3
C76 C -0.1256(16) 0.5621(7) 0.6573(8) 0.063(5) Uani 0.2 1 d G U P G 3
H76 H -0.1800 0.5759 0.6864 0.076 Uiso 0.2 1 calc R U P G 3
C77 C 0.038(2) 0.6206(10) 0.7100(15) 0.079(7) Uani 0.2 1 d D U P G 3
H77A H -0.0265 0.6283 0.7390 0.119 Uiso 0.2 1 calc R U P G 3
H77B H 0.0409 0.6487 0.6768 0.119 Uiso 0.2 1 calc R U P G 3
H77C H 0.1210 0.6167 0.7403 0.119 Uiso 0.2 1 calc R U P G 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
Mg1 O2 1.9751(15) . ?
Mg1 O1 1.9963(16) . ?
Mg1 N3 2.105(9) . ?
Mg1 N1 2.1359(18) . ?
Mg1 N3A 2.205(9) . ?
Mg1 N4 2.257(7) . ?
Mg1 N4A 2.304(8) . ?
Mg1 N2 2.326(2) . ?
O1 C1 1.296(3) . ?
N1 C15 1.284(3) . ?
N1 C16 1.464(3) . ?
C1 C6 1.431(3) . ?
C1 C2 1.437(3) . ?
O2 C22 1.295(2) . ?
N2 C21 1.454(4) . ?
N2 C17 1.460(3) . ?
N2 H2 0.96(4) . ?
C2 C3 1.384(3) . ?
C2 C7 1.537(3) . ?
C3 C4 1.406(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(4) . ?
C4 C11 1.531(3) . ?
C5 C6 1.407(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.444(3) . ?
C7 C9 1.526(4) . ?
C7 C8 1.532(3) . ?
C7 C10 1.534(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.485(10) . ?
C11 C12A 1.497(11) . ?
C11 C13A 1.529(9) . ?
C11 C14 1.539(8) . ?
C11 C12 1.541(7) . ?
C11 C14A 1.549(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C15 H15 0.9500 . ?
C16 C17 1.493(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.525(3) . ?
C17 H17 1.0000 . ?
C18 C19A 1.46(4) . ?
C18 C19 1.528(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C19 C20 1.518(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19A C20 1.44(4) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C20 C21 1.519(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 H20C 0.9900 . ?
C20 H20D 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.429(3) . ?
C22 C23 1.438(3) . ?
C23 C24 1.375(3) . ?
C23 C28 1.535(3) . ?
C24 C25 1.411(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.370(3) . ?
C25 C32 1.532(3) . ?
C26 C27 1.414(3) . ?
C26 H26 0.9500 . ?
C27 C36 1.439(3) . ?
C28 C31 1.534(3) . ?
C28 C29 1.538(3) . ?
C28 C30 1.538(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C34 1.530(4) . ?
C32 C35 1.531(3) . ?
C32 C33 1.531(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N3A 1.272(10) . ?
C36 N3 1.337(9) . ?
C36 H36 0.9500 . ?
N3 C37 1.463(10) . ?
N4 C42 1.462(11) . ?
N4 C38 1.47(2) . ?
N4 H4 0.885(19) . ?
C37 C38 1.537(19) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.56(2) . ?
C38 H38 1.0000 . ?
C39 C40 1.463(17) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.452(17) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.522(16) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
N3A C37A 1.464(10) . ?
N4A C42A 1.488(11) . ?
N4A C38A 1.50(2) . ?
N4A H4A 0.88(2) . ?
C37A C38A 1.52(2) . ?
C37A H37C 0.9900 . ?
C37A H37D 0.9900 . ?
C38A C39A 1.47(3) . ?
C38A H38A 1.0000 . ?
C39A C40A 1.564(14) . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C40A C41A 1.573(18) . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
C41A C42A 1.541(14) . ?
C41A H41C 0.9900 . ?
C41A H41D 0.9900 . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C43 C44 1.477(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C49 1.350(5) . ?
C44 C45 1.450(6) . ?
C45 C46 1.386(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.314(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.317(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.336(6) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C51 C52 1.3900 . ?
C51 C56 1.3900 . ?
C51 C57 1.482(10) . ?
C52 C53 1.3900 . ?
C52 H52 0.9500 . ?
C53 C54 1.3900 . ?
C53 H53 0.9500 . ?
C54 C55 1.3900 . ?
C54 H54 0.9500 . ?
C55 C56 1.3900 . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C61 C67 1.426(15) . ?
C62 C63 1.3900 . ?
C62 H62 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63 0.9500 . ?
C64 C65 1.3900 . ?
C64 H64 0.9500 . ?
C65 C66 1.3900 . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C71 C72 1.3900 . ?
C71 C76 1.3900 . ?
C71 C77 1.460(17) . ?
C72 C73 1.3900 . ?
C72 H72 0.9500 . ?
C73 C74 1.3900 . ?
C73 H73 0.9500 . ?
C74 C75 1.3900 . ?
C74 H74 0.9500 . ?
C75 C76 1.3900 . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mg1 O1 106.45(7) . . ?
O2 Mg1 N3 85.8(3) . . ?
O1 Mg1 N3 93.55(17) . . ?
O2 Mg1 N1 94.23(7) . . ?
O1 Mg1 N1 85.11(7) . . ?
N3 Mg1 N1 178.62(18) . . ?
O2 Mg1 N3A 84.1(3) . . ?
O1 Mg1 N3A 106.38(19) . . ?
N1 Mg1 N3A 168.4(2) . . ?
O2 Mg1 N4 163.2(2) . . ?
O1 Mg1 N4 78.14(17) . . ?
N3 Mg1 N4 77.7(3) . . ?
N1 Mg1 N4 102.3(2) . . ?
O2 Mg1 N4A 155.72(19) . . ?
O1 Mg1 N4A 91.21(18) . . ?
N1 Mg1 N4A 104.0(2) . . ?
N3A Mg1 N4A 74.8(3) . . ?
O2 Mg1 N2 85.21(7) . . ?
O1 Mg1 N2 158.95(7) . . ?
N3 Mg1 N2 104.93(17) . . ?
N1 Mg1 N2 76.45(8) . . ?
N3A Mg1 N2 91.97(19) . . ?
N4 Mg1 N2 95.78(17) . . ?
N4A Mg1 N2 83.61(19) . . ?
C1 O1 Mg1 135.93(13) . . ?
C15 N1 C16 118.30(19) . . ?
C15 N1 Mg1 126.40(15) . . ?
C16 N1 Mg1 114.81(15) . . ?
O1 C1 C6 121.82(19) . . ?
O1 C1 C2 121.55(17) . . ?
C6 C1 C2 116.62(19) . . ?
C22 O2 Mg1 135.96(12) . . ?
C21 N2 C17 113.4(2) . . ?
C21 N2 Mg1 125.54(16) . . ?
C17 N2 Mg1 108.81(16) . . ?
C21 N2 H2 110(2) . . ?
C17 N2 H2 102(2) . . ?
Mg1 N2 H2 92(2) . . ?
C3 C2 C1 119.07(19) . . ?
C3 C2 C7 120.9(2) . . ?
C1 C2 C7 120.01(19) . . ?
C2 C3 C4 124.6(2) . . ?
C2 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
C5 C4 C3 116.0(2) . . ?
C5 C4 C11 123.5(2) . . ?
C3 C4 C11 120.4(2) . . ?
C4 C5 C6 123.1(2) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 C15 116.81(18) . . ?
C1 C6 C15 122.6(2) . . ?
C9 C7 C8 106.7(2) . . ?
C9 C7 C10 110.6(2) . . ?
C8 C7 C10 107.0(2) . . ?
C9 C7 C2 110.8(2) . . ?
C8 C7 C2 112.45(19) . . ?
C10 C7 C2 109.2(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12A C11 C13A 111.0(11) . . ?
C13 C11 C4 108.7(6) . . ?
C12A C11 C4 108.1(7) . . ?
C13A C11 C4 114.9(6) . . ?
C13 C11 C14 113.7(8) . . ?
C4 C11 C14 112.8(5) . . ?
C13 C11 C12 109.8(9) . . ?
C4 C11 C12 107.9(5) . . ?
C14 C11 C12 103.7(5) . . ?
C12A C11 C14A 114.0(11) . . ?
C13A C11 C14A 100.0(12) . . ?
C4 C11 C14A 108.9(6) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C12A H12D 109.5 . . ?
C11 C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C11 C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C11 C13A H13D 109.5 . . ?
C11 C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
C11 C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C11 C14A H14D 109.5 . . ?
C11 C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
C11 C14A H14F 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
N1 C15 C6 127.85(18) . . ?
N1 C15 H15 116.1 . . ?
C6 C15 H15 116.1 . . ?
N1 C16 C17 110.8(2) . . ?
N1 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
N2 C17 C16 110.4(2) . . ?
N2 C17 C18 113.3(2) . . ?
C16 C17 C18 112.9(2) . . ?
N2 C17 H17 106.6 . . ?
C16 C17 H17 106.6 . . ?
C18 C17 H17 106.6 . . ?
C19A C18 C17 114.0(12) . . ?
C17 C18 C19 112.0(3) . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C19A C18 H18C 108.7 . . ?
C17 C18 H18C 108.7 . . ?
C19A C18 H18D 108.7 . . ?
C17 C18 H18D 108.7 . . ?
H18C C18 H18D 107.6 . . ?
C20 C19 C18 109.8(3) . . ?
C20 C19 H19A 109.7 . . ?
C18 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C20 C19A C18 119(3) . . ?
C20 C19A H19C 107.6 . . ?
C18 C19A H19C 107.6 . . ?
C20 C19A H19D 107.6 . . ?
C18 C19A H19D 107.6 . . ?
H19C C19A H19D 107.0 . . ?
C19A C20 C21 114.0(12) . . ?
C19 C20 C21 111.5(3) . . ?
C19 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
C19 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C19A C20 H20C 108.8 . . ?
C21 C20 H20C 108.7 . . ?
C19A C20 H20D 108.7 . . ?
C21 C20 H20D 108.7 . . ?
H20C C20 H20D 107.6 . . ?
N2 C21 C20 114.0(2) . . ?
N2 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
N2 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
O2 C22 C27 121.84(18) . . ?
O2 C22 C23 121.12(16) . . ?
C27 C22 C23 117.04(17) . . ?
C24 C23 C22 118.88(17) . . ?
C24 C23 C28 121.42(18) . . ?
C22 C23 C28 119.69(17) . . ?
C23 C24 C25 124.7(2) . . ?
C23 C24 H24 117.6 . . ?
C25 C24 H24 117.6 . . ?
C26 C25 C24 116.31(18) . . ?
C26 C25 C32 124.57(19) . . ?
C24 C25 C32 119.1(2) . . ?
C25 C26 C27 122.37(18) . . ?
C25 C26 H26 118.8 . . ?
C27 C26 H26 118.8 . . ?
C26 C27 C22 120.60(19) . . ?
C26 C27 C36 116.61(18) . . ?
C22 C27 C36 122.79(18) . . ?
C31 C28 C23 112.09(18) . . ?
C31 C28 C29 107.6(2) . . ?
C23 C28 C29 110.10(18) . . ?
C31 C28 C30 107.4(2) . . ?
C23 C28 C30 109.41(19) . . ?
C29 C28 C30 110.2(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C32 C35 108.5(2) . . ?
C34 C32 C33 109.7(2) . . ?
C35 C32 C33 108.2(2) . . ?
C34 C32 C25 109.87(19) . . ?
C35 C32 C25 111.6(2) . . ?
C33 C32 C25 108.95(19) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3A C36 C27 127.2(5) . . ?
N3 C36 C27 125.6(4) . . ?
N3 C36 H36 117.2 . . ?
C27 C36 H36 117.2 . . ?
C36 N3 C37 118.5(6) . . ?
C36 N3 Mg1 125.7(5) . . ?
C37 N3 Mg1 115.6(5) . . ?
C42 N4 C38 111.8(10) . . ?
C42 N4 Mg1 125.6(5) . . ?
C38 N4 Mg1 110.1(9) . . ?
C42 N4 H4 104(3) . . ?
C38 N4 H4 109(3) . . ?
Mg1 N4 H4 94(3) . . ?
N3 C37 C38 110.1(8) . . ?
N3 C37 H37A 109.6 . . ?
C38 C37 H37A 109.6 . . ?
N3 C37 H37B 109.6 . . ?
C38 C37 H37B 109.6 . . ?
H37A C37 H37B 108.1 . . ?
N4 C38 C37 108.6(11) . . ?
N4 C38 C39 111.1(14) . . ?
C37 C38 C39 110.9(12) . . ?
N4 C38 H38 108.7 . . ?
C37 C38 H38 108.7 . . ?
C39 C38 H38 108.7 . . ?
C40 C39 C38 112.2(11) . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C41 C40 C39 109.8(9) . . ?
C41 C40 H40A 109.7 . . ?
C39 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C39 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
C40 C41 C42 115.5(10) . . ?
C40 C41 H41A 108.4 . . ?
C42 C41 H41A 108.4 . . ?
C40 C41 H41B 108.4 . . ?
C42 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
N4 C42 C41 109.4(9) . . ?
N4 C42 H42A 109.8 . . ?
C41 C42 H42A 109.8 . . ?
N4 C42 H42B 109.8 . . ?
C41 C42 H42B 109.8 . . ?
H42A C42 H42B 108.2 . . ?
C36 N3A C37A 119.9(7) . . ?
C36 N3A Mg1 122.6(6) . . ?
C37A N3A Mg1 115.6(6) . . ?
C42A N4A C38A 110.8(10) . . ?
C42A N4A Mg1 114.3(5) . . ?
C38A N4A Mg1 105.4(9) . . ?
C42A N4A H4A 108(4) . . ?
C38A N4A H4A 101(4) . . ?
Mg1 N4A H4A 116(4) . . ?
N3A C37A C38A 109.8(9) . . ?
N3A C37A H37C 109.7 . . ?
C38A C37A H37C 109.7 . . ?
N3A C37A H37D 109.7 . . ?
C38A C37A H37D 109.7 . . ?
H37C C37A H37D 108.2 . . ?
C39A C38A N4A 113.9(14) . . ?
C39A C38A C37A 112.0(13) . . ?
N4A C38A C37A 105.9(12) . . ?
C39A C38A H38A 108.3 . . ?
N4A C38A H38A 108.3 . . ?
C37A C38A H38A 108.3 . . ?
C38A C39A C40A 109.5(12) . . ?
C38A C39A H39C 109.8 . . ?
C40A C39A H39C 109.8 . . ?
C38A C39A H39D 109.8 . . ?
C40A C39A H39D 109.8 . . ?
H39C C39A H39D 108.2 . . ?
C39A C40A C41A 113.5(9) . . ?
C39A C40A H40C 108.9 . . ?
C41A C40A H40C 108.9 . . ?
C39A C40A H40D 108.9 . . ?
C41A C40A H40D 108.9 . . ?
H40C C40A H40D 107.7 . . ?
C42A C41A C40A 107.6(11) . . ?
C42A C41A H41C 110.2 . . ?
C40A C41A H41C 110.2 . . ?
C42A C41A H41D 110.2 . . ?
C40A C41A H41D 110.2 . . ?
H41C C41A H41D 108.5 . . ?
N4A C42A C41A 115.2(8) . . ?
N4A C42A H42C 108.5 . . ?
C41A C42A H42C 108.5 . . ?
N4A C42A H42D 108.5 . . ?
C41A C42A H42D 108.5 . . ?
H42C C42A H42D 107.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C49 C44 C45 115.7(3) . . ?
C49 C44 C43 122.1(5) . . ?
C45 C44 C43 122.2(5) . . ?
C46 C45 C44 119.3(3) . . ?
C46 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
C47 C46 C45 118.3(4) . . ?
C47 C46 H46 120.8 . . ?
C45 C46 H46 120.8 . . ?
C46 C47 C48 124.0(4) . . ?
C46 C47 H47 118.0 . . ?
C48 C47 H47 118.0 . . ?
C47 C48 C49 119.7(4) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C48 C49 C44 123.0(4) . . ?
C48 C49 H49 118.5 . . ?
C44 C49 H49 118.5 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 C57 119.9(8) . . ?
C56 C51 C57 120.1(8) . . ?
C53 C52 C51 120.0 . . ?
C53 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C56 C55 C54 120.0 . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C55 C56 C51 120.0 . . ?
C55 C56 H56 120.0 . . ?
C51 C56 H56 120.0 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 C67 125.2(13) . . ?
C66 C61 C67 114.2(13) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 120.0 . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C63 C64 C65 120.0 . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
C66 C65 C64 120.0 . . ?
C66 C65 H65 120.0 . . ?
C64 C65 H65 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 H66 120.0 . . ?
C61 C66 H66 120.0 . . ?
C61 C67 H67A 109.5 . . ?
C61 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C61 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C72 C71 C76 120.0 . . ?
C72 C71 C77 120.4(16) . . ?
C76 C71 C77 114.8(16) . . ?
C73 C72 C71 120.0 . . ?
C73 C72 H72 120.0 . . ?
C71 C72 H72 120.0 . . ?
C74 C73 C72 120.0 . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C73 C74 C75 120.0 . . ?
C73 C74 H74 120.0 . . ?
C75 C74 H74 120.0 . . ?
C76 C75 C74 120.0 . . ?
C76 C75 H75 120.0 . . ?
C74 C75 H75 120.0 . . ?
C75 C76 C71 120.0 . . ?
C75 C76 H76 120.0 . . ?
C71 C76 H76 120.0 . . ?
C71 C77 H77A 109.5 . . ?
C71 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C71 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 C6 1.2(3) . . . . ?
Mg1 O1 C1 C2 179.92(14) . . . . ?
O1 C1 C2 C3 -178.52(19) . . . . ?
C6 C1 C2 C3 0.2(3) . . . . ?
O1 C1 C2 C7 -1.3(3) . . . . ?
C6 C1 C2 C7 177.4(2) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C7 C2 C3 C4 -177.4(2) . . . . ?
C2 C3 C4 C5 -0.3(3) . . . . ?
C2 C3 C4 C11 176.4(2) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C11 C4 C5 C6 -175.7(2) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C4 C5 C6 C15 176.6(2) . . . . ?
O1 C1 C6 C5 179.07(19) . . . . ?
C2 C1 C6 C5 0.3(3) . . . . ?
O1 C1 C6 C15 1.7(3) . . . . ?
C2 C1 C6 C15 -177.08(19) . . . . ?
C3 C2 C7 C9 -125.8(2) . . . . ?
C1 C2 C7 C9 57.1(3) . . . . ?
C3 C2 C7 C8 -6.4(3) . . . . ?
C1 C2 C7 C8 176.4(2) . . . . ?
C3 C2 C7 C10 112.1(3) . . . . ?
C1 C2 C7 C10 -65.0(3) . . . . ?
C5 C4 C11 C13 -129.5(10) . . . . ?
C3 C4 C11 C13 53.9(10) . . . . ?
C5 C4 C11 C12A 89.8(13) . . . . ?
C3 C4 C11 C12A -86.7(13) . . . . ?
C5 C4 C11 C13A -145.6(9) . . . . ?
C3 C4 C11 C13A 37.8(10) . . . . ?
C5 C4 C11 C14 -2.5(6) . . . . ?
C3 C4 C11 C14 -179.0(6) . . . . ?
C5 C4 C11 C12 111.4(4) . . . . ?
C3 C4 C11 C12 -65.1(5) . . . . ?
C5 C4 C11 C14A -34.5(15) . . . . ?
C3 C4 C11 C14A 149.0(15) . . . . ?
C16 N1 C15 C6 -177.4(2) . . . . ?
Mg1 N1 C15 C6 -5.8(4) . . . . ?
C5 C6 C15 N1 -176.5(2) . . . . ?
C1 C6 C15 N1 1.0(4) . . . . ?
C15 N1 C16 C17 -150.5(2) . . . . ?
Mg1 N1 C16 C17 37.0(3) . . . . ?
C21 N2 C17 C16 -178.3(2) . . . . ?
Mg1 N2 C17 C16 36.9(2) . . . . ?
C21 N2 C17 C18 -50.5(3) . . . . ?
Mg1 N2 C17 C18 164.7(2) . . . . ?
N1 C16 C17 N2 -49.2(3) . . . . ?
N1 C16 C17 C18 -177.2(2) . . . . ?
N2 C17 C18 C19A 7(3) . . . . ?
C16 C17 C18 C19A 134(3) . . . . ?
N2 C17 C18 C19 52.0(4) . . . . ?
C16 C17 C18 C19 178.5(3) . . . . ?
C17 C18 C19 C20 -52.9(4) . . . . ?
C17 C18 C19A C20 37(5) . . . . ?
C18 C19A C20 C21 -37(5) . . . . ?
C18 C19 C20 C21 53.0(4) . . . . ?
C17 N2 C21 C20 51.2(4) . . . . ?
Mg1 N2 C21 C20 -170.9(2) . . . . ?
C19A C20 C21 N2 -8(3) . . . . ?
C19 C20 C21 N2 -53.0(4) . . . . ?
Mg1 O2 C22 C27 8.7(3) . . . . ?
Mg1 O2 C22 C23 -171.83(14) . . . . ?
O2 C22 C23 C24 -177.08(18) . . . . ?
C27 C22 C23 C24 2.5(3) . . . . ?
O2 C22 C23 C28 2.1(3) . . . . ?
C27 C22 C23 C28 -178.35(18) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C28 C23 C24 C25 179.7(2) . . . . ?
C23 C24 C25 C26 -0.8(3) . . . . ?
C23 C24 C25 C32 179.2(2) . . . . ?
C24 C25 C26 C27 1.3(3) . . . . ?
C32 C25 C26 C27 -178.8(2) . . . . ?
C25 C26 C27 C22 0.2(3) . . . . ?
C25 C26 C27 C36 179.7(2) . . . . ?
O2 C22 C27 C26 177.47(18) . . . . ?
C23 C22 C27 C26 -2.1(3) . . . . ?
O2 C22 C27 C36 -2.0(3) . . . . ?
C23 C22 C27 C36 178.4(2) . . . . ?
C24 C23 C28 C31 -3.0(3) . . . . ?
C22 C23 C28 C31 177.8(2) . . . . ?
C24 C23 C28 C29 -122.7(2) . . . . ?
C22 C23 C28 C29 58.1(3) . . . . ?
C24 C23 C28 C30 116.0(2) . . . . ?
C22 C23 C28 C30 -63.2(3) . . . . ?
C26 C25 C32 C34 -119.3(2) . . . . ?
C24 C25 C32 C34 60.6(3) . . . . ?
C26 C25 C32 C35 1.1(3) . . . . ?
C24 C25 C32 C35 -179.0(2) . . . . ?
C26 C25 C32 C33 120.5(3) . . . . ?
C24 C25 C32 C33 -59.6(3) . . . . ?
C26 C27 C36 N3A -164.9(5) . . . . ?
C22 C27 C36 N3A 14.6(6) . . . . ?
C26 C27 C36 N3 168.0(4) . . . . ?
C22 C27 C36 N3 -12.5(5) . . . . ?
C27 C36 N3 C37 -165.4(4) . . . . ?
C27 C36 N3 Mg1 19.4(7) . . . . ?
C36 N3 C37 C38 -142.4(8) . . . . ?
Mg1 N3 C37 C38 33.3(8) . . . . ?
C42 N4 C38 C37 -177.5(8) . . . . ?
Mg1 N4 C38 C37 38.1(11) . . . . ?
C42 N4 C38 C39 -55.3(12) . . . . ?
Mg1 N4 C38 C39 160.3(8) . . . . ?
N3 C37 C38 N4 -46.8(11) . . . . ?
N3 C37 C38 C39 -169.1(9) . . . . ?
N4 C38 C39 C40 53.7(12) . . . . ?
C37 C38 C39 C40 174.6(9) . . . . ?
C38 C39 C40 C41 -51.7(12) . . . . ?
C39 C40 C41 C42 54.2(14) . . . . ?
C38 N4 C42 C41 55.0(12) . . . . ?
Mg1 N4 C42 C41 -167.2(6) . . . . ?
C40 C41 C42 N4 -55.7(14) . . . . ?
C27 C36 N3A C37A 168.5(4) . . . . ?
C27 C36 N3A Mg1 -28.0(7) . . . . ?
C36 N3A C37A C38A 140.0(8) . . . . ?
Mg1 N3A C37A C38A -24.7(8) . . . . ?
C42A N4A C38A C39A 57.0(14) . . . . ?
Mg1 N4A C38A C39A -178.9(9) . . . . ?
C42A N4A C38A C37A -179.5(8) . . . . ?
Mg1 N4A C38A C37A -55.4(9) . . . . ?
N3A C37A C38A C39A 178.3(10) . . . . ?
N3A C37A C38A N4A 53.6(10) . . . . ?
N4A C38A C39A C40A -55.9(15) . . . . ?
C37A C38A C39A C40A -176.0(9) . . . . ?
C38A C39A C40A C41A 53.7(14) . . . . ?
C39A C40A C41A C42A -50.4(13) . . . . ?
C38A N4A C42A C41A -55.0(13) . . . . ?
Mg1 N4A C42A C41A -173.9(8) . . . . ?
C40A C41A C42A N4A 51.7(13) . . . . ?
C49 C44 C45 C46 -1.1(5) . . . . ?
C43 C44 C45 C46 179.5(4) . . . . ?
C44 C45 C46 C47 1.4(5) . . . . ?
C45 C46 C47 C48 -0.8(6) . . . . ?
C46 C47 C48 C49 -0.1(7) . . . . ?
C47 C48 C49 C44 0.5(7) . . . . ?
C45 C44 C49 C48 0.2(6) . . . . ?
C43 C44 C49 C48 179.6(5) . . . . ?
C56 C51 C52 C53 0.0 . . . . ?
C57 C51 C52 C53 -178.6(9) . . . . ?
C51 C52 C53 C54 0.0 . . . . ?
C52 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 C56 0.0 . . . . ?
C54 C55 C56 C51 0.0 . . . . ?
C52 C51 C56 C55 0.0 . . . . ?
C57 C51 C56 C55 178.6(9) . . . . ?
C66 C61 C62 C63 0.0 . . . . ?
C67 C61 C62 C63 169.9(17) . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C66 0.0 . . . . ?
C64 C65 C66 C61 0.0 . . . . ?
C62 C61 C66 C65 0.0 . . . . ?
C67 C61 C66 C65 -170.9(15) . . . . ?
C76 C71 C72 C73 0.0 . . . . ?
C77 C71 C72 C73 -154(2) . . . . ?
C71 C72 C73 C74 0.0 . . . . ?
C72 C73 C74 C75 0.0 . . . . ?
C73 C74 C75 C76 0.0 . . . . ?
C74 C75 C76 C71 0.0 . . . . ?
C72 C71 C76 C75 0.0 . . . . ?
C77 C71 C76 C75 155(2) . . . . ?

