#Supplementary Material (ESI) for Dalton Transactions
#This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Michael Hill'
_publ_contact_author_address     
;
Department of Chemistry
University of Bath
Bath
BA2 7AY
UNITED KINGDOM
;

_publ_contact_author_email       MSH27@BATH.AC.UK

_publ_section_title              
;
Reversibility in the protonolysis of a
beta-diketiminate stabilised calcium bis(trimethylsilyl)amide with
benzylamine
;
loop_
_publ_author_name
'Michael Hill'
'A. Barrett'
'Mark R. Crimmin'
'Garbriele I. Kociok-Kohn'
'Jennifer R. Lachs'
;
P.Procopiou
;

data_k07msh3
_database_code_depnum_ccdc_archive 'CCDC 667077'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H98 Ca2 N6'
_chemical_formula_sum            'C72 H98 Ca2 N6'
_chemical_formula_weight         1127.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'

loop_
_symmetry_equiv_pos_as_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                   11.5238(2)
_cell_length_b                   20.5104(3)
_cell_length_c                   14.4226(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6660(10)
_cell_angle_gamma                90.00
_cell_volume                     3397.60(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    42141
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '239 1.5 degree images with \w scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            44109
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.99
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7741
_reflns_number_gt                5632
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_reduction        
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
SHELXL97 -Program for Crystal Structure Analysis (Release 97-2).
Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at,
Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998
;
_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          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+1.6642P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7741
_refine_ls_number_parameters     367
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1354
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca Ca 0.55442(4) 0.054151(18) 0.58629(3) 0.03051(11) Uani 1 1 d . . .
N1 N 0.55239(14) 0.04602(7) 0.74878(10) 0.0292(3) Uani 1 1 d . . .
C1 C 0.54849(19) -0.01779(9) 0.78925(12) 0.0326(4) Uani 1 1 d . . .
C2 C 0.4460(2) -0.05527(10) 0.77732(14) 0.0374(4) Uani 1 1 d . . .
C3 C 0.3355(2) -0.02814(11) 0.72654(17) 0.0453(5) Uani 1 1 d . . .
H3 H 0.3599 0.0068 0.6839 0.054 Uiso 1 1 calc R . .
C4 C 0.2571(3) 0.0037(3) 0.7928(3) 0.1078(15) Uani 1 1 d . . .
H4A H 0.3019 0.0357 0.8314 0.162 Uiso 1 1 calc R . .
H4B H 0.2264 -0.0297 0.8329 0.162 Uiso 1 1 calc R . .
H4C H 0.1924 0.0255 0.7572 0.162 Uiso 1 1 calc R . .
C5 C 0.2665(4) -0.07693(16) 0.6673(3) 0.0895(12) Uani 1 1 d . . .
H5A H 0.1973 -0.0557 0.6368 0.134 Uiso 1 1 calc R . .
H5B H 0.2425 -0.1128 0.7064 0.134 Uiso 1 1 calc R . .
H5C H 0.3146 -0.0941 0.6199 0.134 Uiso 1 1 calc R . .
C6 C 0.4465(2) -0.11797(11) 0.81512(16) 0.0474(6) Uani 1 1 d . . .
H6 H 0.3782 -0.1439 0.8069 0.057 Uiso 1 1 calc R . .
C7 C 0.5448(3) -0.14307(11) 0.86444(16) 0.0499(6) Uani 1 1 d . . .
H7 H 0.5429 -0.1854 0.8912 0.060 Uiso 1 1 calc R . .
C8 C 0.6445(2) -0.10661(10) 0.87441(15) 0.0466(6) Uani 1 1 d . . .
H8 H 0.7119 -0.1244 0.9075 0.056 Uiso 1 1 calc R . .
C9 C 0.6497(2) -0.04382(10) 0.83701(14) 0.0384(5) Uani 1 1 d . . .
C10 C 0.7648(2) -0.00713(11) 0.84575(17) 0.0488(6) Uani 1 1 d . . .
H10 H 0.7514 0.0370 0.8173 0.059 Uiso 1 1 calc R . .
C11 C 0.8543(3) -0.04236(14) 0.7921(2) 0.0645(7) Uani 1 1 d . . .
H11A H 0.9279 -0.0182 0.7979 0.097 Uiso 1 1 calc R . .
H11B H 0.8258 -0.0453 0.7263 0.097 Uiso 1 1 calc R . .
H11C H 0.