_refine_diff_density_max         0.793
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_s16mdj48
_database_code_depnum_ccdc_archive 'CCDC 1534476'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H80 N4 O4 Ti'
_chemical_formula_weight         825.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7501(3)
_cell_length_b                   14.1972(4)
_cell_length_c                   19.0565(7)
_cell_angle_alpha                76.731(3)
_cell_angle_beta                 80.759(3)
_cell_angle_gamma                71.707(3)
_cell_volume                     2426.49(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12939
_cell_measurement_theta_min      3.7220
_cell_measurement_theta_max      73.2450

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.828
_shelx_estimated_absorpt_T_min   0.771
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_T_min  0.85734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            21882
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.340
_diffrn_reflns_theta_max         72.125
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9545
_reflns_number_gt                8916
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0560P)²+1.0259P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9545
_refine_ls_number_parameters     568
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Ti1 Ti 0.28529(3) 0.97904(2) 0.25940(2) 0.01986(8) Uani 1 1 d . . . . .
O1 O 0.26655(14) 0.96710(9) 0.16946(6) 0.0365(3) Uani 1 1 d . . . . .
N1 N 0.52866(13) 0.93211(9) 0.23164(6) 0.0202(2) Uani 1 1 d . . . . .
C1 C 0.1963(2) 1.00397(14) 0.10611(10) 0.0383(4) Uani 1 1 d . . . . .
H1 H 0.1518 1.0786 0.1018 0.046 Uiso 1 1 calc R U . . .
H2 H 0.639(2) 0.8794(17) 0.1068(12) 0.042(6) Uiso 1 1 d . . . . .
H4 H 0.229(3) 1.037(2) 0.4841(14) 0.065(8) Uiso 1 1 d . . . . .
O2 O 0.10392(13) 1.03055(9) 0.29655(7) 0.0375(3) Uani 1 1 d . . . . .
N2 N 0.69236(18) 0.80663(11) 0.12316(8) 0.0363(3) Uani 1 1 d . . . . .
C2 C 0.3046(3) 0.9853(2) 0.04179(12) 0.0641(7) Uani 1 1 d . . . . .
H2A H 0.3818 1.0158 0.0419 0.096 Uiso 1 1 calc R U . . .
H2B H 0.2562 1.0156 -0.0027 0.096 Uiso 1 1 calc R U . . .
H2C H 0.3465 0.9124 0.0441 0.096 Uiso 1 1 calc R U . . .
O3 O 0.31336(11) 1.11303(8) 0.23150(6) 0.0233(2) Uani 1 1 d . . . . .
N3 N 0.37778(13) 0.96152(9) 0.36591(6) 0.0196(2) Uani 1 1 d . . . . .
C3 C 0.0768(2) 0.95594(17) 0.11120(12) 0.0495(5) Uani 1 1 d . . . . .
H3A H 0.1185 0.8826 0.1160 0.074 Uiso 1 1 calc R U . . .
H3B H 0.0258 0.9830 0.0673 0.074 Uiso 1 1 calc R U . . .
H3C H 0.0084 0.9710 0.1536 0.074 Uiso 1 1 calc R U . . .
O4 O 0.29448(12) 0.83945(8) 0.29917(5) 0.0230(2) Uani 1 1 d . . . . .
N4 N 0.2764(2) 1.09115(12) 0.48183(8) 0.0437(4) Uani 1 1 d . . . . .
C4 C -0.0206(3) 1.0984(2) 0.31961(15) 0.0353(6) Uani 0.7 1 d . . P A 1
H4A H 0.0001 1.1650 0.3105 0.042 Uiso 0.7 1 calc R U P A 1
C5 C -0.0439(8) 1.0660(6) 0.4008(3) 0.0534(17) Uani 0.7 1 d . . P A 1
H5A H -0.0626 1.0000 0.4123 0.080 Uiso 0.7 1 calc R U P A 1
H5B H -0.1271 1.1159 0.4202 0.080 Uiso 0.7 1 calc R U P A 1
H5C H 0.0431 1.0611 0.4226 0.080 Uiso 0.7 1 calc R U P A 1
C6 C -0.1399(6) 1.1124(5) 0.2788(4) 0.0700(16) Uani 0.7 1 d . . P A 1
H6A H -0.1082 1.1245 0.2269 0.105 Uiso 0.7 1 calc R U P A 1
H6B H -0.2197 1.1706 0.2902 0.105 Uiso 0.7 1 calc R U P A 1
H6C H -0.1730 1.0516 0.2916 0.105 Uiso 0.7 1 calc R U P A 1
C7 C 0.40295(16) 1.15560(11) 0.18499(8) 0.0203(3) Uani 1 1 d . . . . .
C8 C 0.54699(16) 1.09928(11) 0.16838(8) 0.0213(3) Uani 1 1 d . . . . .
C9 C 0.64548(16) 1.14482(11) 0.12208(8) 0.0224(3) Uani 1 1 d . . . . .
H9 H 0.7428 1.1054 0.1130 0.027 Uiso 1 1 calc R U . . .
C10 C 0.60379(17) 1.24538(11) 0.08963(8) 0.0234(3) Uani 1 1 d . . . . .
C11 C 0.45876(17) 1.29987(11) 0.10560(8) 0.0240(3) Uani 1 1 d . . . . .
H11 H 0.4282 1.3690 0.0830 0.029 Uiso 1 1 calc R U . . .
C12 C 0.35700(16) 1.26030(11) 0.15191(8) 0.0219(3) Uani 1 1 d . . . . .
C13 C 0.70654(18) 1.29906(12) 0.03905(9) 0.0282(3) Uani 1 1 d . . . . .
C14 C 0.86085(18) 1.22871(13) 0.03110(10) 0.0349(4) Uani 1 1 d . . . . .
H14A H 0.9231 1.2658 -0.0015 0.052 Uiso 1 1 calc R U . . .
H14B H 0.8599 1.1713 0.0110 0.052 Uiso 1 1 calc R U . . .
H14C H 0.8985 1.2040 0.0787 0.052 Uiso 1 1 calc R U . . .
C15 C 0.6514(2) 1.33789(15) -0.03636(10) 0.0405(4) Uani 1 1 d . . . . .
H15A H 0.5533 1.3844 -0.0325 0.061 Uiso 1 1 calc R U . . .
H15B H 0.6495 1.2807 -0.0564 0.061 Uiso 1 1 calc R U . . .
H15C H 0.7163 1.3734 -0.0683 0.061 Uiso 1 1 calc R U . . .
C16 C 0.7118(2) 1.38848(14) 0.07000(11) 0.0396(4) Uani 1 1 d . . . . .
H16A H 0.6161 1.4386 0.0698 0.059 Uiso 1 1 calc R U . . .
H16B H 0.7838 1.4195 0.0402 0.059 Uiso 1 1 calc R U . . .
H16C H 0.7388 1.3644 0.1198 0.059 Uiso 1 1 calc R U . . .
C17 C 0.20194(17) 1.32634(11) 0.16763(8) 0.0262(3) Uani 1 1 d . . . . .
C18 C 0.09281(19) 1.28332(14) 0.14576(11) 0.0379(4) Uani 1 1 d . . . . .
H18A H 0.1103 1.2831 0.0937 0.057 Uiso 1 1 calc R U . . .
H18B H -0.0060 1.3253 0.1569 0.057 Uiso 1 1 calc R U . . .
H18C H 0.1043 1.2141 0.1727 0.057 Uiso 1 1 calc R U . . .
C19 C 0.1767(2) 1.43562(13) 0.12586(11) 0.0398(4) Uani 1 1 d . . . . .
H19A H 0.1927 1.4360 0.0737 0.060 Uiso 1 1 calc R U . . .
H19B H 0.2445 1.4655 0.1392 0.060 Uiso 1 1 calc R U . . .
H19C H 0.0769 1.4751 0.1380 0.060 Uiso 1 1 calc R U . . .
C20 C 0.1719(2) 1.33163(14) 0.24795(9) 0.0392(4) Uani 1 1 d . . . . .
H20A H 0.0736 1.3756 0.2573 0.059 Uiso 1 1 calc R U . . .
H20B H 0.2424 1.3590 0.2614 0.059 Uiso 1 1 calc R U . . .
H20C H 0.1803 1.2637 0.2767 0.059 Uiso 1 1 calc R U . . .
C21 C 0.60248(16) 0.99235(11) 0.19805(8) 0.0216(3) Uani 1 1 d . . . . .
H21 H 0.7047 0.9638 0.1919 0.026 Uiso 1 1 calc R U . . .
C22 C 0.61349(16) 0.82535(11) 0.25047(8) 0.0232(3) Uani 1 1 d . . . . .
H22A H 0.5703 0.7937 0.2969 0.028 Uiso 1 1 calc R U . . .
H22B H 0.7140 0.8215 0.2570 0.028 Uiso 1 1 calc R U . . .
C23 C 0.61686(17) 0.76713(11) 0.19168(8) 0.0241(3) Uani 1 1 d . . . . .
H23 H 0.5152 0.7735 0.1836 0.029 Uiso 1 1 calc R U . . .
C24 C 0.6955(2) 0.65760(12) 0.21657(9) 0.0331(4) Uani 1 1 d . . . . .
H24A H 0.6419 0.6302 0.2612 0.040 Uiso 1 1 calc R U . . .
H24B H 0.7932 0.6520 0.2286 0.040 Uiso 1 1 calc R U . . .
C25 C 0.7107(3) 0.59528(14) 0.15969(12) 0.0493(5) Uani 1 1 d . . . . .
H25A H 0.7695 0.5251 0.1767 0.059 Uiso 1 1 calc R U . . .
H25B H 0.6136 0.5935 0.1519 0.059 Uiso 1 1 calc R U . . .
C26 C 0.7824(3) 0.63948(16) 0.08948(12) 0.0547(6) Uani 1 1 d . . . . .
H26A H 0.7844 0.6012 0.0518 0.066 Uiso 1 1 calc R U . . .
H26B H 0.8838 0.6336 0.0958 0.066 Uiso 1 1 calc R U . . .
C27 C 0.7011(3) 0.74921(15) 0.06558(10) 0.0467(5) Uani 1 1 d . . . . .
H27A H 0.7516 0.7781 0.0204 0.056 Uiso 1 1 calc R U . . .
H27B H 0.6020 0.7548 0.0555 0.056 Uiso 1 1 calc R U . . .
C28 C 0.28371(16) 0.78130(11) 0.36348(8) 0.0200(3) Uani 1 1 d . . . . .
C29 C 0.22670(16) 0.69784(11) 0.37341(8) 0.0217(3) Uani 1 1 d . . . . .
C30 C 0.22603(16) 0.63714(11) 0.44192(8) 0.0230(3) Uani 1 1 d . . . . .
H30 H 0.1866 0.5821 0.4488 0.028 Uiso 1 1 calc R U . . .
C31 C 0.27958(16) 0.65137(11) 0.50181(8) 0.0222(3) Uani 1 1 d . . . . .
C32 C 0.33203(16) 0.73368(11) 0.49100(8) 0.0220(3) Uani 1 1 d . . . . .
H32 H 0.3687 0.7462 0.5302 0.026 Uiso 1 1 calc R U . . .
C33 C 0.33271(16) 0.79962(11) 0.42347(8) 0.0207(3) Uani 1 1 d . . . . .
C34 C 0.16561(18) 0.67745(12) 0.31073(8) 0.0260(3) Uani 1 1 d . . . . .
C35 C 0.0376(2) 0.76857(14) 0.28518(10) 0.0368(4) Uani 1 1 d . . . . .
H35A H -0.0416 0.7758 0.3242 0.055 Uiso 1 1 calc R U . . .
H35B H 0.0037 0.7580 0.2427 0.055 Uiso 1 1 calc R U . . .
H35C H 0.0691 0.8300 0.2724 0.055 Uiso 1 1 calc R U . . .
C36 C 0.2834(2) 0.65894(15) 0.24749(10) 0.0379(4) Uani 1 1 d . . . . .
H36A H 0.3153 0.7198 0.2289 0.057 Uiso 1 1 calc R U . . .
H36B H 0.2441 0.6431 0.2089 0.057 Uiso 1 1 calc R U . . .
H36C H 0.3662 0.6021 0.2644 0.057 Uiso 1 1 calc R U . . .
C37 C 0.1092(2) 0.58452(14) 0.33311(10) 0.0392(4) Uani 1 1 d . . . . .
H37A H 0.1883 0.5249 0.3499 0.059 Uiso 1 1 calc R U . . .
H37B H 0.0723 0.5741 0.2915 0.059 Uiso 1 1 calc R U . . .
H37C H 0.0308 0.5952 0.3723 0.059 Uiso 1 1 calc R U . . .
C38 C 0.27398(18) 0.57922(12) 0.57510(8) 0.0266(3) Uani 1 1 d . . . . .
C39 C 0.3599(4) 0.5954(2) 0.62860(12) 0.0752(9) Uani 1 1 d . . . . .
H39A H 0.3204 0.6649 0.6369 0.113 Uiso 1 1 calc R U . . .
H39B H 0.4618 0.5837 0.6090 0.113 Uiso 1 1 calc R U . . .
H39C H 0.3531 0.5481 0.6745 0.113 Uiso 1 1 calc R U . . .
C40 C 0.1171(2) 0.59614(18) 0.60685(13) 0.0584(7) Uani 1 1 d . . . . .
H40A H 0.1122 0.5483 0.6526 0.088 Uiso 1 1 calc R U . . .
H40B H 0.0604 0.5857 0.5728 0.088 Uiso 1 1 calc R U . . .
H28 H 0.0774 0.6654 0.6157 0.088 Uiso 1 1 calc R U . . .
C41 C 0.3336(3) 0.46894(14) 0.56592(11) 0.0516(6) Uani 1 1 d . . . . .
H41A H 0.4362 0.4550 0.5472 0.077 Uiso 1 1 calc R U . . .
H41B H 0.2788 0.4568 0.5318 0.077 Uiso 1 1 calc R U . . .
H41C H 0.3240 0.4244 0.6129 0.077 Uiso 1 1 calc R U . . .
C42 C 0.38723(16) 0.88517(11) 0.41842(8) 0.0212(3) Uani 1 1 d . . . . .
H42 H 0.4351 0.8848 0.4582 0.025 Uiso 1 1 calc R U . . .
C43 C 0.44087(16) 1.03845(11) 0.37647(8) 0.0225(3) Uani 1 1 d . . . . .
H43A H 0.4880 1.0658 0.3296 0.027 Uiso 1 1 calc R U . . .
H43B H 0.5164 1.0063 0.4106 0.027 Uiso 1 1 calc R U . . .
C44 C 0.32638(17) 1.12515(11) 0.40609(8) 0.0225(3) Uani 1 1 d . . . . .
H44 H 0.2422 1.1512 0.3761 0.027 Uiso 1 1 calc R U . . .
C45 C 0.1622(3) 1.17440(14) 0.51171(11) 0.0453(5) Uani 1 1 d . . . . .
H45A H 0.1273 1.1486 0.5620 0.054 Uiso 1 1 calc R U . . .
H45B H 0.0787 1.1997 0.4821 0.054 Uiso 1 1 calc R U . . .
C46 C 0.2257(2) 1.25956(14) 0.51060(11) 0.0418(4) Uani 1 1 d . . . . .
H46A H 0.1492 1.3165 0.5277 0.050 Uiso 1 1 calc R U . . .
H46B H 0.3032 1.2357 0.5438 0.050 Uiso 1 1 calc R U . . .
C47 C 0.2878(2) 1.29533(13) 0.43465(10) 0.0351(4) Uani 1 1 d . . . . .
H47A H 0.2078 1.3289 0.4032 0.042 Uiso 1 1 calc R U . . .
H47B H 0.3383 1.3455 0.4357 0.042 Uiso 1 1 calc R U . . .
C48 C 0.39295(18) 1.20821(12) 0.40344(10) 0.0310(4) Uani 1 1 d . . . . .
H48A H 0.4253 1.2331 0.3525 0.037 Uiso 1 1 calc R U . . .
H48B H 0.4794 1.1808 0.4310 0.037 Uiso 1 1 calc R U . . .
C4' C -0.0385(6) 1.0393(5) 0.3292(4) 0.0366(14) Uani 0.3 1 d D . P A 2
H4' H -0.0413 0.9677 0.3455 0.044 Uiso 0.3 1 calc R U P A 2
C5' C -0.0900(19) 1.0840(18) 0.3973(8) 0.062(5) Uani 0.3 1 d D . P A 2
H5'1 H -0.0678 1.1485 0.3898 0.093 Uiso 0.3 1 calc R U P A 2
H5'2 H -0.0404 1.0372 0.4380 0.093 Uiso 0.3 1 calc R U P A 2
H5'3 H -0.1950 1.0953 0.4079 0.093 Uiso 0.3 1 calc R U P A 2
C6' C -0.152(2) 1.0849(17) 0.2757(13) 0.150(12) Uani 0.3 1 d D . P A 2
H6'1 H -0.1230 1.1372 0.2384 0.225 Uiso 0.3 1 calc R U P A 2
H6'2 H -0.2456 1.1151 0.3011 0.225 Uiso 0.3 1 calc R U P A 2
H6'3 H -0.1605 1.0320 0.2530 0.225 Uiso 0.3 1 calc R U 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
Ti1 O2 1.7852(12) . ?
Ti1 O1 1.8037(12) . ?
Ti1 O4 1.9316(10) . ?
Ti1 O3 1.9473(10) . ?
Ti1 N1 2.2628(13) . ?
Ti1 N3 2.2825(12) . ?
O1 C1 1.397(2) . ?
N1 C21 1.2831(19) . ?
N1 C22 1.4727(18) . ?
C1 C2 1.498(3) . ?
C1 C3 1.504(3) . ?
O2 C4 1.372(3) . ?
O2 C4' 1.408(5) . ?
N2 C23 1.475(2) . ?
N2 C27 1.487(2) . ?
O3 C7 1.3232(17) . ?
N3 C42 1.2860(19) . ?
N3 C43 1.4745(17) . ?
O4 C28 1.3203(17) . ?
N4 C44 1.468(2) . ?
N4 C45 1.497(2) . ?
C4 C6 1.438(5) . ?
C4 C5 1.511(7) . ?
C7 C8 1.407(2) . ?
C7 C12 1.432(2) . ?
C8 C9 1.405(2) . ?
C8 C21 1.451(2) . ?
C9 C10 1.377(2) . ?
C10 C11 1.405(2) . ?
C10 C13 1.531(2) . ?
C11 C12 1.386(2) . ?
C12 C17 1.532(2) . ?
C13 C14 1.529(2) . ?
C13 C16 1.535(2) . ?
C13 C15 1.535(2) . ?
C17 C20 1.526(2) . ?
C17 C18 1.532(2) . ?
C17 C19 1.535(2) . ?
C22 C23 1.528(2) . ?
C23 C24 1.503(2) . ?
C24 C25 1.512(3) . ?
C25 C26 1.504(3) . ?
C26 C27 1.509(3) . ?
C28 C33 1.412(2) . ?
C28 C29 1.423(2) . ?
C29 C30 1.390(2) . ?
C29 C34 1.537(2) . ?
C30 C31 1.407(2) . ?
C31 C32 1.378(2) . ?
C31 C38 1.535(2) . ?
C32 C33 1.407(2) . ?
C33 C42 1.450(2) . ?
C34 C37 1.532(2) . ?
C34 C36 1.534(2) . ?
C34 C35 1.536(2) . ?
C38 C39 1.516(3) . ?
C38 C40 1.517(3) . ?
C38 C41 1.530(2) . ?
C43 C44 1.528(2) . ?
C44 C48 1.502(2) . ?
C45 C46 1.517(3) . ?
C46 C47 1.514(3) . ?
C47 C48 1.510(2) . ?
C4' C6' 1.514(5) . ?
C4' C5' 1.518(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 104.60(6) . . ?
O2 Ti1 O4 95.83(5) . . ?
O1 Ti1 O4 92.75(5) . . ?
O2 Ti1 O3 90.99(5) . . ?
O1 Ti1 O3 96.09(5) . . ?
O4 Ti1 O3 167.12(5) . . ?
O2 Ti1 N1 166.05(6) . . ?
O1 Ti1 N1 87.99(5) . . ?
O4 Ti1 N1 89.43(4) . . ?
O3 Ti1 N1 81.56(4) . . ?
O2 Ti1 N3 92.36(6) . . ?
O1 Ti1 N3 162.39(5) . . ?
O4 Ti1 N3 80.65(4) . . ?
O3 Ti1 N3 88.19(4) . . ?
N1 Ti1 N3 75.71(4) . . ?
C1 O1 Ti1 149.78(12) . . ?
C21 N1 C22 115.10(12) . . ?
C21 N1 Ti1 124.68(10) . . ?
C22 N1 Ti1 120.20(9) . . ?
O1 C1 C2 109.68(18) . . ?
O1 C1 C3 109.31(16) . . ?
C2 C1 C3 112.59(18) . . ?
C4 O2 Ti1 161.02(16) . . ?
C4' O2 Ti1 162.0(3) . . ?
C23 N2 C27 111.96(14) . . ?
C7 O3 Ti1 136.18(9) . . ?
C42 N3 C43 114.98(12) . . ?
C42 N3 Ti1 124.98(10) . . ?
C43 N3 Ti1 119.94(9) . . ?
C28 O4 Ti1 138.20(9) . . ?
C44 N4 C45 111.56(14) . . ?
O2 C4 C6 112.4(3) . . ?
O2 C4 C5 106.7(3) . . ?
C6 C4 C5 116.9(5) . . ?
O3 C7 C8 120.52(13) . . ?
O3 C7 C12 120.93(13) . . ?
C8 C7 C12 118.53(13) . . ?
C9 C8 C7 121.12(13) . . ?
C9 C8 C21 116.40(13) . . ?
C7 C8 C21 122.47(13) . . ?
C10 C9 C8 121.37(14) . . ?
C9 C10 C11 116.68(14) . . ?
C9 C10 C13 123.62(14) . . ?
C11 C10 C13 119.69(13) . . ?
C12 C11 C10 124.91(14) . . ?
C11 C12 C7 117.35(14) . . ?
C11 C12 C17 121.25(13) . . ?
C7 C12 C17 121.40(13) . . ?
C14 C13 C10 111.95(13) . . ?
C14 C13 C16 108.25(14) . . ?
C10 C13 C16 109.15(14) . . ?
C14 C13 C15 108.30(15) . . ?
C10 C13 C15 109.64(13) . . ?
C16 C13 C15 109.52(15) . . ?
C20 C17 C18 110.12(15) . . ?
C20 C17 C12 109.98(13) . . ?
C18 C17 C12 110.09(13) . . ?
C20 C17 C19 106.61(14) . . ?
C18 C17 C19 107.56(14) . . ?
C12 C17 C19 112.39(13) . . ?
N1 C21 C8 127.16(14) . . ?
N1 C22 C23 111.43(12) . . ?
N2 C23 C24 109.19(13) . . ?
N2 C23 C22 110.86(13) . . ?
C24 C23 C22 108.75(13) . . ?
C23 C24 C25 112.19(15) . . ?
C26 C25 C24 110.49(17) . . ?
C25 C26 C27 110.48(17) . . ?
N2 C27 C26 109.98(17) . . ?
O4 C28 C33 120.12(13) . . ?
O4 C28 C29 121.07(13) . . ?
C33 C28 C29 118.79(13) . . ?
C30 C29 C28 117.56(13) . . ?
C30 C29 C34 121.59(13) . . ?
C28 C29 C34 120.84(13) . . ?
C29 C30 C31 124.73(13) . . ?
C32 C31 C30 116.48(13) . . ?
C32 C31 C38 123.16(14) . . ?
C30 C31 C38 120.33(13) . . ?
C31 C32 C33 121.72(14) . . ?
C32 C33 C28 120.63(13) . . ?
C32 C33 C42 117.24(13) . . ?
C28 C33 C42 122.12(13) . . ?
C37 C34 C36 107.48(14) . . ?
C37 C34 C35 107.37(14) . . ?
C36 C34 C35 109.70(15) . . ?
C37 C34 C29 112.34(13) . . ?
C36 C34 C29 110.44(13) . . ?
C35 C34 C29 109.43(13) . . ?
C39 C38 C40 108.7(2) . . ?
C39 C38 C41 108.21(18) . . ?
C40 C38 C41 107.63(16) . . ?
C39 C38 C31 112.28(14) . . ?
C40 C38 C31 108.95(14) . . ?
C41 C38 C31 110.92(13) . . ?
N3 C42 C33 127.02(13) . . ?
N3 C43 C44 112.01(12) . . ?
N4 C44 C48 108.13(14) . . ?
N4 C44 C43 110.56(12) . . ?
C48 C44 C43 108.87(13) . . ?
N4 C45 C46 109.20(18) . . ?
C47 C46 C45 110.32(15) . . ?
C48 C47 C46 111.20(15) . . ?
C44 C48 C47 112.07(14) . . ?
O2 C4' C6' 113.1(12) . . ?
O2 C4' C5' 120.2(9) . . ?
C6' C4' C5' 109.9(13) . . ?

_refine_diff_density_max         0.727
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.043

####################################################################### 
# 
# 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_s16mdj49
_database_code_depnum_ccdc_archive 'CCDC 1534477'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H144 N4 O8 Zr2'
_chemical_formula_weight         1568.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3200(4)
_cell_length_b                   11.4648(5)
_cell_length_c                   18.7325(7)
_cell_angle_alpha                78.072(3)
_cell_angle_beta                 72.528(3)
_cell_angle_gamma                76.808(3)
_cell_volume                     2232.65(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11943
_cell_measurement_theta_min      4.1610
_cell_measurement_theta_max      71.9680

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.317
_shelx_estimated_absorpt_T_min   0.723
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_T_min  0.86376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            16035
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.005
_diffrn_reflns_theta_max         72.415
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16035
_reflns_number_gt                14040
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16035
_refine_ls_number_parameters     479
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.002
_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
Zr1 Zr 0.71726(2) 0.41513(2) 0.77974(2) 0.01496(7) Uani 1 1 d . . . . .
O1 O 0.88662(17) 0.44452(17) 0.75454(11) 0.0230(4) Uani 1 1 d . . . . .
N1 N 0.50263(18) 0.40320(18) 0.78828(11) 0.0153(4) Uani 1 1 d . . . . .
C1 C 1.0117(2) 0.4608(2) 0.74145(16) 0.0242(6) Uani 1 1 d . . . . .
O2 O 0.70582(18) 0.29140(16) 0.86752(10) 0.0233(4) Uani 1 1 d . . . . .
N2 N 0.31237(19) 0.41797(18) 0.88275(12) 0.0167(4) Uani 1 1 d . . . . .
C2 C 1.0963(3) 0.3371(3) 0.7364(2) 0.0443(9) Uani 1 1 d . . . . .
H2A H 1.0715 0.2830 0.7841 0.066 Uiso 1 1 calc R U . . .
H2B H 1.1840 0.3458 0.7273 0.066 Uiso 1 1 calc R U . . .
H2C H 1.0879 0.3030 0.6948 0.066 Uiso 1 1 calc R U . . .
O3 O 0.62736(16) 0.58185(15) 0.80320(10) 0.0205(4) Uani 1 1 d . . . . .
C3 C 1.0467(3) 0.5444(3) 0.6672(2) 0.0389(7) Uani 1 1 d . . . . .
H3A H 1.0384 0.5087 0.6261 0.058 Uiso 1 1 calc R U . . .
H3B H 1.1338 0.5555 0.6571 0.058 Uiso 1 1 calc R U . . .
H3C H 0.9904 0.6231 0.6705 0.058 Uiso 1 1 calc R U . . .
O4 O 0.73276(16) 0.36096(17) 0.68256(10) 0.0220(4) Uani 1 1 d . . . . .
C4 C 1.0174(4) 0.5143(4) 0.8075(2) 0.0475(9) Uani 1 1 d . . . . .
H4A H 0.9709 0.5977 0.8056 0.071 Uiso 1 1 calc R U . . .
H4B H 1.1053 0.5140 0.8046 0.071 Uiso 1 1 calc R U . . .
H4C H 0.9795 0.4659 0.8551 0.071 Uiso 1 1 calc R U . . .
C5 C 0.7284(3) 0.2124(3) 0.93269(16) 0.0279(6) Uani 1 1 d . . . . .
C6 C 0.8662(3) 0.1974(4) 0.9301(2) 0.0550(11) Uani 1 1 d . . . . .
H6A H 0.9186 0.1664 0.8836 0.082 Uiso 1 1 calc R U . . .
H6B H 0.8834 0.1401 0.9741 0.082 Uiso 1 1 calc R U . . .
H6C H 0.8856 0.2760 0.9312 0.082 Uiso 1 1 calc R U . . .
C7 C 0.6952(4) 0.0909(3) 0.9320(3) 0.0535(10) Uani 1 1 d . . . . .
H7A H 0.6059 0.1021 0.9339 0.080 Uiso 1 1 calc R U . . .
H7B H 0.7119 0.0337 0.9761 0.080 Uiso 1 1 calc R U . . .
H7C H 0.7466 0.0588 0.8856 0.080 Uiso 1 1 calc R U . . .
C8 C 0.6449(4) 0.2674(4) 1.00178(18) 0.0464(9) Uani 1 1 d . . . . .
H8A H 0.6660 0.3462 1.0007 0.070 Uiso 1 1 calc R U . . .
H8B H 0.6581 0.2133 1.0477 0.070 Uiso 1 1 calc R U . . .
H8C H 0.5565 0.2784 1.0016 0.070 Uiso 1 1 calc R U . . .
C9 C 0.5169(2) 0.6584(2) 0.80375(14) 0.0170(5) Uani 1 1 d . . . . .
C10 C 0.4068(2) 0.6083(2) 0.82547(13) 0.0164(5) Uani 1 1 d . . . . .
C11 C 0.2929(2) 0.6802(2) 0.81882(13) 0.0172(5) Uani 1 1 d . . . . .
H11 H 0.2199 0.6444 0.8320 0.021 Uiso 1 1 calc R U . . .
C12 C 0.2842(2) 0.8043(2) 0.79299(14) 0.0186(5) Uani 1 1 d . . . . .
C13 C 0.3936(2) 0.8530(2) 0.77666(14) 0.0198(5) Uani 1 1 d . . . . .
H13 H 0.3879 0.9379 0.7614 0.024 Uiso 1 1 calc R U . . .
C14 C 0.5107(2) 0.7842(2) 0.78144(14) 0.0195(5) Uani 1 1 d . . . . .
C15 C 0.1595(2) 0.8811(2) 0.78168(15) 0.0232(5) Uani 1 1 d . . . . .
C16 C 0.1281(3) 0.8403(3) 0.7163(2) 0.0449(8) Uani 1 1 d . . . . .
H16A H 0.1289 0.7528 0.7271 0.067 Uiso 1 1 calc R U . . .
H16B H 0.1911 0.8593 0.6686 0.067 Uiso 1 1 calc R U . . .
H16C H 0.0445 0.8832 0.7119 0.067 Uiso 1 1 calc R U . . .
C17 C 0.0531(3) 0.8609(3) 0.8525(2) 0.0435(8) Uani 1 1 d . . . . .
H17A H 0.0701 0.8859 0.8949 0.065 Uiso 1 1 calc R U . . .
H17B H 0.0468 0.7748 0.8644 0.065 Uiso 1 1 calc R U . . .
H17C H -0.0263 0.9088 0.8439 0.065 Uiso 1 1 calc R U . . .
C18 C 0.1622(3) 1.0155(3) 0.7608(2) 0.0453(9) Uani 1 1 d . . . . .
H18A H 0.0803 1.0590 0.7538 0.068 Uiso 1 1 calc R U . . .
H18B H 0.2279 1.0299 0.7137 0.068 Uiso 1 1 calc R U . . .
H18C H 0.1801 1.0445 0.8015 0.068 Uiso 1 1 calc R U . . .
C19 C 0.6276(3) 0.8429(2) 0.76313(17) 0.0261(6) Uani 1 1 d . . . . .
C20 C 0.7269(3) 0.7986(3) 0.69348(19) 0.0345(7) Uani 1 1 d . . . . .
H20A H 0.6921 0.8219 0.6495 0.052 Uiso 1 1 calc R U . . .
H20B H 0.7505 0.7102 0.7030 0.052 Uiso 1 1 calc R U . . .
H20C H 0.8014 0.8354 0.6834 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6839(3) 0.8104(3) 0.8316(2) 0.0390(7) Uani 1 1 d . . . . .
H21A H 0.7589 0.8471 0.8198 0.058 Uiso 1 1 calc R U . . .
H21B H 0.7070 0.7221 0.8429 0.058 Uiso 1 1 calc R U . . .
H21C H 0.6215 0.8411 0.8756 0.058 Uiso 1 1 calc R U . . .
C22 C 0.5952(3) 0.9814(3) 0.7472(2) 0.0407(8) Uani 1 1 d . . . . .
H22A H 0.5649 1.0055 0.7016 0.061 Uiso 1 1 calc R U . . .
H22B H 0.6705 1.0158 0.7397 0.061 Uiso 1 1 calc R U . . .
H22C H 0.5294 1.0113 0.7903 0.061 Uiso 1 1 calc R U . . .
C23 C 0.4244(2) 0.4737(2) 0.85154(13) 0.0162(5) Uani 1 1 d . . . . .
H23 H 0.4711 0.4559 0.8913 0.019 Uiso 1 1 calc R U . . .
C24 C 0.2371(2) 0.4453(2) 0.95814(14) 0.0220(5) Uani 1 1 d . . . . .
H24A H 0.2008 0.5327 0.9553 0.026 Uiso 1 1 calc R U . . .
H24B H 0.2913 0.4253 0.9934 0.026 Uiso 1 1 calc R U . . .
C25 C 0.1320(3) 0.3710(3) 0.98705(15) 0.0262(6) Uani 1 1 d . . . . .
H25A H 0.0725 0.3991 0.9551 0.031 Uiso 1 1 calc R U . . .
H25B H 0.0853 0.3849 1.0393 0.031 Uiso 1 1 calc R U . . .
C26 C 0.1809(3) 0.2352(2) 0.98652(16) 0.0264(6) Uani 1 1 d . . . . .
H26A H 0.1089 0.1926 0.9985 0.032 Uiso 1 1 calc R U . . .
H26B H 0.2265 0.2032 1.0260 0.032 Uiso 1 1 calc R U . . .
C27 C 0.2691(2) 0.2107(2) 0.90930(15) 0.0232(5) Uani 1 1 d . . . . .
H27A H 0.3085 0.1240 0.9118 0.028 Uiso 1 1 calc R U . . .
H27B H 0.2210 0.2304 0.8708 0.028 Uiso 1 1 calc R U . . .
C28 C 0.3693(2) 0.2884(2) 0.88796(14) 0.0182(5) Uani 1 1 d . . . . .
H28 H 0.4157 0.2680 0.9280 0.022 Uiso 1 1 calc R U . . .
C29 C 0.4639(2) 0.2811(2) 0.81175(14) 0.0198(5) Uani 1 1 d . . . . .
H29A H 0.5373 0.2164 0.8159 0.024 Uiso 1 1 calc R U . . .
H29B H 0.4253 0.2646 0.7748 0.024 Uiso 1 1 calc R U . . .
C30 C 0.4770(2) 0.4598(2) 0.71396(14) 0.0186(5) Uani 1 1 d . . . . .
H30A H 0.5075 0.5380 0.6975 0.022 Uiso 1 1 calc R U . . .
H30B H 0.3850 0.4769 0.7202 0.022 Uiso 1 1 calc R U . . .
C31 C 0.5393(2) 0.3802(2) 0.65389(14) 0.0191(5) Uani 1 1 d . . . . .
C32 C 0.6688(2) 0.3360(2) 0.63883(14) 0.0188(5) Uani 1 1 d . . . . .
C33 C 0.7310(2) 0.2706(2) 0.57808(14) 0.0201(5) Uani 1 1 d . . . . .
C34 C 0.6569(3) 0.2497(2) 0.53577(14) 0.0225(5) Uani 1 1 d . . . . .
H34 H 0.6974 0.2052 0.4948 0.027 Uiso 1 1 calc R U . . .
C35 C 0.5274(3) 0.2902(2) 0.55017(14) 0.0209(5) Uani 1 1 d . . . . .
C36 C 0.4701(2) 0.3562(2) 0.60991(15) 0.0209(5) Uani 1 1 d . . . . .
H36 H 0.3820 0.3856 0.6210 0.025 Uiso 1 1 calc R U . . .
C37 C 0.8747(3) 0.2272(2) 0.55815(15) 0.0239(5) Uani 1 1 d . . . . .
C38 C 0.9225(3) 0.1675(3) 0.48617(17) 0.0331(6) Uani 1 1 d . . . . .
H38A H 0.8834 0.0964 0.4939 0.050 Uiso 1 1 calc R U . . .
H38B H 1.0142 0.1426 0.4749 0.050 Uiso 1 1 calc R U . . .
H38C H 0.9006 0.2256 0.4438 0.050 Uiso 1 1 calc R U . . .
C39 C 0.9413(3) 0.3361(3) 0.54387(17) 0.0321(6) Uani 1 1 d . . . . .
H39A H 0.9136 0.3976 0.5046 0.048 Uiso 1 1 calc R U . . .
H39B H 1.0326 0.3093 0.5272 0.048 Uiso 1 1 calc R U . . .
H39C H 0.9202 0.3707 0.5907 0.048 Uiso 1 1 calc R U . . .
C40 C 0.9118(3) 0.1336(3) 0.62286(18) 0.0359(7) Uani 1 1 d . . . . .
H40A H 0.8850 0.1703 0.6693 0.054 Uiso 1 1 calc R U . . .
H40B H 1.0034 0.1072 0.6096 0.054 Uiso 1 1 calc R U . . .
H40C H 0.8708 0.0636 0.6309 0.054 Uiso 1 1 calc R U . . .
C41 C 0.4487(3) 0.2609(3) 0.50425(15) 0.0262(6) Uani 1 1 d . . . . .
C42 C 0.3864(4) 0.1529(3) 0.5491(2) 0.0465(9) Uani 1 1 d . . . . .
H42A H 0.3314 0.1364 0.5220 0.070 Uiso 1 1 calc R U . . .
H42B H 0.3365 0.1717 0.5993 0.070 Uiso 1 1 calc R U . . .
H42C H 0.4515 0.0814 0.5545 0.070 Uiso 1 1 calc R U . . .
C43 C 0.5303(3) 0.2297(4) 0.42676(19) 0.0461(9) Uani 1 1 d . . . . .
H43A H 0.5732 0.2973 0.3990 0.069 Uiso 1 1 calc R U . . .
H43B H 0.4770 0.2151 0.3980 0.069 Uiso 1 1 calc R U . . .
H43C H 0.5930 0.1567 0.4337 0.069 Uiso 1 1 calc R U . . .
C44 C 0.3450(3) 0.3691(3) 0.49126(19) 0.0373(7) Uani 1 1 d . . . . .
H44A H 0.3826 0.4415 0.4682 0.056 Uiso 1 1 calc R U . . .
H44B H 0.2843 0.3831 0.5398 0.056 Uiso 1 1 calc R U . . .
H44C H 0.3018 0.3517 0.4575 0.056 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
Zr1 O1 1.9229(18) . ?
Zr1 O2 1.9300(17) . ?
Zr1 O4 1.9890(18) . ?
Zr1 O3 2.0181(18) . ?
Zr1 N1 2.420(2) . ?
O1 C1 1.412(3) . ?
N1 C30 1.492(3) . ?
N1 C29 1.501(3) . ?
N1 C23 1.510(3) . ?
C1 C4 1.514(4) . ?
C1 C3 1.517(4) . ?
C1 C2 1.522(4) . ?
O2 C5 1.414(3) . ?
N2 C23 1.459(3) . ?
N2 C24 1.469(3) . ?
N2 C28 1.474(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C9 1.353(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
O4 C32 1.350(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C8 1.516(4) . ?
C5 C6 1.517(5) . ?
C5 C7 1.527(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.405(3) . ?
C9 C14 1.408(3) . ?
C10 C11 1.388(3) . ?
C10 C23 1.506(3) . ?
C11 C12 1.397(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(4) . ?
C12 C15 1.532(3) . ?
C13 C14 1.398(4) . ?
C13 H13 0.9500 . ?
C14 C19 1.536(4) . ?
C15 C18 1.514(4) . ?
C15 C17 1.518(4) . ?
C15 C16 1.556(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C22 1.532(4) . ?
C19 C20 1.535(4) . ?
C19 C21 1.541(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C24 C25 1.523(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.529(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.530(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.511(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.511(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.500(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.395(4) . ?
C31 C32 1.400(4) . ?
C32 C33 1.409(4) . ?
C33 C34 1.400(4) . ?
C33 C37 1.541(4) . ?
C34 C35 1.394(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(4) . ?
C35 C41 1.537(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.534(4) . ?
C37 C40 1.537(4) . ?
C37 C39 1.540(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C43 1.532(4) . ?
C41 C42 1.533(4) . ?
C41 C44 1.536(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 O2 104.28(8) . . ?
O1 Zr1 O4 96.16(8) . . ?
O2 Zr1 O4 116.18(8) . . ?
O1 Zr1 O3 97.63(8) . . ?
O2 Zr1 O3 113.98(8) . . ?
O4 Zr1 O3 122.23(8) . . ?
O1 Zr1 N1 168.83(7) . . ?
O2 Zr1 N1 86.77(7) . . ?
O4 Zr1 N1 77.11(7) . . ?
O3 Zr1 N1 78.97(7) . . ?
C1 O1 Zr1 175.59(18) . . ?
C30 N1 C29 109.81(19) . . ?
C30 N1 C23 112.41(18) . . ?
C29 N1 C23 104.35(18) . . ?
C30 N1 Zr1 107.83(14) . . ?
C29 N1 Zr1 118.18(14) . . ?
C23 N1 Zr1 104.20(13) . . ?
O1 C1 C4 107.5(2) . . ?
O1 C1 C3 108.7(2) . . ?
C4 C1 C3 111.7(3) . . ?
O1 C1 C2 107.8(2) . . ?
C4 C1 C2 111.2(3) . . ?
C3 C1 C2 110.0(3) . . ?
C5 O2 Zr1 163.41(18) . . ?
C23 N2 C24 114.9(2) . . ?
C23 N2 C28 100.94(18) . . ?
C24 N2 C28 109.45(19) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C9 O3 Zr1 141.00(16) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C32 O4 Zr1 144.91(16) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C5 C8 108.2(3) . . ?
O2 C5 C6 109.0(2) . . ?
C8 C5 C6 110.8(3) . . ?
O2 C5 C7 107.8(3) . . ?
C8 C5 C7 110.5(3) . . ?
C6 C5 C7 110.5(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C9 C10 117.9(2) . . ?
O3 C9 C14 121.9(2) . . ?
C10 C9 C14 120.2(2) . . ?
C11 C10 C9 120.5(2) . . ?
C11 C10 C23 124.1(2) . . ?
C9 C10 C23 115.3(2) . . ?
C10 C11 C12 120.9(2) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 117.2(2) . . ?
C13 C12 C15 122.5(2) . . ?
C11 C12 C15 120.2(2) . . ?
C14 C13 C12 124.0(2) . . ?
C14 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
C13 C14 C9 116.9(2) . . ?
C13 C14 C19 121.7(2) . . ?
C9 C14 C19 121.4(2) . . ?
C18 C15 C17 108.8(3) . . ?
C18 C15 C12 113.6(2) . . ?
C17 C15 C12 110.5(2) . . ?
C18 C15 C16 107.4(3) . . ?
C17 C15 C16 107.5(3) . . ?
C12 C15 C16 108.8(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C19 C20 108.2(3) . . ?
C22 C19 C14 111.8(2) . . ?
C20 C19 C14 110.7(2) . . ?
C22 C19 C21 107.3(3) . . ?
C20 C19 C21 109.5(3) . . ?
C14 C19 C21 109.4(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 C10 118.1(2) . . ?
N2 C23 N1 103.92(18) . . ?
C10 C23 N1 112.00(19) . . ?
N2 C23 H23 107.4 . . ?
C10 C23 H23 107.4 . . ?
N1 C23 H23 107.4 . . ?
N2 C24 C25 109.2(2) . . ?
N2 C24 H24A 109.8 . . ?
C25 C24 H24A 109.8 . . ?
N2 C24 H24B 109.8 . . ?
C25 C24 H24B 109.8 . . ?
H24A C24 H24B 108.3 . . ?
C24 C25 C26 112.7(2) . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 C27 111.0(2) . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C26 108.5(2) . . ?
C28 C27 H27A 110.0 . . ?
C26 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
C26 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
N2 C28 C27 110.7(2) . . ?
N2 C28 C29 102.75(19) . . ?
C27 C28 C29 117.0(2) . . ?
N2 C28 H28 108.7 . . ?
C27 C28 H28 108.7 . . ?
C29 C28 H28 108.7 . . ?
N1 C29 C28 104.79(19) . . ?
N1 C29 H29A 110.8 . . ?
C28 C29 H29A 110.8 . . ?
N1 C29 H29B 110.8 . . ?
C28 C29 H29B 110.8 . . ?
H29A C29 H29B 108.9 . . ?
N1 C30 C31 112.3(2) . . ?
N1 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
N1 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C36 C31 C32 119.8(2) . . ?
C36 C31 C30 120.3(2) . . ?
C32 C31 C30 119.8(2) . . ?
O4 C32 C31 118.2(2) . . ?
O4 C32 C33 121.1(2) . . ?
C31 C32 C33 120.6(2) . . ?
C34 C33 C32 117.0(2) . . ?
C34 C33 C37 121.8(2) . . ?
C32 C33 C37 121.3(2) . . ?
C35 C34 C33 123.9(2) . . ?
C35 C34 H34 118.0 . . ?
C33 C34 H34 118.0 . . ?
C36 C35 C34 117.2(2) . . ?
C36 C35 C41 120.6(2) . . ?
C34 C35 C41 122.2(2) . . ?
C35 C36 C31 121.4(2) . . ?
C35 C36 H36 119.3 . . ?
C31 C36 H36 119.3 . . ?
C38 C37 C40 107.7(2) . . ?
C38 C37 C33 111.9(2) . . ?
C40 C37 C33 110.3(2) . . ?
C38 C37 C39 107.4(2) . . ?
C40 C37 C39 109.7(3) . . ?
C33 C37 C39 109.7(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C41 C42 109.4(3) . . ?
C43 C41 C44 108.0(3) . . ?
C42 C41 C44 108.5(3) . . ?
C43 C41 C35 111.5(2) . . ?
C42 C41 C35 108.5(2) . . ?
C44 C41 C35 110.9(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_refine_diff_density_max         0.592
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_s16mdj60
_database_code_depnum_ccdc_archive 'CCDC 1534479'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H68 N4 O4 Ti'
_chemical_formula_weight         812.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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                   10.4459(5)
_cell_length_b                   30.1019(4)
_cell_length_c                   14.9279(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.009(3)
_cell_angle_gamma                90
_cell_volume                     4573.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    31803
_cell_measurement_theta_min      3.3810
_cell_measurement_theta_max      72.9380

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_F_000             1752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.939
_shelx_estimated_absorpt_T_min   0.594
_shelx_estimated_absorpt_T_max   0.643
_exptl_absorpt_correction_T_min  0.80696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            63922
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.936
_diffrn_reflns_theta_max         73.097
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9133
_reflns_number_gt                8793
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0541P)²+2.6099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9133
_refine_ls_number_parameters     534
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Ti1 Ti 0.28334(2) 0.12949(2) 0.78808(2) 0.01835(8) Uani 1 1 d . . . . .
O1 O 0.18485(11) 0.18160(4) 0.76744(8) 0.0278(2) Uani 1 1 d . . . . .
N1 N 0.46088(12) 0.17281(4) 0.79845(8) 0.0196(2) Uani 1 1 d . . . . .
C1 C 0.13165(18) 0.21009(6) 0.69415(13) 0.0352(4) Uani 1 1 d . . . . .
H1 H 0.1140 0.1927 0.6355 0.042 Uiso 1 1 calc R U . . .
O2 O 0.14694(10) 0.09187(4) 0.78933(8) 0.0261(2) Uani 1 1 d . . . . .
N2 N 0.32050(12) 0.15553(4) 0.93068(9) 0.0201(2) Uani 1 1 d . . . . .
C2 C 0.2270(2) 0.24716(7) 0.68788(15) 0.0440(5) Uani 1 1 d . . . . .
H2A H 0.2460 0.2640 0.7455 0.066 Uiso 1 1 calc R U . . .
H2B H 0.1881 0.2670 0.6369 0.066 Uiso 1 1 calc R U . . .
H2C H 0.3087 0.2345 0.6772 0.066 Uiso 1 1 calc R U . . .
O3 O 0.30525(10) 0.12111(4) 0.66652(7) 0.0247(2) Uani 1 1 d . . . . .
N3 N 0.61926(14) 0.26348(4) 0.93692(10) 0.0289(3) Uani 1 1 d . . . . .
C3 C 0.0027(2) 0.22880(7) 0.70888(17) 0.0499(5) Uani 1 1 d . . . . .
H3A H -0.0569 0.2043 0.7143 0.075 Uiso 1 1 calc R U . . .
H3B H -0.0376 0.2476 0.6565 0.075 Uiso 1 1 calc R U . . .
H3C H 0.0195 0.2466 0.7653 0.075 Uiso 1 1 calc R U . . .
O4 O 0.41669(10) 0.08936(3) 0.84834(7) 0.0211(2) Uani 1 1 d . . . . .
N4 N 0.18432(14) 0.19132(5) 1.06125(10) 0.0302(3) Uani 1 1 d . . . . .
C4 C 0.01043(16) 0.09561(6) 0.74984(14) 0.0342(4) Uani 1 1 d . . . . .
H4 H -0.0020 0.1191 0.7013 0.041 Uiso 1 1 calc R U . . .
C5 C -0.04009(19) 0.05253(7) 0.70486(15) 0.0448(5) Uani 1 1 d . . . . .
H5A H 0.0090 0.0449 0.6582 0.067 Uiso 1 1 calc R U . . .
H5B H -0.1336 0.0556 0.6756 0.067 Uiso 1 1 calc R U . . .
H5C H -0.0287 0.0290 0.7514 0.067 Uiso 1 1 calc R U . . .
C6 C -0.0608(2) 0.10994(9) 0.8218(2) 0.0635(8) Uani 1 1 d . . . . .
H6A H -0.0524 0.0869 0.8691 0.095 Uiso 1 1 calc R U . . .
H6B H -0.1539 0.1146 0.7933 0.095 Uiso 1 1 calc R U . . .
H6C H -0.0226 0.1377 0.8500 0.095 Uiso 1 1 calc R U . . .
C7 C 0.39836(15) 0.12481(5) 0.61962(10) 0.0216(3) Uani 1 1 d . . . . .
C8 C 0.38675(15) 0.10159(5) 0.53529(11) 0.0258(3) Uani 1 1 d . . . . .
C9 C 0.48549(16) 0.10799(6) 0.48766(11) 0.0286(3) Uani 1 1 d . . . . .
H9 H 0.4776 0.0929 0.4308 0.034 Uiso 1 1 calc R U . . .
C10 C 0.59616(16) 0.13520(5) 0.51795(11) 0.0269(3) Uani 1 1 d . . . . .
C11 C 0.60637(15) 0.15639(5) 0.60078(11) 0.0237(3) Uani 1 1 d . . . . .
H11 H 0.6807 0.1746 0.6239 0.028 Uiso 1 1 calc R U . . .
C12 C 0.50953(14) 0.15178(5) 0.65236(10) 0.0218(3) Uani 1 1 d . . . . .
C13 C 0.27151(18) 0.06947(6) 0.50022(12) 0.0338(4) Uani 1 1 d . . . . .
C14 C 0.13905(18) 0.09398(7) 0.48245(14) 0.0413(4) Uani 1 1 d . . . . .
H14A H 0.1302 0.1093 0.5386 0.062 Uiso 1 1 calc R U . . .
H14B H 0.0674 0.0725 0.4644 0.062 Uiso 1 1 calc R U . . .
H14C H 0.1352 0.1157 0.4330 0.062 Uiso 1 1 calc R U . . .
C15 C 0.2730(2) 0.03256(6) 0.57106(16) 0.0448(5) Uani 1 1 d . . . . .
H15A H 0.3564 0.0164 0.5808 0.067 Uiso 1 1 calc R U . . .
H15B H 0.2001 0.0120 0.5484 0.067 Uiso 1 1 calc R U . . .
H15C H 0.2634 0.0457 0.6293 0.067 Uiso 1 1 calc R U . . .
C16 C 0.2815(2) 0.04734(9) 0.40906(16) 0.0564(6) Uani 1 1 d . . . . .
H16A H 0.2804 0.0703 0.3623 0.085 Uiso 1 1 calc R U . . .
H16B H 0.2069 0.0272 0.3887 0.085 Uiso 1 1 calc R U . . .
H16C H 0.3637 0.0305 0.4182 0.085 Uiso 1 1 calc R U . . .
C17 C 0.69812(17) 0.14041(7) 0.45896(12) 0.0337(4) Uani 1 1 d . . . . .
C18 C 0.6316(3) 0.15861(11) 0.36495(17) 0.0664(8) Uani 1 1 d . . . . .
H18A H 0.5663 0.1372 0.3331 0.100 Uiso 1 1 calc R U . . .
H18B H 0.6976 0.1636 0.3287 0.100 Uiso 1 1 calc R U . . .
H18C H 0.5879 0.1867 0.3725 0.100 Uiso 1 1 calc R U . . .
C19 C 0.7582(2) 0.09525(9) 0.44577(19) 0.0586(6) Uani 1 1 d . . . . .
H19A H 0.8019 0.0832 0.5058 0.088 Uiso 1 1 calc R U . . .
H19B H 0.8224 0.0988 0.4075 0.088 Uiso 1 1 calc R U . . .
H19C H 0.6886 0.0749 0.4155 0.088 Uiso 1 1 calc R U . . .
C20 C 0.8104(3) 0.17154(11) 0.5026(2) 0.0710(8) Uani 1 1 d . . . . .
H20A H 0.7755 0.2014 0.5078 0.107 Uiso 1 1 calc R U . . .
H20B H 0.8749 0.1726 0.4641 0.107 Uiso 1 1 calc R U . . .
H20C H 0.8528 0.1606 0.5639 0.107 Uiso 1 1 calc R U . . .
C21 C 0.53162(14) 0.17567(5) 0.73901(10) 0.0216(3) Uani 1 1 d . . . . .
H21 H 0.6050 0.1951 0.7527 0.026 Uiso 1 1 calc R U . . .
C22 C 0.49053(14) 0.19891(5) 0.88444(10) 0.0203(3) Uani 1 1 d . . . . .
H22 H 0.4242 0.2234 0.8765 0.024 Uiso 1 1 calc R U . . .
C23 C 0.62410(15) 0.22069(5) 0.91237(10) 0.0227(3) Uani 1 1 d . . . . .
C24 C 0.74179(16) 0.19831(6) 0.91573(11) 0.0272(3) Uani 1 1 d . . . . .
H24 H 0.7417 0.1678 0.8990 0.033 Uiso 1 1 calc R U . . .
C25 C 0.85926(17) 0.22126(7) 0.94388(12) 0.0342(4) Uani 1 1 d . . . . .
H25 H 0.9409 0.2069 0.9460 0.041 Uiso 1 1 calc R U . . .
C26 C 0.85497(18) 0.26539(7) 0.96871(12) 0.0382(4) Uani 1 1 d . . . . .
H26 H 0.9336 0.2821 0.9877 0.046 Uiso 1 1 calc R U . . .
C27 C 0.73441(19) 0.28459(6) 0.96527(12) 0.0370(4) Uani 1 1 d . . . . .
H27 H 0.7326 0.3147 0.9842 0.044 Uiso 1 1 calc R U . . .
C28 C 0.46147(14) 0.16802(5) 0.96040(10) 0.0193(3) Uani 1 1 d . . . . .
H28 H 0.4745 0.1852 1.0191 0.023 Uiso 1 1 calc R U . . .
C29 C 0.27617(15) 0.12806(5) 1.00008(11) 0.0237(3) Uani 1 1 d . . . . .
H29A H 0.3409 0.1041 1.0211 0.028 Uiso 1 1 calc R U . . .
H29B H 0.1911 0.1140 0.9715 0.028 Uiso 1 1 calc R U . . .
C30 C 0.26039(14) 0.15526(5) 1.08186(11) 0.0233(3) Uani 1 1 d . . . . .
C31 C 0.31641(17) 0.14294(6) 1.17167(12) 0.0308(3) Uani 1 1 d . . . . .
H31 H 0.3722 0.1177 1.1841 0.037 Uiso 1 1 calc R U . . .
C32 C 0.28934(19) 0.16821(6) 1.24307(12) 0.0359(4) Uani 1 1 d . . . . .
H32 H 0.3252 0.1602 1.3052 0.043 Uiso 1 1 calc R U . . .
C33 C 0.20992(18) 0.20491(6) 1.22242(12) 0.0358(4) Uani 1 1 d . . . . .
H33 H 0.1893 0.2227 1.2699 0.043 Uiso 1 1 calc R U . . .
C34 C 0.16099(18) 0.21535(6) 1.13124(13) 0.0357(4) Uani 1 1 d . . . . .
H34 H 0.1076 0.2411 1.1173 0.043 Uiso 1 1 calc R U . . .
C35 C 0.52679(14) 0.09137(5) 0.91486(10) 0.0194(3) Uani 1 1 d . . . . .
C36 C 0.54927(14) 0.12746(5) 0.97616(10) 0.0200(3) Uani 1 1 d . . . . .
C37 C 0.65826(15) 0.12777(5) 1.05028(10) 0.0223(3) Uani 1 1 d . . . . .
H37 H 0.6694 0.1517 1.0928 0.027 Uiso 1 1 calc R U . . .
C38 C 0.75051(14) 0.09386(5) 1.06309(11) 0.0240(3) Uani 1 1 d . . . . .
C39 C 0.72919(15) 0.05937(5) 0.99899(11) 0.0248(3) Uani 1 1 d . . . . .
H39 H 0.7924 0.0362 1.0064 0.030 Uiso 1 1 calc R U . . .
C40 C 0.62115(14) 0.05669(5) 0.92485(11) 0.0218(3) Uani 1 1 d . . . . .
C41 C 0.87146(15) 0.09321(6) 1.14366(12) 0.0300(3) Uani 1 1 d . . . . .
C42 C 0.8913(2) 0.13740(7) 1.19527(15) 0.0458(5) Uani 1 1 d . . . . .
H42A H 0.9711 0.1359 1.2444 0.069 Uiso 1 1 calc R U . . .
H42B H 0.8154 0.1433 1.2219 0.069 Uiso 1 1 calc R U . . .
H42C H 0.9000 0.1613 1.1525 0.069 Uiso 1 1 calc R U . . .
C43 C 0.8546(2) 0.05698(9) 1.21124(16) 0.0594(7) Uani 1 1 d . . . . .
H43A H 0.8467 0.0281 1.1803 0.089 Uiso 1 1 calc R U . . .
H43B H 0.7751 0.0628 1.2338 0.089 Uiso 1 1 calc R U . . .
H43C H 0.9311 0.0568 1.2631 0.089 Uiso 1 1 calc R U . . .
C44 C 0.99476(19) 0.08498(10) 1.10752(18) 0.0610(7) Uani 1 1 d . . . . .
H44A H 0.9895 0.0556 1.0787 0.091 Uiso 1 1 calc R U . . .
H44B H 1.0722 0.0863 1.1586 0.091 Uiso 1 1 calc R U . . .
H44C H 1.0018 0.1078 1.0620 0.091 Uiso 1 1 calc R U . . .
C45 C 0.60468(16) 0.01840(5) 0.85548(12) 0.0263(3) Uani 1 1 d . . . . .
C46 C 0.59264(18) 0.03690(6) 0.75774(12) 0.0331(4) Uani 1 1 d . . . . .
H46A H 0.5837 0.0122 0.7139 0.050 Uiso 1 1 calc R U . . .
H46B H 0.6715 0.0541 0.7555 0.050 Uiso 1 1 calc R U . . .
H46C H 0.5151 0.0561 0.7416 0.050 Uiso 1 1 calc R U . . .
C47 C 0.48208(18) -0.00904(6) 0.85923(14) 0.0365(4) Uani 1 1 d . . . . .
H47A H 0.4695 -0.0322 0.8118 0.055 Uiso 1 1 calc R U . . .
H47B H 0.4050 0.0104 0.8484 0.055 Uiso 1 1 calc R U . . .
H47C H 0.4936 -0.0229 0.9199 0.055 Uiso 1 1 calc R U . . .
C48 C 0.72387(19) -0.01279(6) 0.87491(14) 0.0381(4) Uani 1 1 d . . . . .
H48A H 0.7329 -0.0263 0.9358 0.057 Uiso 1 1 calc R U . . .
H48B H 0.8034 0.0042 0.8732 0.057 Uiso 1 1 calc R U . . .
H48C H 0.7114 -0.0362 0.8281 0.057 Uiso 1 1 calc R U . . .
H2 H 0.273(2) 0.1785(7) 0.9228(14) 0.030(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.8233(11) . ?
Ti1 O1 1.8631(11) . ?
Ti1 O3 1.8962(11) . ?
Ti1 O4 1.9091(10) . ?
Ti1 N2 2.2192(13) . ?
Ti1 N1 2.2440(12) . ?
O1 C1 1.403(2) . ?
N1 C21 1.2790(19) . ?
N1 C22 1.4770(18) . ?
C1 C2 1.513(3) . ?
C1 C3 1.521(3) . ?
O2 C4 1.4196(19) . ?
N2 C29 1.4790(19) . ?
N2 C28 1.4875(18) . ?
O3 C7 1.3249(19) . ?
N3 C27 1.342(2) . ?
N3 C23 1.343(2) . ?
O4 C35 1.3409(18) . ?
N4 C34 1.338(2) . ?
N4 C30 1.339(2) . ?
C4 C5 1.501(3) . ?
C4 C6 1.501(3) . ?
C7 C12 1.411(2) . ?
C7 C8 1.421(2) . ?
C8 C9 1.392(2) . ?
C8 C13 1.541(2) . ?
C9 C10 1.406(2) . ?
C10 C11 1.374(2) . ?
C10 C17 1.535(2) . ?
C11 C12 1.409(2) . ?
C12 C21 1.452(2) . ?
C13 C15 1.532(3) . ?
C13 C14 1.537(3) . ?
C13 C16 1.540(2) . ?
C17 C18 1.521(3) . ?
C17 C20 1.528(3) . ?
C17 C19 1.528(3) . ?
C22 C23 1.513(2) . ?
C22 C28 1.548(2) . ?
C23 C24 1.393(2) . ?
C24 C25 1.388(2) . ?
C25 C26 1.383(3) . ?
C26 C27 1.376(3) . ?
C28 C36 1.5134(19) . ?
C29 C30 1.509(2) . ?
C30 C31 1.387(2) . ?
C31 C32 1.389(2) . ?
C32 C33 1.374(3) . ?
C33 C34 1.378(3) . ?
C35 C36 1.406(2) . ?
C35 C40 1.420(2) . ?
C36 C37 1.398(2) . ?
C37 C38 1.387(2) . ?
C38 C39 1.395(2) . ?
C38 C41 1.536(2) . ?
C39 C40 1.394(2) . ?
C40 C45 1.533(2) . ?
C41 C43 1.523(3) . ?
C41 C44 1.524(3) . ?
C41 C42 1.528(3) . ?
C45 C48 1.534(2) . ?
C45 C47 1.535(2) . ?
C45 C46 1.540(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 96.94(5) . . ?
O2 Ti1 O3 100.96(5) . . ?
O1 Ti1 O3 97.75(5) . . ?
O2 Ti1 O4 95.24(5) . . ?
O1 Ti1 O4 158.09(5) . . ?
O3 Ti1 O4 97.72(5) . . ?
O2 Ti1 N2 100.24(5) . . ?
O1 Ti1 N2 80.33(5) . . ?
O3 Ti1 N2 158.78(5) . . ?
O4 Ti1 N2 79.63(5) . . ?
O2 Ti1 N1 174.78(5) . . ?
O1 Ti1 N1 86.51(5) . . ?
O3 Ti1 N1 82.38(5) . . ?
O4 Ti1 N1 80.28(4) . . ?
N2 Ti1 N1 76.41(5) . . ?
C1 O1 Ti1 138.66(11) . . ?
C21 N1 C22 121.76(12) . . ?
C21 N1 Ti1 126.07(10) . . ?
C22 N1 Ti1 112.18(9) . . ?
O1 C1 C2 110.40(15) . . ?
O1 C1 C3 108.78(16) . . ?
C2 C1 C3 110.66(17) . . ?
C4 O2 Ti1 131.35(11) . . ?
C29 N2 C28 112.18(12) . . ?
C29 N2 Ti1 117.37(9) . . ?
C28 N2 Ti1 108.85(8) . . ?
C7 O3 Ti1 139.09(10) . . ?
C27 N3 C23 117.00(15) . . ?
C35 O4 Ti1 137.19(9) . . ?
C34 N4 C30 117.51(15) . . ?
O2 C4 C5 109.66(15) . . ?
O2 C4 C6 109.81(16) . . ?
C5 C4 C6 112.80(17) . . ?
O3 C7 C12 120.67(13) . . ?
O3 C7 C8 120.03(14) . . ?
C12 C7 C8 119.30(14) . . ?
C9 C8 C7 117.35(14) . . ?
C9 C8 C13 121.69(14) . . ?
C7 C8 C13 120.93(14) . . ?
C8 C9 C10 124.51(15) . . ?
C11 C10 C9 116.84(15) . . ?
C11 C10 C17 123.06(15) . . ?
C9 C10 C17 120.09(15) . . ?
C10 C11 C12 121.75(15) . . ?
C11 C12 C7 120.21(14) . . ?
C11 C12 C21 116.64(13) . . ?
C7 C12 C21 123.15(13) . . ?
C15 C13 C14 109.63(16) . . ?
C15 C13 C16 107.72(17) . . ?
C14 C13 C16 107.01(17) . . ?
C15 C13 C8 109.58(15) . . ?
C14 C13 C8 111.18(14) . . ?
C16 C13 C8 111.62(15) . . ?
C18 C17 C20 108.7(2) . . ?
C18 C17 C19 108.48(19) . . ?
C20 C17 C19 107.6(2) . . ?
C18 C17 C10 109.52(15) . . ?
C20 C17 C10 112.52(16) . . ?
C19 C17 C10 109.94(16) . . ?
N1 C21 C12 125.72(14) . . ?
N1 C22 C23 118.04(12) . . ?
N1 C22 C28 106.25(11) . . ?
C23 C22 C28 112.28(12) . . ?
N3 C23 C24 122.77(14) . . ?
N3 C23 C22 113.70(14) . . ?
C24 C23 C22 123.50(14) . . ?
C25 C24 C23 118.87(16) . . ?
C26 C25 C24 118.66(17) . . ?
C27 C26 C25 118.57(16) . . ?
N3 C27 C26 124.11(17) . . ?
N2 C28 C36 111.53(12) . . ?
N2 C28 C22 106.11(11) . . ?
C36 C28 C22 112.73(12) . . ?
N2 C29 C30 111.82(12) . . ?
N4 C30 C31 122.54(15) . . ?
N4 C30 C29 114.89(14) . . ?
C31 C30 C29 122.52(15) . . ?
C30 C31 C32 118.74(16) . . ?
C33 C32 C31 119.00(16) . . ?
C32 C33 C34 118.42(16) . . ?
N4 C34 C33 123.76(17) . . ?
O4 C35 C36 120.44(13) . . ?
O4 C35 C40 120.26(13) . . ?
C36 C35 C40 119.29(13) . . ?
C37 C36 C35 120.50(13) . . ?
C37 C36 C28 118.35(13) . . ?
C35 C36 C28 121.05(13) . . ?
C38 C37 C36 121.40(14) . . ?
C37 C38 C39 117.02(14) . . ?
C37 C38 C41 122.73(15) . . ?
C39 C38 C41 120.25(14) . . ?
C40 C39 C38 124.28(14) . . ?
C39 C40 C35 117.36(14) . . ?
C39 C40 C45 121.84(13) . . ?
C35 C40 C45 120.79(14) . . ?
C43 C41 C44 110.6(2) . . ?
C43 C41 C42 108.19(18) . . ?
C44 C41 C42 106.90(17) . . ?
C43 C41 C38 109.30(14) . . ?
C44 C41 C38 109.66(15) . . ?
C42 C41 C38 112.22(14) . . ?
C40 C45 C48 111.69(14) . . ?
C40 C45 C47 110.33(13) . . ?
C48 C45 C47 108.18(14) . . ?
C40 C45 C46 109.92(13) . . ?
C48 C45 C46 106.87(14) . . ?
C47 C45 C46 109.77(15) . . ?

_refine_diff_density_max         0.447
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_s16mdj47
_database_code_depnum_ccdc_archive 'CCDC 1534475'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H70 N2 O4 Ti'
_chemical_formula_weight         714.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6663(4)
_cell_length_b                   13.5176(5)
_cell_length_c                   14.0421(4)
_cell_angle_alpha                100.146(3)
_cell_angle_beta                 92.922(2)
_cell_angle_gamma                107.314(3)
_cell_volume                     2068.41(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12890
_cell_measurement_theta_min      4.4100
_cell_measurement_theta_max      73.3340

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.058
_shelx_estimated_absorpt_T_min   0.748
_shelx_estimated_absorpt_T_max   0.904
_exptl_absorpt_correction_T_min  0.73320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.638
_oxdiff_exptl_absorpt_empirical_full_max 1.939
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            25143
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.217
_diffrn_reflns_theta_max         73.488
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8285
_reflns_number_gt                7496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0589P)²+0.5855P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8285
_refine_ls_number_parameters     462
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.19371(2) 0.36040(2) 0.19205(2) 0.02032(8) Uani 1 1 d . . . . .
O1 O 0.08521(11) 0.23054(10) 0.18089(9) 0.0338(3) Uani 1 1 d . . . . .
N1 N 0.32788(10) 0.53420(10) 0.25601(9) 0.0199(3) Uani 1 1 d . . . . .
C1 C 0.03982(17) 0.13142(14) 0.11581(14) 0.0360(4) Uani 1 1 d . . . . .
H1 H 0.0805 0.1367 0.0551 0.043 Uiso 1 1 calc R U . . .
O2 O 0.18437(11) 0.39273(10) 0.07420(8) 0.0318(3) Uani 1 1 d . . . . .
N2 N 0.25712(11) 0.35864(10) 0.34784(9) 0.0212(3) Uani 1 1 d . . . . .
C2 C -0.0938(2) 0.1088(2) 0.0897(2) 0.0805(11) Uani 1 1 d . . . . .
H2A H -0.1356 0.1012 0.1480 0.121 Uiso 1 1 calc R U . . .
H2B H -0.1251 0.0431 0.0407 0.121 Uiso 1 1 calc R U . . .
H2C H -0.1074 0.1673 0.0633 0.121 Uiso 1 1 calc R U . . .
O3 O 0.08578(9) 0.42753(9) 0.25322(8) 0.0247(2) Uani 1 1 d . . . . .
C3 C 0.0708(4) 0.04859(18) 0.1605(2) 0.0864(11) Uani 1 1 d . . . . .
H3A H 0.1586 0.0682 0.1751 0.130 Uiso 1 1 calc R U . . .
H3B H 0.0412 -0.0196 0.1148 0.130 Uiso 1 1 calc R U . . .
H3C H 0.0327 0.0430 0.2207 0.130 Uiso 1 1 calc R U . . .
O4 O 0.33041(10) 0.31192(9) 0.17179(8) 0.0249(2) Uani 1 1 d . . . . .
C4 C 0.14504(18) 0.41614(17) -0.01309(13) 0.0400(4) Uani 1 1 d . . . . .
H4 H 0.1560 0.4937 -0.0024 0.048 Uiso 1 1 calc R U . . .
C5 C 0.2216(2) 0.3892(2) -0.09123(15) 0.0497(5) Uani 1 1 d . . . . .
H5A H 0.3070 0.4271 -0.0691 0.075 Uiso 1 1 calc R U . . .
H5B H 0.1985 0.4102 -0.1509 0.075 Uiso 1 1 calc R U . . .
H5C H 0.2089 0.3129 -0.1044 0.075 Uiso 1 1 calc R U . . .
C6 C 0.0122(2) 0.3562(3) -0.04064(19) 0.0729(9) Uani 1 1 d . . . . .
H6A H 0.0007 0.2800 -0.0540 0.109 Uiso 1 1 calc R U . . .
H6B H -0.0167 0.3761 -0.0989 0.109 Uiso 1 1 calc R U . . .
H6C H -0.0333 0.3735 0.0131 0.109 Uiso 1 1 calc R U . . .
C7 C 0.06784(13) 0.52077(12) 0.28038(11) 0.0210(3) Uani 1 1 d . . . . .
C8 C 0.15746(13) 0.61401(13) 0.27337(11) 0.0217(3) Uani 1 1 d . . . . .
C9 C 0.14206(13) 0.71215(13) 0.30630(11) 0.0233(3) Uani 1 1 d . . . . .
H9 H 0.2047 0.7746 0.3025 0.028 Uiso 1 1 calc R U . . .
C10 C 0.03720(14) 0.72066(13) 0.34454(12) 0.0248(3) Uani 1 1 d . . . . .
C11 C -0.05263(13) 0.62648(13) 0.34829(11) 0.0253(3) Uani 1 1 d . . . . .
H11 H -0.1255 0.6311 0.3731 0.030 Uiso 1 1 calc R U . . .
C12 C -0.04152(13) 0.52656(13) 0.31783(11) 0.0228(3) Uani 1 1 d . . . . .
C13 C 0.01797(15) 0.82743(14) 0.38284(13) 0.0297(3) Uani 1 1 d . . . . .
C14 C -0.09459(17) 0.83489(16) 0.32653(19) 0.0487(5) Uani 1 1 d . . . . .
H14A H -0.0825 0.8311 0.2576 0.073 Uiso 1 1 calc R U . . .
H14B H -0.1079 0.9022 0.3529 0.073 Uiso 1 1 calc R U . . .
H14C H -0.1651 0.7762 0.3332 0.073 Uiso 1 1 calc R U . . .
C15 C 0.0026(2) 0.83707(17) 0.49187(16) 0.0510(5) Uani 1 1 d . . . . .
H15A H -0.0680 0.7797 0.5009 0.076 Uiso 1 1 calc R U . . .
H15B H -0.0091 0.9053 0.5173 0.076 Uiso 1 1 calc R U . . .
H15C H 0.0749 0.8324 0.5269 0.076 Uiso 1 1 calc R U . . .
C16 C 0.12518(16) 0.92046(14) 0.37145(15) 0.0359(4) Uani 1 1 d . . . . .
H16A H 0.1975 0.9197 0.4096 0.054 Uiso 1 1 calc R U . . .
H16B H 0.1082 0.9868 0.3948 0.054 Uiso 1 1 calc R U . . .
H16C H 0.1387 0.9147 0.3027 0.054 Uiso 1 1 calc R U . . .
C17 C -0.14280(14) 0.42497(13) 0.32192(13) 0.0277(3) Uani 1 1 d . . . . .
C18 C -0.25684(17) 0.44802(17) 0.35608(18) 0.0463(5) Uani 1 1 d . . . . .
H18A H -0.2381 0.4907 0.4223 0.069 Uiso 1 1 calc R U . . .
H18B H -0.3201 0.3812 0.3555 0.069 Uiso 1 1 calc R U . . .
H18C H -0.2851 0.4869 0.3122 0.069 Uiso 1 1 calc R U . . .
C19 C -0.17941(15) 0.35465(15) 0.21964(14) 0.0368(4) Uani 1 1 d . . . . .
H19A H -0.1987 0.3958 0.1738 0.055 Uiso 1 1 calc R U . . .
H19B H -0.2504 0.2941 0.2210 0.055 Uiso 1 1 calc R U . . .
H19C H -0.1124 0.3293 0.1990 0.055 Uiso 1 1 calc R U . . .
C20 C -0.10094(18) 0.36423(16) 0.39175(15) 0.0419(4) Uani 1 1 d . . . . .
H20A H -0.0326 0.3430 0.3678 0.063 Uiso 1 1 calc R U . . .
H20B H -0.1675 0.3011 0.3956 0.063 Uiso 1 1 calc R U . . .
H20C H -0.0759 0.4097 0.4566 0.063 Uiso 1 1 calc R U . . .
C21 C 0.26934(13) 0.60952(12) 0.22566(11) 0.0227(3) Uani 1 1 d . . . . .
H21A H 0.2477 0.5897 0.1543 0.027 Uiso 1 1 calc R U . . .
H21B H 0.3290 0.6812 0.2404 0.027 Uiso 1 1 calc R U . . .
C22 C 0.44537(13) 0.54920(13) 0.21383(11) 0.0228(3) Uani 1 1 d . . . . .
H22A H 0.4309 0.5455 0.1430 0.027 Uiso 1 1 calc R U . . .
H22B H 0.4758 0.4900 0.2225 0.027 Uiso 1 1 calc R U . . .
C23 C 0.54324(14) 0.65344(14) 0.25847(12) 0.0278(3) Uani 1 1 d . . . . .
H23A H 0.5182 0.7134 0.2435 0.033 Uiso 1 1 calc R U . . .
H23B H 0.6194 0.6552 0.2298 0.033 Uiso 1 1 calc R U . . .
C24 C 0.56417(14) 0.66489(14) 0.36872(12) 0.0301(4) Uani 1 1 d . . . . .
H24A H 0.6215 0.7356 0.3975 0.036 Uiso 1 1 calc R U . . .
H24B H 0.6001 0.6109 0.3837 0.036 Uiso 1 1 calc R U . . .
C25 C 0.44475(14) 0.65122(13) 0.41337(11) 0.0257(3) Uani 1 1 d . . . . .
H25A H 0.4589 0.6513 0.4835 0.031 Uiso 1 1 calc R U . . .
H25B H 0.4162 0.7122 0.4076 0.031 Uiso 1 1 calc R U . . .
C26 C 0.34632(13) 0.54890(12) 0.36458(10) 0.0212(3) Uani 1 1 d . . . . .
H26 H 0.2688 0.5536 0.3893 0.025 Uiso 1 1 calc R U . . .
C27 C 0.36498(13) 0.44941(12) 0.38914(10) 0.0223(3) Uani 1 1 d . . . . .
H27A H 0.4375 0.4380 0.3615 0.027 Uiso 1 1 calc R U . . .
H27B H 0.3773 0.4568 0.4606 0.027 Uiso 1 1 calc R U . . .
C28 C 0.27154(14) 0.25615(13) 0.35852(11) 0.0239(3) Uani 1 1 d . . . . .
H28A H 0.1926 0.2004 0.3389 0.029 Uiso 1 1 calc R U . . .
H28B H 0.2946 0.2594 0.4281 0.029 Uiso 1 1 calc R U . . .
C29 C 0.36477(13) 0.22456(12) 0.29938(11) 0.0222(3) Uani 1 1 d . . . . .
C30 C 0.38492(13) 0.24973(12) 0.20702(11) 0.0215(3) Uani 1 1 d . . . . .
C31 C 0.46292(13) 0.20692(12) 0.15085(11) 0.0219(3) Uani 1 1 d . . . . .
C32 C 0.51927(13) 0.14382(12) 0.19084(11) 0.0228(3) Uani 1 1 d . . . . .
H32 H 0.5717 0.1153 0.1533 0.027 Uiso 1 1 calc R U . . .
C33 C 0.50292(13) 0.12020(12) 0.28303(11) 0.0224(3) Uani 1 1 d . . . . .
C34 C 0.42439(14) 0.16182(13) 0.33564(11) 0.0237(3) Uani 1 1 d . . . . .
H34 H 0.4110 0.1469 0.3985 0.028 Uiso 1 1 calc R U . . .
C35 C 0.47998(14) 0.22511(13) 0.04645(11) 0.0241(3) Uani 1 1 d . . . . .
C36 C 0.52552(16) 0.34313(14) 0.04463(12) 0.0308(4) Uani 1 1 d . . . . .
H36A H 0.4622 0.3751 0.0617 0.046 Uiso 1 1 calc R U . . .
H36B H 0.5461 0.3523 -0.0207 0.046 Uiso 1 1 calc R U . . .
H36C H 0.5974 0.3776 0.0918 0.046 Uiso 1 1 calc R U . . .
C37 C 0.35808(16) 0.17372(16) -0.01732(12) 0.0341(4) Uani 1 1 d . . . . .
H37A H 0.2980 0.2048 0.0100 0.051 Uiso 1 1 calc R U . . .
H37B H 0.3311 0.0974 -0.0190 0.051 Uiso 1 1 calc R U . . .
H37C H 0.3676 0.1862 -0.0835 0.051 Uiso 1 1 calc R U . . .
C38 C 0.57181(17) 0.17533(15) 0.00037(12) 0.0335(4) Uani 1 1 d . . . . .
H38A H 0.5812 0.1902 -0.0651 0.050 Uiso 1 1 calc R U . . .
H38B H 0.5428 0.0986 -0.0037 0.050 Uiso 1 1 calc R U . . .
H38C H 0.6499 0.2054 0.0406 0.050 Uiso 1 1 calc R U . . .
C39 C 0.56278(14) 0.04707(13) 0.32331(12) 0.0252(3) Uani 1 1 d . . . . .
C40 C 0.46828(17) -0.06254(14) 0.31138(14) 0.0344(4) Uani 1 1 d . . . . .
H40A H 0.4003 -0.0565 0.3477 0.052 Uiso 1 1 calc R U . . .
H40B H 0.5050 -0.1105 0.3366 0.052 Uiso 1 1 calc R U . . .
H40C H 0.4392 -0.0906 0.2423 0.052 Uiso 1 1 calc R U . . .
C41 C 0.67088(17) 0.03547(17) 0.27004(14) 0.0385(4) Uani 1 1 d . . . . .
H41A H 0.6432 0.0017 0.2017 0.058 Uiso 1 1 calc R U . . .
H41B H 0.7091 -0.0083 0.3007 0.058 Uiso 1 1 calc R U . . .
H41C H 0.7295 0.1055 0.2737 0.058 Uiso 1 1 calc R U . . .
C42 C 0.60842(16) 0.08982(15) 0.43163(12) 0.0315(4) Uani 1 1 d . . . . .
H42A H 0.6668 0.1608 0.4400 0.047 Uiso 1 1 calc R U . . .
H42B H 0.6475 0.0427 0.4556 0.047 Uiso 1 1 calc R U . . .
H42C H 0.5401 0.0933 0.4685 0.047 Uiso 1 1 calc R U . . .
H2 H 0.1973(18) 0.3658(16) 0.3755(14) 0.025(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.7906(12) . ?
Ti1 O1 1.8079(12) . ?
Ti1 O4 1.9121(11) . ?
Ti1 O3 1.9138(11) . ?
Ti1 N2 2.2797(13) . ?
Ti1 N1 2.3876(13) . ?
O1 C1 1.417(2) . ?
N1 C21 1.4906(19) . ?
N1 C22 1.4933(17) . ?
N1 C26 1.4982(18) . ?
C1 C3 1.497(3) . ?
C1 C2 1.509(3) . ?
O2 C4 1.407(2) . ?
N2 C28 1.476(2) . ?
N2 C27 1.4769(19) . ?
O3 C7 1.3316(19) . ?
O4 C30 1.3373(19) . ?
C4 C5 1.512(3) . ?
C4 C6 1.513(3) . ?
C7 C8 1.401(2) . ?
C7 C12 1.423(2) . ?
C8 C9 1.393(2) . ?
C8 C21 1.5093(19) . ?
C9 C10 1.388(2) . ?
C10 C11 1.399(2) . ?
C10 C13 1.534(2) . ?
C11 C12 1.389(2) . ?
C12 C17 1.534(2) . ?
C13 C16 1.525(2) . ?
C13 C14 1.537(2) . ?
C13 C15 1.538(3) . ?
C17 C20 1.532(3) . ?
C17 C18 1.535(2) . ?
C17 C19 1.537(2) . ?
C22 C23 1.530(2) . ?
C23 C24 1.528(2) . ?
C24 C25 1.531(2) . ?
C25 C26 1.530(2) . ?
C26 C27 1.518(2) . ?
C28 C29 1.516(2) . ?
C29 C34 1.389(2) . ?
C29 C30 1.411(2) . ?
C30 C31 1.418(2) . ?
C31 C32 1.393(2) . ?
C31 C35 1.542(2) . ?
C32 C33 1.396(2) . ?
C33 C34 1.390(2) . ?
C33 C39 1.534(2) . ?
C35 C36 1.530(2) . ?
C35 C38 1.538(2) . ?
C35 C37 1.539(2) . ?
C39 C41 1.532(2) . ?
C39 C42 1.535(2) . ?
C39 C40 1.536(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 105.58(6) . . ?
O2 Ti1 O4 94.26(5) . . ?
O1 Ti1 O4 95.80(6) . . ?
O2 Ti1 O3 100.04(5) . . ?
O1 Ti1 O3 91.88(5) . . ?
O4 Ti1 O3 161.33(5) . . ?
O2 Ti1 N2 163.25(5) . . ?
O1 Ti1 N2 90.52(5) . . ?
O4 Ti1 N2 79.25(5) . . ?
O3 Ti1 N2 83.70(5) . . ?
O2 Ti1 N1 90.06(5) . . ?
O1 Ti1 N1 163.11(5) . . ?
O4 Ti1 N1 89.21(5) . . ?
O3 Ti1 N1 78.89(4) . . ?
N2 Ti1 N1 74.54(5) . . ?
C1 O1 Ti1 141.38(12) . . ?
C21 N1 C22 108.89(12) . . ?
C21 N1 C26 111.54(11) . . ?
C22 N1 C26 110.83(11) . . ?
C21 N1 Ti1 106.72(8) . . ?
C22 N1 Ti1 110.26(9) . . ?
C26 N1 Ti1 108.52(9) . . ?
O1 C1 C3 109.41(17) . . ?
O1 C1 C2 108.63(17) . . ?
C3 C1 C2 114.0(2) . . ?
C4 O2 Ti1 164.55(12) . . ?
C28 N2 C27 112.93(12) . . ?
C28 N2 Ti1 112.76(9) . . ?
C27 N2 Ti1 112.28(9) . . ?
C7 O3 Ti1 143.38(10) . . ?
C30 O4 Ti1 139.05(10) . . ?
O2 C4 C5 109.18(16) . . ?
O2 C4 C6 109.34(19) . . ?
C5 C4 C6 112.27(19) . . ?
O3 C7 C8 120.07(13) . . ?
O3 C7 C12 120.38(14) . . ?
C8 C7 C12 119.55(14) . . ?
C9 C8 C7 120.43(14) . . ?
C9 C8 C21 118.99(14) . . ?
C7 C8 C21 120.51(14) . . ?
C10 C9 C8 121.45(15) . . ?
C9 C10 C11 117.19(15) . . ?
C9 C10 C13 122.83(15) . . ?
C11 C10 C13 119.97(14) . . ?
C12 C11 C10 123.84(14) . . ?
C11 C12 C7 117.49(14) . . ?
C11 C12 C17 122.30(14) . . ?
C7 C12 C17 120.20(14) . . ?
C16 C13 C10 112.10(14) . . ?
C16 C13 C14 107.83(15) . . ?
C10 C13 C14 109.95(15) . . ?
C16 C13 C15 107.92(16) . . ?
C10 C13 C15 108.75(15) . . ?
C14 C13 C15 110.28(17) . . ?
C20 C17 C12 110.44(13) . . ?
C20 C17 C18 108.22(16) . . ?
C12 C17 C18 112.02(14) . . ?
C20 C17 C19 109.57(16) . . ?
C12 C17 C19 109.71(14) . . ?
C18 C17 C19 106.78(15) . . ?
N1 C21 C8 115.12(12) . . ?
N1 C22 C23 114.60(12) . . ?
C22 C23 C24 110.35(13) . . ?
C23 C24 C25 110.38(13) . . ?
C26 C25 C24 112.79(13) . . ?
N1 C26 C27 108.11(12) . . ?
N1 C26 C25 113.60(12) . . ?
C27 C26 C25 114.23(12) . . ?
N2 C27 C26 108.67(12) . . ?
N2 C28 C29 114.47(12) . . ?
C34 C29 C30 120.02(14) . . ?
C34 C29 C28 117.55(13) . . ?
C30 C29 C28 122.23(14) . . ?
O4 C30 C29 120.89(13) . . ?
O4 C30 C31 120.01(13) . . ?
C29 C30 C31 119.09(14) . . ?
C32 C31 C30 118.16(14) . . ?
C32 C31 C35 120.84(13) . . ?
C30 C31 C35 120.93(14) . . ?
C31 C32 C33 123.61(14) . . ?
C34 C33 C32 116.89(14) . . ?
C34 C33 C39 120.81(14) . . ?
C32 C33 C39 122.22(14) . . ?
C33 C34 C29 122.19(14) . . ?
C36 C35 C38 107.12(13) . . ?
C36 C35 C37 109.47(14) . . ?
C38 C35 C37 107.79(14) . . ?
C36 C35 C31 111.26(13) . . ?
C38 C35 C31 112.28(13) . . ?
C37 C35 C31 108.84(13) . . ?
C41 C39 C33 112.31(13) . . ?
C41 C39 C42 107.52(14) . . ?
C33 C39 C42 110.79(13) . . ?
C41 C39 C40 108.81(15) . . ?
C33 C39 C40 108.30(13) . . ?
C42 C39 C40 109.04(14) . . ?

_refine_diff_density_max         0.351
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.045

####################################################################### 
# 
# 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_s16mdj52
_database_code_depnum_ccdc_archive 'CCDC 1534478'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H80 N4 O4 Zr'
_chemical_formula_sum            'C48 H80 N4 O4 Zr'
_chemical_formula_weight         868.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7777(2)
_cell_length_b                   14.3460(3)
_cell_length_c                   19.2145(6)
_cell_angle_alpha                76.662(2)
_cell_angle_beta                 81.066(2)
_cell_angle_gamma                71.741(2)
_cell_volume                     2480.42(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    452
_cell_measurement_theta_min      3.6610
_cell_measurement_theta_max      22.5080

_exptl_crystal_description       cube
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.143
_shelx_estimated_absorpt_T_min   0.739
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_T_min  0.27970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.501
_oxdiff_exptl_absorpt_empirical_full_max 2.011
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            31337
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.307
_diffrn_reflns_theta_max         73.592
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9948
_reflns_number_gt                9152
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
two ipr groups are disordered in the ratio 56:44. 
C5/C5A in this disorder was refined with ADP restraintrs.
The N-H hydrogen atoms have been found in the difference Fourier map 
and were refined with bond lenght restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)²+0.8663P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9948
_refine_ls_number_parameters     586
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.002
_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
Zr1 Zr 0.72817(2) 0.51785(2) 0.74005(2) 0.02371(5) Uani 1 1 d . . . . .
O1 O 0.75669(16) 0.53228(12) 0.83344(7) 0.0419(3) Uani 1 1 d . . . . .
O2 O 0.92006(14) 0.45998(11) 0.69815(7) 0.0396(3) Uani 1 1 d . . . . .
O3 O 0.71415(13) 0.66516(9) 0.69548(6) 0.0283(2) Uani 1 1 d . . . . .
O4 O 0.68603(12) 0.38149(8) 0.77071(6) 0.0286(2) Uani 1 1 d . . . . .
N1 N 0.47206(15) 0.56226(10) 0.77153(7) 0.0257(3) Uani 1 1 d . . . . .
N2 N 0.3152(2) 0.68820(14) 0.88049(10) 0.0518(5) Uani 1 1 d D . . . .
H2 H 0.361(3) 0.6153(13) 0.8971(13) 0.053(7) Uiso 1 1 d D . . . .
N3 N 0.62547(14) 0.54452(10) 0.62921(7) 0.0238(3) Uani 1 1 d . . . . .
N4 N 0.7382(3) 0.41074(14) 0.51915(10) 0.0530(5) Uani 1 1 d D . . . .
H4 H 0.780(3) 0.4608(18) 0.5178(16) 0.074(9) Uiso 1 1 d D . . . .
C1 C 0.7843(4) 0.5662(4) 0.89308(18) 0.0337(10) Uani 0.567(7) 1 d . . P A 1
H1 H 0.732671 0.639031 0.890179 0.040 Uiso 0.567(7) 1 calc R U P A 1
C2 C 0.7299(13) 0.5051(10) 0.9612(6) 0.082(4) Uani 0.567(7) 1 d . . P A 1
H2A H 0.626506 0.514241 0.960418 0.123 Uiso 0.567(7) 1 calc R U P A 1
H2B H 0.745125 0.527470 1.003152 0.123 Uiso 0.567(7) 1 calc R U P A 1
H2C H 0.783008 0.434149 0.964046 0.123 Uiso 0.567(7) 1 calc R U P A 1
C3 C 0.9481(18) 0.5479(9) 0.8918(6) 0.046(3) Uani 0.567(7) 1 d . . P A 1
H3A H 0.997597 0.476549 0.893662 0.069 Uiso 0.567(7) 1 calc R U P A 1
H3B H 0.968570 0.568437 0.933327 0.069 Uiso 0.567(7) 1 calc R U P A 1
H3C H 0.982530 0.586884 0.847476 0.069 Uiso 0.567(7) 1 calc R U P A 1
C4 C 1.0506(5) 0.3918(5) 0.6760(2) 0.0454(11) Uani 0.567(7) 1 d . . P A 1
H4A H 1.046760 0.321062 0.690887 0.054 Uiso 0.567(7) 1 calc R U P A 1
C5 C 1.1650(10) 0.4104(11) 0.7141(7) 0.142(5) Uani 0.567(7) 1 d . U P A 1
H5A H 1.166877 0.480014 0.697743 0.213 Uiso 0.567(7) 1 calc R U P A 1
H5B H 1.260390 0.365429 0.702553 0.213 Uiso 0.567(7) 1 calc R U P A 1
H5C H 1.140279 0.397660 0.766152 0.213 Uiso 0.567(7) 1 calc R U P A 1
C1A C 0.8129(6) 0.5022(6) 0.9021(3) 0.0424(15) Uani 0.433(7) 1 d . . P A 2
H1A H 0.857274 0.427990 0.912885 0.051 Uiso 0.433(7) 1 calc R U P A 2
C2A C 0.6907(17) 0.5318(11) 0.9543(8) 0.068(4) Uani 0.433(7) 1 d . . P A 2
H2D H 0.642602 0.603569 0.940679 0.102 Uiso 0.433(7) 1 calc R U P A 2
H2E H 0.725237 0.517655 1.001981 0.102 Uiso 0.433(7) 1 calc R U P A 2
H2F H 0.622048 0.494105 0.955532 0.102 Uiso 0.433(7) 1 calc R U P A 2
C3A C 0.926(3) 0.5540(14) 0.8934(8) 0.061(5) Uani 0.433(7) 1 d . . P A 2
H3D H 0.998301 0.533529 0.854063 0.092 Uiso 0.433(7) 1 calc R U P A 2
H3E H 0.973241 0.536038 0.938001 0.092 Uiso 0.433(7) 1 calc R U P A 2
H3F H 0.881708 0.626507 0.882260 0.092 Uiso 0.433(7) 1 calc R U P A 2
C4A C 1.0684(5) 0.4426(5) 0.6711(3) 0.0360(13) Uani 0.433(7) 1 d . . P A 2
H4B H 1.097953 0.504469 0.667361 0.043 Uiso 0.433(7) 1 calc R U P A 2
C5A C 1.1543(11) 0.3569(7) 0.7283(5) 0.064(2) Uani 0.433(7) 1 d . U P A 2
H5D H 1.134513 0.377802 0.774868 0.097 Uiso 0.433(7) 1 calc R U P A 2
H5E H 1.258092 0.342463 0.713402 0.097 Uiso 0.433(7) 1 calc R U P A 2
H5F H 1.124173 0.296613 0.732627 0.097 Uiso 0.433(7) 1 calc R U P A 2
C6 C 1.0867(4) 0.4176(3) 0.59971(17) 0.0861(10) Uani 1 1 d . . . . .
H6A H 1.177147 0.369498 0.585727 0.129 Uiso 0.567(7) 1 calc R U P A 1
H6B H 1.008910 0.415853 0.573871 0.129 Uiso 0.567(7) 1 calc R U P A 1
H6C H 1.098477 0.485023 0.587714 0.129 Uiso 0.567(7) 1 calc R U P A 1
H6D H 1.188403 0.405599 0.580796 0.129 Uiso 0.433(7) 1 calc R U P A 2
H6E H 1.057200 0.357242 0.603339 0.129 Uiso 0.433(7) 1 calc R U P A 2
H6F H 1.026620 0.473298 0.567323 0.129 Uiso 0.433(7) 1 calc R U P A 2
C7 C 0.71848(17) 0.72516(12) 0.63207(9) 0.0241(3) Uani 1 1 d . . . . .
C8 C 0.66673(17) 0.70740(12) 0.57331(9) 0.0246(3) Uani 1 1 d . . . . .
C9 C 0.66389(18) 0.77401(12) 0.50640(9) 0.0262(3) Uani 1 1 d . . . . .
H9 H 0.625222 0.762246 0.467919 0.031 Uiso 1 1 calc R U . . .
C10 C 0.71591(17) 0.85584(12) 0.49549(9) 0.0273(3) Uani 1 1 d . . . . .
C11 C 0.77126(18) 0.86970(12) 0.55418(9) 0.0284(3) Uani 1 1 d . . . . .
H11 H 0.809781 0.924646 0.547105 0.034 Uiso 1 1 calc R U . . .
C12 C 0.77384(18) 0.80884(12) 0.62196(9) 0.0270(3) Uani 1 1 d . . . . .
C13 C 0.71889(19) 0.92765(13) 0.42267(10) 0.0316(4) Uani 1 1 d . . . . .
C14 C 0.6672(3) 1.03673(15) 0.43215(12) 0.0516(6) Uani 1 1 d . . . . .
H14A H 0.729138 1.046983 0.463455 0.077 Uiso 1 1 calc R U . . .
H14B H 0.567106 1.052082 0.453869 0.077 Uiso 1 1 calc R U . . .
H14C H 0.672151 1.080951 0.385196 0.077 Uiso 1 1 calc R U . . .
C15 C 0.8737(2) 0.90670(17) 0.38776(13) 0.0526(6) Uani 1 1 d . . . . .
H15A H 0.876560 0.952753 0.341499 0.079 Uiso 1 1 calc R U . . .
H15B H 0.908123 0.837595 0.380110 0.079 Uiso 1 1 calc R U . . .
H15C H 0.935977 0.916269 0.419240 0.079 Uiso 1 1 calc R U . . .
C16 C 0.6233(3) 0.9155(2) 0.37211(13) 0.0679(8) Uani 1 1 d . . . . .
H16A H 0.628546 0.962166 0.326329 0.102 Uiso 1 1 calc R U . . .
H16B H 0.523120 0.929759 0.393660 0.102 Uiso 1 1 calc R U . . .
H16C H 0.656612 0.846748 0.363744 0.102 Uiso 1 1 calc R U . . .
C17 C 0.8355(2) 0.82882(14) 0.68396(10) 0.0330(4) Uani 1 1 d . . . . .
C18 C 0.8885(3) 0.92257(17) 0.66171(12) 0.0477(5) Uani 1 1 d . . . . .
H18A H 0.963269 0.914423 0.621392 0.072 Uiso 1 1 calc R U . . .
H18B H 0.928901 0.931772 0.702392 0.072 Uiso 1 1 calc R U . . .
H18C H 0.807203 0.981275 0.647170 0.072 Uiso 1 1 calc R U . . .
C19 C 0.7198(3) 0.84498(17) 0.74750(11) 0.0448(5) Uani 1 1 d . . . . .
H19A H 0.636533 0.901340 0.731668 0.067 Uiso 1 1 calc R U . . .
H19B H 0.760277 0.859551 0.785973 0.067 Uiso 1 1 calc R U . . .
H19C H 0.688904 0.784365 0.765391 0.067 Uiso 1 1 calc R U . . .
C20 C 0.9659(2) 0.74009(16) 0.70806(12) 0.0430(5) Uani 1 1 d . . . . .
H20A H 0.936069 0.678717 0.722638 0.064 Uiso 1 1 calc R U . . .
H20B H 1.003068 0.751952 0.748743 0.064 Uiso 1 1 calc R U . . .
H20C H 1.041839 0.732925 0.668201 0.064 Uiso 1 1 calc R U . . .
C21 C 0.61439(18) 0.62185(12) 0.57800(9) 0.0250(3) Uani 1 1 d . . . . .
H21 H 0.565975 0.622896 0.538489 0.030 Uiso 1 1 calc R U . . .
C22 C 0.56345(18) 0.46822(12) 0.61792(9) 0.0276(3) Uani 1 1 d . . . . .
H22A H 0.492317 0.499395 0.581696 0.033 Uiso 1 1 calc R U . . .
H22B H 0.511523 0.443524 0.663445 0.033 Uiso 1 1 calc R U . . .
C23 C 0.67859(19) 0.37998(12) 0.59274(9) 0.0278(3) Uani 1 1 d . . . . .
H23 H 0.757868 0.353780 0.625570 0.033 Uiso 1 1 calc R U . . .
C24 C 0.6109(2) 0.29928(14) 0.59350(13) 0.0422(5) Uani 1 1 d . . . . .
H24A H 0.527455 0.327441 0.564076 0.051 Uiso 1 1 calc R U . . .
H24B H 0.574108 0.275873 0.643354 0.051 Uiso 1 1 calc R U . . .
C25 C 0.7152(2) 0.21136(15) 0.56499(12) 0.0432(5) Uani 1 1 d . . . . .
H25A H 0.663357 0.163108 0.562638 0.052 Uiso 1 1 calc R U . . .
H25B H 0.791737 0.177039 0.598139 0.052 Uiso 1 1 calc R U . . .
C26 C 0.7836(3) 0.24462(16) 0.49115(12) 0.0497(5) Uani 1 1 d . . . . .
H26A H 0.709095 0.270530 0.456454 0.060 Uiso 1 1 calc R U . . .
H26B H 0.858294 0.186768 0.475464 0.060 Uiso 1 1 calc R U . . .
C27 C 0.8524(3) 0.32613(16) 0.49213(12) 0.0527(6) Uani 1 1 d . . . . .
H27A H 0.932082 0.299186 0.523938 0.063 Uiso 1 1 calc R U . . .
H27B H 0.892684 0.350128 0.443145 0.063 Uiso 1 1 calc R U . . .
C28 C 0.59608(17) 0.33871(12) 0.81561(9) 0.0241(3) Uani 1 1 d . . . . .
C29 C 0.64106(18) 0.23490(12) 0.84725(9) 0.0262(3) Uani 1 1 d . . . . .
C30 C 0.53959(18) 0.19464(12) 0.89222(9) 0.0281(3) Uani 1 1 d . . . . .
H30 H 0.569527 0.125673 0.913696 0.034 Uiso 1 1 calc R U . . .
C31 C 0.39548(18) 0.24914(13) 0.90809(9) 0.0283(3) Uani 1 1 d . . . . .
C32 C 0.35505(18) 0.34908(13) 0.87718(9) 0.0280(3) Uani 1 1 d . . . . .
H32 H 0.258344 0.388166 0.886576 0.034 Uiso 1 1 calc R U . . .
C33 C 0.45318(18) 0.39512(12) 0.83195(9) 0.0260(3) Uani 1 1 d . . . . .
C34 C 0.7968(2) 0.17067(13) 0.83281(10) 0.0331(4) Uani 1 1 d . . . . .
C35 C 0.8321(3) 0.16938(16) 0.75253(12) 0.0523(6) Uani 1 1 d . . . . .
H35A H 0.929215 0.124277 0.744408 0.078 Uiso 1 1 calc R U . . .
H35B H 0.828389 0.237097 0.725966 0.078 Uiso 1 1 calc R U . . .
H35C H 0.761266 0.145955 0.735822 0.078 Uiso 1 1 calc R U . . .
C36 C 0.9013(2) 0.21254(17) 0.85912(13) 0.0485(5) Uani 1 1 d . . . . .
H36A H 0.878497 0.212004 0.910682 0.073 Uiso 1 1 calc R U . . .
H36B H 0.891500 0.281337 0.833160 0.073 Uiso 1 1 calc R U . . .
H36C H 1.000721 0.171092 0.850340 0.073 Uiso 1 1 calc R U . . .
C37 C 0.8209(2) 0.06113(15) 0.87179(13) 0.0481(5) Uani 1 1 d . . . . .
H37A H 0.803332 0.058186 0.923762 0.072 Uiso 1 1 calc R U . . .
H37B H 0.920745 0.022491 0.860098 0.072 Uiso 1 1 calc R U . . .
H37C H 0.754113 0.032905 0.856343 0.072 Uiso 1 1 calc R U . . .
C38 C 0.2930(2) 0.19543(14) 0.95765(11) 0.0344(4) Uani 1 1 d . . . . .
C39 C 0.3484(3) 0.15551(18) 1.03229(12) 0.0491(5) Uani 1 1 d . . . . .
H39A H 0.350993 0.211479 1.052687 0.074 Uiso 1 1 calc R U . . .
H39B H 0.445901 0.109209 1.028347 0.074 Uiso 1 1 calc R U . . .
H39C H 0.283563 0.120290 1.063591 0.074 Uiso 1 1 calc R U . . .
C40 C 0.2868(2) 0.10815(15) 0.92577(14) 0.0463(5) Uani 1 1 d . . . . .
H40A H 0.217219 0.075938 0.955706 0.069 Uiso 1 1 calc R U . . .
H40B H 0.382723 0.059287 0.924291 0.069 Uiso 1 1 calc R U . . .
H40C H 0.256562 0.133534 0.876971 0.069 Uiso 1 1 calc R U . . .
C41 C 0.1397(2) 0.26539(15) 0.96555(13) 0.0437(5) Uani 1 1 d . . . . .
H41A H 0.077123 0.228405 0.996950 0.065 Uiso 1 1 calc R U . . .
H41B H 0.102401 0.291481 0.918214 0.065 Uiso 1 1 calc R U . . .
H41C H 0.141095 0.321141 0.986547 0.065 Uiso 1 1 calc R U . . .
C42 C 0.39920(18) 0.50157(12) 0.80407(9) 0.0272(3) Uani 1 1 d . . . . .
H42 H 0.297461 0.530012 0.810645 0.033 Uiso 1 1 calc R U . . .
C43 C 0.38681(19) 0.66800(12) 0.75350(10) 0.0304(4) Uani 1 1 d . . . . .
H43A H 0.285692 0.671813 0.748813 0.037 Uiso 1 1 calc R U . . .
H43B H 0.426834 0.699482 0.706688 0.037 Uiso 1 1 calc R U . . .
C44 C 0.3888(2) 0.72562(13) 0.81112(10) 0.0328(4) Uani 1 1 d . . . . .
H44 H 0.491288 0.717960 0.818011 0.039 Uiso 1 1 calc R U . . .
C45 C 0.3132(3) 0.83386(14) 0.78637(12) 0.0433(5) Uani 1 1 d . . . . .
H45A H 0.213723 0.840887 0.776374 0.052 Uiso 1 1 calc R U . . .
H45B H 0.364573 0.859508 0.740984 0.052 Uiso 1 1 calc R U . . .
C46 C 0.3060(4) 0.89579(17) 0.84070(15) 0.0649(7) Uani 1 1 d . . . . .
H46A H 0.249902 0.965890 0.823302 0.078 Uiso 1 1 calc R U . . .
H46B H 0.404899 0.895214 0.846908 0.078 Uiso 1 1 calc R U . . .
C47 C 0.2356(4) 0.8554(2) 0.91173(17) 0.0764(9) Uani 1 1 d . . . . .
H47A H 0.238747 0.893571 0.947979 0.092 Uiso 1 1 calc R U . . .
H47B H 0.132927 0.863566 0.906872 0.092 Uiso 1 1 calc R U . . .
C48 C 0.3122(4) 0.74639(19) 0.93635(13) 0.0663(8) Uani 1 1 d . . . . .
H48A H 0.412339 0.738783 0.945556 0.080 Uiso 1 1 calc R U . . .
H48B H 0.261775 0.719896 0.981785 0.080 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
Zr1 O1 1.9245(13) . ?
Zr1 O2 1.9289(13) . ?
Zr1 O3 2.0587(11) . ?
Zr1 O4 2.0596(12) . ?
Zr1 N3 2.3954(13) . ?
Zr1 N1 2.3979(14) . ?
O1 C1A 1.429(5) . ?
O1 C1 1.435(3) . ?
O2 C4 1.417(4) . ?
O2 C4A 1.426(5) . ?
O3 C7 1.3229(19) . ?
O4 C28 1.3238(19) . ?
N1 C42 1.287(2) . ?
N1 C43 1.473(2) . ?
N2 C44 1.482(3) . ?
N2 C48 1.496(3) . ?
N2 H2 0.996(16) . ?
N3 C21 1.290(2) . ?
N3 C22 1.4762(19) . ?
N4 C23 1.467(2) . ?
N4 C27 1.500(3) . ?
N4 H4 0.923(17) . ?
C1 C2 1.521(12) . ?
C1 C3 1.536(17) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C6 1.443(5) . ?
C4 C5 1.546(12) . ?
C4 H4A 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C1A C2A 1.458(16) . ?
C1A C3A 1.49(2) . ?
C1A H1A 1.0000 . ?
C2A H2D 0.9800 . ?
C2A H2E 0.9800 . ?
C2A H2F 0.9800 . ?
C3A H3D 0.9800 . ?
C3A H3E 0.9800 . ?
C3A H3F 0.9800 . ?
C4A C6 1.468(6) . ?
C4A C5A 1.563(10) . ?
C4A H4B 1.0000 . ?
C5A H5D 0.9800 . ?
C5A H5E 0.9800 . ?
C5A H5F 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 H6D 0.9800 . ?
C6 H6E 0.9800 . ?
C6 H6F 0.9800 . ?
C7 C8 1.410(2) . ?
C7 C12 1.428(2) . ?
C8 C9 1.412(2) . ?
C8 C21 1.451(2) . ?
C9 C10 1.381(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(2) . ?
C10 C13 1.537(2) . ?
C11 C12 1.390(2) . ?
C11 H11 0.9500 . ?
C12 C17 1.534(2) . ?
C13 C16 1.520(3) . ?
C13 C15 1.525(3) . ?
C13 C14 1.531(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C20 1.535(3) . ?
C17 C19 1.537(3) . ?
C17 C18 1.537(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
C22 C23 1.525(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.499(2) . ?
C23 H23 1.0000 . ?
C24 C25 1.507(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.510(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.526(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C33 1.406(2) . ?
C28 C29 1.427(2) . ?
C29 C30 1.388(2) . ?
C29 C34 1.534(2) . ?
C30 C31 1.406(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(2) . ?
C31 C38 1.534(2) . ?
C32 C33 1.409(2) . ?
C32 H32 0.9500 . ?
C33 C42 1.450(2) . ?
C34 C35 1.531(3) . ?
C34 C36 1.531(3) . ?
C34 C37 1.538(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C41 1.528(3) . ?
C38 C39 1.531(3) . ?
C38 C40 1.536(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42 0.9500 . ?
C43 C44 1.532(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.494(2) . ?
C44 H44 1.0000 . ?
C45 C46 1.500(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.505(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.505(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?

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 Zr1 O2 104.64(6) . . ?
O1 Zr1 O3 92.94(6) . . ?
O2 Zr1 O3 97.31(5) . . ?
O1 Zr1 O4 97.70(6) . . ?
O2 Zr1 O4 92.78(5) . . ?
O3 Zr1 O4 163.02(5) . . ?
O1 Zr1 N3 161.42(6) . . ?
O2 Zr1 N3 91.98(5) . . ?
O3 Zr1 N3 76.47(4) . . ?
O4 Zr1 N3 89.60(5) . . ?
O1 Zr1 N1 89.59(5) . . ?
O2 Zr1 N1 163.43(5) . . ?
O3 Zr1 N1 90.29(5) . . ?
O4 Zr1 N1 76.65(5) . . ?
N3 Zr1 N1 75.45(5) . . ?
C1A O1 Zr1 156.5(3) . . ?
C1 O1 Zr1 165.5(2) . . ?
C4 O2 Zr1 163.6(3) . . ?
C4A O2 Zr1 163.3(3) . . ?
C7 O3 Zr1 140.58(10) . . ?
C28 O4 Zr1 139.75(11) . . ?
C42 N1 C43 115.26(14) . . ?
C42 N1 Zr1 125.89(11) . . ?
C43 N1 Zr1 118.85(10) . . ?
C44 N2 C48 111.65(18) . . ?
C44 N2 H2 110.7(15) . . ?
C48 N2 H2 111.2(15) . . ?
C21 N3 C22 115.49(14) . . ?
C21 N3 Zr1 126.17(11) . . ?
C22 N3 Zr1 118.30(10) . . ?
C23 N4 C27 112.24(16) . . ?
C23 N4 H4 109.4(19) . . ?
C27 N4 H4 107.9(19) . . ?
O1 C1 C2 107.3(6) . . ?
O1 C1 C3 108.8(6) . . ?
C2 C1 C3 109.9(7) . . ?
O1 C1 H1 110.3 . . ?
C2 C1 H1 110.3 . . ?
C3 C1 H1 110.3 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 C6 111.0(4) . . ?
O2 C4 C5 103.2(6) . . ?
C6 C4 C5 107.3(7) . . ?
O2 C4 H4A 111.7 . . ?
C6 C4 H4A 111.7 . . ?
C5 C4 H4A 111.7 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C1A C2A 106.4(7) . . ?
O1 C1A C3A 103.6(7) . . ?
C2A C1A C3A 115.9(11) . . ?
O1 C1A H1A 110.2 . . ?
C2A C1A H1A 110.2 . . ?
C3A C1A H1A 110.2 . . ?
C1A C2A H2D 109.5 . . ?
C1A C2A H2E 109.5 . . ?
H2D C2A H2E 109.5 . . ?
C1A C2A H2F 109.5 . . ?
H2D C2A H2F 109.5 . . ?
H2E C2A H2F 109.5 . . ?
C1A C3A H3D 109.5 . . ?
C1A C3A H3E 109.5 . . ?
H3D C3A H3E 109.5 . . ?
C1A C3A H3F 109.5 . . ?
H3D C3A H3F 109.5 . . ?
H3E C3A H3F 109.5 . . ?
O2 C4A C6 109.0(4) . . ?
O2 C4A C5A 105.4(5) . . ?
C6 C4A C5A 113.9(6) . . ?
O2 C4A H4B 109.5 . . ?
C6 C4A H4B 109.5 . . ?
C5A C4A H4B 109.5 . . ?
C4A C5A H5D 109.5 . . ?
C4A C5A H5E 109.5 . . ?
H5D C5A H5E 109.5 . . ?
C4A C5A H5F 109.5 . . ?
H5D C5A H5F 109.5 . . ?
H5E C5A H5F 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4A C6 H6D 109.5 . . ?
C4A C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
C4A C6 H6F 109.5 . . ?
H6D C6 H6F 109.5 . . ?
H6E C6 H6F 109.5 . . ?
O3 C7 C8 119.94(14) . . ?
O3 C7 C12 121.08(15) . . ?
C8 C7 C12 118.97(15) . . ?
C7 C8 C9 120.34(15) . . ?
C7 C8 C21 122.63(15) . . ?
C9 C8 C21 117.03(15) . . ?
C10 C9 C8 121.67(16) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 116.71(15) . . ?
C9 C10 C13 122.87(16) . . ?
C11 C10 C13 120.39(15) . . ?
C12 C11 C10 124.70(15) . . ?
C12 C11 H11 117.6 . . ?
C10 C11 H11 117.6 . . ?
C11 C12 C7 117.54(15) . . ?
C11 C12 C17 121.91(15) . . ?
C7 C12 C17 120.55(15) . . ?
C16 C13 C15 108.7(2) . . ?
C16 C13 C14 107.91(19) . . ?
C15 C13 C14 108.16(17) . . ?
C16 C13 C10 111.96(15) . . ?
C15 C13 C10 109.05(15) . . ?
C14 C13 C10 110.98(15) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 C20 109.59(15) . . ?
C12 C17 C19 110.64(15) . . ?
C20 C17 C19 109.87(17) . . ?
C12 C17 C18 112.08(16) . . ?
C20 C17 C18 107.17(16) . . ?
C19 C17 C18 107.39(16) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 C8 128.01(15) . . ?
N3 C21 H21 116.0 . . ?
C8 C21 H21 116.0 . . ?
N3 C22 C23 112.33(13) . . ?
N3 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
N3 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
N4 C23 C24 108.41(16) . . ?
N4 C23 C22 110.39(15) . . ?
C24 C23 C22 109.02(15) . . ?
N4 C23 H23 109.7 . . ?
C24 C23 H23 109.7 . . ?
C22 C23 H23 109.7 . . ?
C23 C24 C25 112.64(17) . . ?
C23 C24 H24A 109.1 . . ?
C25 C24 H24A 109.1 . . ?
C23 C24 H24B 109.1 . . ?
C25 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C24 C25 C26 111.03(19) . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C27 110.30(17) . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
N4 C27 C26 108.4(2) . . ?
N4 C27 H27A 110.0 . . ?
C26 C27 H27A 110.0 . . ?
N4 C27 H27B 110.0 . . ?
C26 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
O4 C28 C33 120.15(14) . . ?
O4 C28 C29 120.93(15) . . ?
C33 C28 C29 118.91(15) . . ?
C30 C29 C28 117.67(15) . . ?
C30 C29 C34 121.33(15) . . ?
C28 C29 C34 120.99(15) . . ?
C29 C30 C31 124.34(15) . . ?
C29 C30 H30 117.8 . . ?
C31 C30 H30 117.8 . . ?
C32 C31 C30 116.83(16) . . ?
C32 C31 C38 123.85(16) . . ?
C30 C31 C38 119.31(15) . . ?
C31 C32 C33 121.78(16) . . ?
C31 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C28 C33 C32 120.43(15) . . ?
C28 C33 C42 122.77(15) . . ?
C32 C33 C42 116.80(15) . . ?
C35 C34 C36 110.30(18) . . ?
C35 C34 C29 110.21(16) . . ?
C36 C34 C29 109.48(15) . . ?
C35 C34 C37 106.70(17) . . ?
C36 C34 C37 107.94(17) . . ?
C29 C34 C37 112.16(15) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C41 C38 C39 108.39(18) . . ?
C41 C38 C31 111.74(15) . . ?
C39 C38 C31 109.67(15) . . ?
C41 C38 C40 108.21(16) . . ?
C39 C38 C40 109.72(17) . . ?
C31 C38 C40 109.08(16) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N1 C42 C33 128.03(16) . . ?
N1 C42 H42 116.0 . . ?
C33 C42 H42 116.0 . . ?
N1 C43 C44 111.42(14) . . ?
N1 C43 H43A 109.3 . . ?
C44 C43 H43A 109.3 . . ?
N1 C43 H43B 109.3 . . ?
C44 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
N2 C44 C45 109.11(16) . . ?
N2 C44 C43 111.33(15) . . ?
C45 C44 C43 108.80(16) . . ?
N2 C44 H44 109.2 . . ?
C45 C44 H44 109.2 . . ?
C43 C44 H44 109.2 . . ?
C44 C45 C46 112.47(19) . . ?
C44 C45 H45A 109.1 . . ?
C46 C45 H45A 109.1 . . ?
C44 C45 H45B 109.1 . . ?
C46 C45 H45B 109.1 . . ?
H45A C45 H45B 107.8 . . ?
C45 C46 C47 110.5(2) . . ?
C45 C46 H46A 109.5 . . ?
C47 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C47 C46 H46B 109.5 . . ?
H46A C46 H46B 108.1 . . ?
C48 C47 C46 110.4(2) . . ?
C48 C47 H47A 109.6 . . ?
C46 C47 H47A 109.6 . . ?
C48 C47 H47B 109.6 . . ?
C46 C47 H47B 109.6 . . ?
H47A C47 H47B 108.1 . . ?
N2 C48 C47 110.3(2) . . ?
N2 C48 H48A 109.6 . . ?
C47 C48 H48A 109.6 . . ?
N2 C48 H48B 109.6 . . ?
C47 C48 H48B 109.6 . . ?
H48A C48 H48B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O1 C1 C2 164.1(7) . . . . ?
Zr1 O1 C1 C3 -77.0(9) . . . . ?
Zr1 O2 C4 C6 127.3(6) . . . . ?
Zr1 O2 C4 C5 -118.1(10) . . . . ?
Zr1 O1 C1A C2A -132.5(8) . . . . ?
Zr1 O1 C1A C3A 104.8(11) . . . . ?
Zr1 O2 C4A C6 -130.9(7) . . . . ?
Zr1 O2 C4A C5A 106.4(10) . . . . ?
Zr1 O3 C7 C8 32.0(3) . . . . ?
Zr1 O3 C7 C12 -148.56(14) . . . . ?
O3 C7 C8 C9 176.67(15) . . . . ?
C12 C7 C8 C9 -2.8(2) . . . . ?
O3 C7 C8 C21 -3.2(2) . . . . ?
C12 C7 C8 C21 177.32(15) . . . . ?
C7 C8 C9 C10 2.4(3) . . . . ?
C21 C8 C9 C10 -177.71(15) . . . . ?
C8 C9 C10 C11 -0.2(2) . . . . ?
C8 C9 C10 C13 177.92(15) . . . . ?
C9 C10 C11 C12 -1.6(3) . . . . ?
C13 C10 C11 C12 -179.81(16) . . . . ?
C10 C11 C12 C7 1.2(3) . . . . ?
C10 C11 C12 C17 -179.66(16) . . . . ?
O3 C7 C12 C11 -178.39(15) . . . . ?
C8 C7 C12 C11 1.1(2) . . . . ?
O3 C7 C12 C17 2.5(2) . . . . ?
C8 C7 C12 C17 -178.09(15) . . . . ?
C9 C10 C13 C16 15.6(3) . . . . ?
C11 C10 C13 C16 -166.3(2) . . . . ?
C9 C10 C13 C15 -104.7(2) . . . . ?
C11 C10 C13 C15 73.4(2) . . . . ?
C9 C10 C13 C14 136.26(19) . . . . ?
C11 C10 C13 C14 -45.7(2) . . . . ?
C11 C12 C17 C20 -117.74(19) . . . . ?
C7 C12 C17 C20 61.4(2) . . . . ?
C11 C12 C17 C19 120.95(19) . . . . ?
C7 C12 C17 C19 -59.9(2) . . . . ?
C11 C12 C17 C18 1.1(3) . . . . ?
C7 C12 C17 C18 -179.78(17) . . . . ?
C22 N3 C21 C8 -178.87(16) . . . . ?
Zr1 N3 C21 C8 3.4(2) . . . . ?
C7 C8 C21 N3 -11.0(3) . . . . ?
C9 C8 C21 N3 169.14(16) . . . . ?
C21 N3 C22 C23 100.33(17) . . . . ?
Zr1 N3 C22 C23 -81.75(15) . . . . ?
C27 N4 C23 C24 -60.8(2) . . . . ?
C27 N4 C23 C22 179.90(18) . . . . ?
N3 C22 C23 N4 -69.68(19) . . . . ?
N3 C22 C23 C24 171.34(15) . . . . ?
N4 C23 C24 C25 56.3(2) . . . . ?
C22 C23 C24 C25 176.50(17) . . . . ?
C23 C24 C25 C26 -54.2(2) . . . . ?
C24 C25 C26 C27 53.9(2) . . . . ?
C23 N4 C27 C26 61.8(2) . . . . ?
C25 C26 C27 N4 -56.8(2) . . . . ?
Zr1 O4 C28 C33 32.8(2) . . . . ?
Zr1 O4 C28 C29 -148.24(13) . . . . ?
O4 C28 C29 C30 -178.22(15) . . . . ?
C33 C28 C29 C30 0.8(2) . . . . ?
O4 C28 C29 C34 2.7(2) . . . . ?
C33 C28 C29 C34 -178.33(15) . . . . ?
C28 C29 C30 C31 0.6(3) . . . . ?
C34 C29 C30 C31 179.67(16) . . . . ?
C29 C30 C31 C32 -0.8(3) . . . . ?
C29 C30 C31 C38 178.91(17) . . . . ?
C30 C31 C32 C33 -0.3(3) . . . . ?
C38 C31 C32 C33 -179.99(16) . . . . ?
O4 C28 C33 C32 177.18(15) . . . . ?
C29 C28 C33 C32 -1.8(2) . . . . ?
O4 C28 C33 C42 -2.9(2) . . . . ?
C29 C28 C33 C42 178.09(15) . . . . ?
C31 C32 C33 C28 1.6(3) . . . . ?
C31 C32 C33 C42 -178.34(16) . . . . ?
C30 C29 C34 C35 120.08(19) . . . . ?
C28 C29 C34 C35 -60.8(2) . . . . ?
C30 C29 C34 C36 -118.43(19) . . . . ?
C28 C29 C34 C36 60.6(2) . . . . ?
C30 C29 C34 C37 1.4(3) . . . . ?
C28 C29 C34 C37 -179.56(17) . . . . ?
C32 C31 C38 C41 2.6(3) . . . . ?
C30 C31 C38 C41 -177.13(17) . . . . ?
C32 C31 C38 C39 -117.6(2) . . . . ?
C30 C31 C38 C39 62.7(2) . . . . ?
C32 C31 C38 C40 122.20(19) . . . . ?
C30 C31 C38 C40 -57.5(2) . . . . ?
C43 N1 C42 C33 -176.33(16) . . . . ?
Zr1 N1 C42 C33 3.1(3) . . . . ?
C28 C33 C42 N1 -11.6(3) . . . . ?
C32 C33 C42 N1 168.33(17) . . . . ?
C42 N1 C43 C44 95.09(18) . . . . ?
Zr1 N1 C43 C44 -84.36(15) . . . . ?
C48 N2 C44 C45 -58.0(3) . . . . ?
C48 N2 C44 C43 -178.1(2) . . . . ?
N1 C43 C44 N2 -65.2(2) . . . . ?
N1 C43 C44 C45 174.47(16) . . . . ?
N2 C44 C45 C46 56.6(3) . . . . ?
C43 C44 C45 C46 178.3(2) . . . . ?
C44 C45 C46 C47 -55.7(3) . . . . ?
C45 C46 C47 C48 54.7(4) . . . . ?
C44 N2 C48 C47 58.8(3) . . . . ?
C46 C47 C48 N2 -56.3(4) . . . . ?

_refine_diff_density_max         0.423
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_S16MDJ13
_database_code_depnum_ccdc_archive 'CCDC 1534474'
_audit_update_record             
;
2017-02-23 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H33 N2 O Zn0.50'
_chemical_formula_weight         362.18

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'

_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'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'-y, -x+1/2, z+1/4'
'y, x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'-y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+3/4'

_cell_length_a                   24.0450(2)
_cell_length_b                   24.0450(2)
_cell_length_c                   14.5399(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8406.42(18)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13457
_cell_measurement_theta_min      3.5430
_cell_measurement_theta_max      71.5810

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             3136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.086
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_T_min  0.8698
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            28432
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.552
_diffrn_reflns_theta_max         72.413
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4148
_reflns_number_gt                3940
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.825
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2014/8 (Sheldrick, 2014)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0390P)²+2.5096P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1711 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4148
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.00946(2) 0.2500 0.1250 0.02898(11) Uani 1 2 d S T P A .
O1 O -0.04475(8) 0.27713(7) 0.02942(12) 0.0391(4) Uani 1 1 d . . . . .
N1 N 0.0696(3) 0.2421(3) 0.2434(6) 0.0302(13) Uani 0.6 1 d . . P A 1
H1 H 0.0450 0.2336 0.2970 0.036 Uiso 0.6 1 calc R U P A 1
C1 C -0.06200(9) 0.32611(9) 0.00651(15) 0.0303(4) Uani 1 1 d . . . . .
N2 N 0.01595(9) 0.33391(8) 0.16812(14) 0.0361(4) Uani 1 1 d . . . . .
C2 C -0.10168(9) 0.33179(10) -0.06681(16) 0.0326(5) Uani 1 1 d . . . . .
C3 C -0.11685(10) 0.38451(10) -0.09422(16) 0.0362(5) Uani 1 1 d . . . . .
H3 H -0.1423 0.3877 -0.1439 0.043 Uiso 1 1 calc R U . . .
C4 C -0.09731(10) 0.43391(11) -0.05390(18) 0.0383(5) Uani 1 1 d . . . . .
C5 C -0.06151(10) 0.42829(10) 0.01873(18) 0.0379(5) Uani 1 1 d . . . . .
H5 H -0.0485 0.4608 0.0489 0.046 Uiso 1 1 calc R U . . .
C6 C -0.04325(9) 0.37568(10) 0.05037(17) 0.0326(5) Uani 1 1 d . . . . .
C7 C -0.12574(11) 0.27959(10) -0.11212(19) 0.0413(6) Uani 1 1 d . . . . .
C8 C -0.15445(13) 0.24331(14) -0.0407(2) 0.0588(8) Uani 1 1 d . . . . .
H8A H -0.1853 0.2640 -0.0129 0.088 Uiso 1 1 calc R U . . .
H8B H -0.1277 0.2329 0.0072 0.088 Uiso 1 1 calc R U . . .
H8C H -0.1689 0.2097 -0.0703 0.088 Uiso 1 1 calc R U . . .
C9 C -0.07981(13) 0.24623(15) -0.1600(2) 0.0560(7) Uani 1 1 d . . . . .
H9A H -0.0958 0.2124 -0.1869 0.084 Uiso 1 1 calc R U . . .
H9B H -0.0512 0.2361 -0.1151 0.084 Uiso 1 1 calc R U . . .
H9C H -0.0631 0.2689 -0.2088 0.084 Uiso 1 1 calc R U . . .
C10 C -0.16913(16) 0.29406(15) -0.1854(3) 0.0698(10) Uani 1 1 d . . . . .
H10A H -0.1840 0.2597 -0.2122 0.105 Uiso 1 1 calc R U . . .
H10B H -0.1517 0.3165 -0.2338 0.105 Uiso 1 1 calc R U . . .
H10C H -0.1995 0.3152 -0.1571 0.105 Uiso 1 1 calc R U . . .
C11 C -0.11717(12) 0.49030(11) -0.0918(2) 0.0483(7) Uani 1 1 d . . . . .
C12 C -0.09369(18) 0.53863(13) -0.0377(4) 0.0995(18) Uani 1 1 d . . . . .
H12A H -0.0531 0.5393 -0.0442 0.149 Uiso 1 1 calc R U . . .
H12B H -0.1034 0.5344 0.0274 0.149 Uiso 1 1 calc R U . . .
H12C H -0.1093 0.5735 -0.0612 0.149 Uiso 1 1 calc R U . . .
C13 C -0.18059(12) 0.49347(13) -0.0863(2) 0.0535(7) Uani 1 1 d . . . . .
H13A H -0.1925 0.4884 -0.0224 0.080 Uiso 1 1 calc R U . . .
H13B H -0.1969 0.4642 -0.1246 0.080 Uiso 1 1 calc R U . . .
H13C H -0.1931 0.5299 -0.1085 0.080 Uiso 1 1 calc R U . . .
C14 C -0.10051(18) 0.49543(17) -0.1927(3) 0.0886(15) Uani 1 1 d . . . . .
H14A H -0.1144 0.5307 -0.2174 0.133 Uiso 1 1 calc R U . . .
H14B H -0.1165 0.4645 -0.2276 0.133 Uiso 1 1 calc R U . . .
H14C H -0.0599 0.4944 -0.1979 0.133 Uiso 1 1 calc R U . . .
C15 C -0.00692(9) 0.37589(9) 0.12877(18) 0.0358(4) Uani 1 1 d . . . . .
H15 H 0.0012 0.4113 0.1546 0.043 Uiso 1 1 calc R U . . .
C16 C 0.0438(4) 0.3401(4) 0.2556(7) 0.0390(17) Uani 0.6 1 d . . P A 1
H16A H 0.0168 0.3342 0.3060 0.047 Uiso 0.6 1 calc R U P A 1
H16B H 0.0586 0.3784 0.2610 0.047 Uiso 0.6 1 calc R U P A 1
C17 C 0.0914(2) 0.29826(19) 0.2647(4) 0.0304(9) Uani 0.6 1 d . . P A 1
H17 H 0.1194 0.3076 0.2161 0.036 Uiso 0.6 1 calc R U P A 1
C18 C 0.1221(5) 0.3002(6) 0.3585(11) 0.036(3) Uani 0.6 1 d . . P A 1
H18A H 0.1408 0.3367 0.3656 0.043 Uiso 0.6 1 calc R U P A 1
H18B H 0.0948 0.2962 0.4090 0.043 Uiso 0.6 1 calc R U P A 1
C19 C 0.16413(17) 0.25495(18) 0.3649(3) 0.0433(9) Uani 0.6 1 d . . P A 1
H19C H 0.1793 0.2542 0.4283 0.052 Uiso 0.6 1 calc R U P A 1
H19D H 0.1952 0.2636 0.3227 0.052 Uiso 0.6 1 calc R U P A 1
C20 C 0.1411(6) 0.1966(6) 0.3412(11) 0.043(2) Uani 0.6 1 d . . P A 1
H20A H 0.1719 0.1693 0.3383 0.052 Uiso 0.6 1 calc R U P A 1
H20B H 0.1147 0.1843 0.3894 0.052 Uiso 0.6 1 calc R U P A 1
C21 C 0.1114(4) 0.1995(4) 0.2479(6) 0.0451(18) Uani 0.6 1 d . . P A 1
H21A H 0.1394 0.2064 0.1992 0.054 Uiso 0.6 1 calc R U P A 1
H21B H 0.0938 0.1631 0.2351 0.054 Uiso 0.6 1 calc R U P A 1
C16A C 0.0606(5) 0.3482(6) 0.2382(10) 0.035(3) Uani 0.4 1 d . . P A 2
H16C H 0.0955 0.3594 0.2071 0.042 Uiso 0.4 1 calc R U P A 2
H16D H 0.0482 0.3791 0.2784 0.042 Uiso 0.4 1 calc R U P A 2
C17A C 0.0689(3) 0.2963(3) 0.2926(5) 0.0311(15) Uani 0.4 1 d . . P A 2
H17A H 0.0322 0.2864 0.3206 0.037 Uiso 0.4 1 calc R U P A 2
C18A C 0.1087(8) 0.3036(10) 0.3683(16) 0.033(3) Uani 0.4 1 d . . P A 2
H18C H 0.0939 0.3315 0.4119 0.040 Uiso 0.4 1 calc R U P A 2
H18D H 0.1441 0.3180 0.3433 0.040 Uiso 0.4 1 calc R U P A 2
C19A C 0.1200(3) 0.2491(3) 0.4203(5) 0.0538(17) Uani 0.4 1 d . . P A 2
H19A H 0.1504 0.2548 0.4653 0.065 Uiso 0.4 1 calc R U P A 2
H19B H 0.0862 0.2376 0.4543 0.065 Uiso 0.4 1 calc R U P A 2
C20A C 0.1358(10) 0.2053(10) 0.3546(17) 0.059(7) Uani 0.4 1 d . . P A 2
H20C H 0.1395 0.1696 0.3879 0.071 Uiso 0.4 1 calc R U P A 2
H20D H 0.1725 0.2146 0.3277 0.071 Uiso 0.4 1 calc R U P A 2
C21A C 0.0936(7) 0.1983(6) 0.2771(9) 0.053(3) Uani 0.4 1 d . . P A 2
H21C H 0.1077 0.1705 0.2327 0.063 Uiso 0.4 1 calc R U P A 2
H21D H 0.0583 0.1841 0.3029 0.063 Uiso 0.4 1 calc R U P A 2
N1A N 0.0828(6) 0.2528(5) 0.2273(9) 0.035(2) Uani 0.4 1 d . . P A 2
H1A H 0.1172 0.2639 0.1933 0.042 Uiso 0.4 1 calc R U 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
Zn1 O1 2.0140(17) . ?
Zn1 O1 2.0140(17) 5 ?
Zn1 N2 2.118(2) 5 ?
Zn1 N2 2.118(2) . ?
Zn1 N1 2.257(9) . ?
Zn1 N1 2.257(9) 5 ?
Zn1 N1A 2.307(15) . ?
Zn1 N1A 2.307(15) 5 ?
O1 C1 1.292(3) . ?
N1 C21 1.435(13) . ?
N1 C17 1.481(9) . ?
N1 H1 1.0000 . ?
C1 C6 1.425(3) . ?
C1 C2 1.437(3) . ?
N2 C15 1.284(3) . ?
N2 C16 1.444(11) . ?
N2 C16A 1.519(15) . ?
C2 C3 1.378(3) . ?
C2 C7 1.531(3) . ?
C3 C4 1.406(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(4) . ?
C4 C11 1.539(3) . ?
C5 C6 1.416(3) . ?
C5 H5 0.9500 . ?
C6 C15 1.436(3) . ?
C7 C8 1.522(4) . ?
C7 C10 1.531(4) . ?
C7 C9 1.532(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.512(5) . ?
C11 C14 1.526(5) . ?
C11 C13 1.529(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?
C16 C17 1.531(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.552(15) . ?
C17 H17 1.0000 . ?
C18 C19 1.488(14) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.549(16) . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C20 C21 1.535(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C16A C17A 1.492(18) . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C17A N1A 1.451(17) . ?
C17A C18A 1.47(2) . ?
C17A H17A 1.0000 . ?
C18A C19A 1.54(2) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
C19A C20A 1.47(3) . ?
C19A H19A 0.9900 . ?
C19A H19B 0.9900 . ?
C20A C21A 1.52(3) . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C21A N1A 1.52(2) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
N1A H1A 1.0000 . ?

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 Zn1 O1 99.32(11) . 5 ?
O1 Zn1 N2 98.74(8) . 5 ?
O1 Zn1 N2 86.76(7) 5 5 ?
O1 Zn1 N2 86.76(7) . . ?
O1 Zn1 N2 98.74(8) 5 . ?
N2 Zn1 N2 171.56(12) 5 . ?
O1 Zn1 N1 165.6(2) . . ?
O1 Zn1 N1 82.04(17) 5 . ?
N2 Zn1 N1 95.6(2) 5 . ?
N2 Zn1 N1 78.9(2) . . ?
O1 Zn1 N1 82.04(17) . 5 ?
O1 Zn1 N1 165.6(2) 5 5 ?
N2 Zn1 N1 78.9(2) 5 5 ?
N2 Zn1 N1 95.6(2) . 5 ?
N1 Zn1 N1 100.2(4) . 5 ?
O1 Zn1 N1A 158.4(3) . . ?
O1 Zn1 N1A 93.4(2) 5 . ?
N2 Zn1 N1A 99.4(4) 5 . ?
N2 Zn1 N1A 74.0(4) . . ?
O1 Zn1 N1A 93.4(2) . 5 ?
O1 Zn1 N1A 158.4(3) 5 5 ?
N2 Zn1 N1A 74.0(4) 5 5 ?
N2 Zn1 N1A 99.4(4) . 5 ?
N1A Zn1 N1A 80.4(6) . 5 ?
C1 O1 Zn1 132.90(16) . . ?
C21 N1 C17 113.1(8) . . ?
C21 N1 Zn1 122.9(6) . . ?
C17 N1 Zn1 108.0(5) . . ?
C21 N1 H1 103.5 . . ?
C17 N1 H1 103.5 . . ?
Zn1 N1 H1 103.5 . . ?
O1 C1 C6 123.0(2) . . ?
O1 C1 C2 119.4(2) . . ?
C6 C1 C2 117.6(2) . . ?
C15 N2 C16 120.6(4) . . ?
C15 N2 C16A 115.0(6) . . ?
C15 N2 Zn1 125.83(16) . . ?
C16 N2 Zn1 113.1(4) . . ?
C16A N2 Zn1 117.8(6) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 C7 122.0(2) . . ?
C1 C2 C7 119.5(2) . . ?
C2 C3 C4 124.6(2) . . ?
C2 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
C5 C4 C3 116.6(2) . . ?
C5 C4 C11 123.9(2) . . ?
C3 C4 C11 119.4(2) . . ?
C4 C5 C6 122.3(2) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C15 116.3(2) . . ?
C1 C6 C15 123.4(2) . . ?
C8 C7 C2 110.4(2) . . ?
C8 C7 C10 107.2(3) . . ?
C2 C7 C10 111.7(2) . . ?
C8 C7 C9 109.7(2) . . ?
C2 C7 C9 110.6(2) . . ?
C10 C7 C9 107.1(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C14 109.9(4) . . ?
C12 C11 C13 107.9(3) . . ?
C14 C11 C13 107.9(3) . . ?
C12 C11 C4 112.0(2) . . ?
C14 C11 C4 109.5(3) . . ?
C13 C11 C4 109.6(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C6 127.7(2) . . ?
N2 C15 H15 116.2 . . ?
C6 C15 H15 116.2 . . ?
N2 C16 C17 110.8(7) . . ?
N2 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
N1 C17 C16 108.4(6) . . ?
N1 C17 C18 112.3(7) . . ?
C16 C17 C18 114.3(7) . . ?
N1 C17 H17 107.1 . . ?
C16 C17 H17 107.1 . . ?
C18 C17 H17 107.1 . . ?
C19 C18 C17 110.8(8) . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 C20 114.0(8) . . ?
C18 C19 H19C 108.8 . . ?
C20 C19 H19C 108.8 . . ?
C18 C19 H19D 108.8 . . ?
C20 C19 H19D 108.8 . . ?
H19C C19 H19D 107.7 . . ?
C21 C20 C19 108.7(9) . . ?
C21 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N1 C21 C20 113.5(9) . . ?
N1 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
N1 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C17A C16A N2 105.1(8) . . ?
C17A C16A H16C 110.7 . . ?
N2 C16A H16C 110.7 . . ?
C17A C16A H16D 110.7 . . ?
N2 C16A H16D 110.7 . . ?
H16C C16A H16D 108.8 . . ?
N1A C17A C18A 115.3(11) . . ?
N1A C17A C16A 106.7(9) . . ?
C18A C17A C16A 112.6(12) . . ?
N1A C17A H17A 107.3 . . ?
C18A C17A H17A 107.3 . . ?
C16A C17A H17A 107.3 . . ?
C17A C18A C19A 112.5(15) . . ?
C17A C18A H18C 109.1 . . ?
C19A C18A H18C 109.1 . . ?
C17A C18A H18D 109.1 . . ?
C19A C18A H18D 109.1 . . ?
H18C C18A H18D 107.8 . . ?
C20A C19A C18A 109.6(13) . . ?
C20A C19A H19A 109.7 . . ?
C18A C19A H19A 109.7 . . ?
C20A C19A H19B 109.7 . . ?
C18A C19A H19B 109.7 . . ?
H19A C19A H19B 108.2 . . ?
C19A C20A C21A 112.8(16) . . ?
C19A C20A H20C 109.0 . . ?
C21A C20A H20C 109.0 . . ?
C19A C20A H20D 109.0 . . ?
C21A C20A H20D 109.0 . . ?
H20C C20A H20D 107.8 . . ?
N1A C21A C20A 111.8(14) . . ?
N1A C21A H21C 109.3 . . ?
C20A C21A H21C 109.3 . . ?
N1A C21A H21D 109.3 . . ?
C20A C21A H21D 109.3 . . ?
H21C C21A H21D 107.9 . . ?
C17A N1A C21A 110.4(10) . . ?
C17A N1A Zn1 105.5(9) . . ?
C21A N1A Zn1 114.4(9) . . ?
C17A N1A H1A 108.8 . . ?
C21A N1A H1A 108.8 . . ?
Zn1 N1A H1A 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 C6 0.1(4) . . . . ?
Zn1 O1 C1 C2 179.67(16) . . . . ?
O1 C1 C2 C3 -175.9(2) . . . . ?
C6 C1 C2 C3 3.8(3) . . . . ?
O1 C1 C2 C7 4.1(3) . . . . ?
C6 C1 C2 C7 -176.3(2) . . . . ?
C1 C2 C3 C4 -1.7(4) . . . . ?
C7 C2 C3 C4 178.4(2) . . . . ?
C2 C3 C4 C5 -1.3(4) . . . . ?
C2 C3 C4 C11 179.4(2) . . . . ?
C3 C4 C5 C6 2.1(4) . . . . ?
C11 C4 C5 C6 -178.6(2) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C4 C5 C6 C15 -178.3(2) . . . . ?
O1 C1 C6 C5 176.6(2) . . . . ?
C2 C1 C6 C5 -3.0(3) . . . . ?
O1 C1 C6 C15 -5.1(4) . . . . ?
C2 C1 C6 C15 175.3(2) . . . . ?
C3 C2 C7 C8 -121.9(3) . . . . ?
C1 C2 C7 C8 58.2(3) . . . . ?
C3 C2 C7 C10 -2.7(4) . . . . ?
C1 C2 C7 C10 177.3(2) . . . . ?
C3 C2 C7 C9 116.5(3) . . . . ?
C1 C2 C7 C9 -63.4(3) . . . . ?
C5 C4 C11 C12 -1.5(4) . . . . ?
C3 C4 C11 C12 177.7(3) . . . . ?
C5 C4 C11 C14 120.6(3) . . . . ?
C3 C4 C11 C14 -60.1(3) . . . . ?
C5 C4 C11 C13 -121.2(3) . . . . ?
C3 C4 C11 C13 58.0(3) . . . . ?
C16 N2 C15 C6 -169.4(4) . . . . ?
C16A N2 C15 C6 169.1(5) . . . . ?
Zn1 N2 C15 C6 2.7(4) . . . . ?
C5 C6 C15 N2 -178.1(2) . . . . ?
C1 C6 C15 N2 3.5(4) . . . . ?
C15 N2 C16 C17 -149.7(4) . . . . ?
Zn1 N2 C16 C17 37.2(6) . . . . ?
C21 N1 C17 C16 178.7(7) . . . . ?
Zn1 N1 C17 C16 39.2(7) . . . . ?
C21 N1 C17 C18 -54.0(9) . . . . ?
Zn1 N1 C17 C18 166.5(6) . . . . ?
N2 C16 C17 N1 -51.3(7) . . . . ?
N2 C16 C17 C18 -177.4(7) . . . . ?
N1 C17 C18 C19 50.7(11) . . . . ?
C16 C17 C18 C19 174.7(7) . . . . ?
C17 C18 C19 C20 -51.0(12) . . . . ?
C18 C19 C20 C21 51.8(13) . . . . ?
C17 N1 C21 C20 56.7(10) . . . . ?
Zn1 N1 C21 C20 -170.7(6) . . . . ?
C19 C20 C21 N1 -53.7(12) . . . . ?
C15 N2 C16A C17A 164.2(6) . . . . ?
Zn1 N2 C16A C17A -28.3(10) . . . . ?
N2 C16A C17A N1A 56.2(11) . . . . ?
N2 C16A C17A C18A -176.4(10) . . . . ?
N1A C17A C18A C19A -53.6(16) . . . . ?
C16A C17A C18A C19A -176.3(11) . . . . ?
C17A C18A C19A C20A 52.3(17) . . . . ?
C18A C19A C20A C21A -53(2) . . . . ?
C19A C20A C21A N1A 55(2) . . . . ?
C18A C17A N1A C21A 52.6(15) . . . . ?
C16A C17A N1A C21A 178.4(10) . . . . ?
C18A C17A N1A Zn1 176.7(11) . . . . ?
C16A C17A N1A Zn1 -57.5(8) . . . . ?
C20A C21A N1A C17A -51.7(17) . . . . ?
C20A C21A N1A Zn1 -170.5(12) . . . . ?

_refine_diff_density_max         0.169
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.030

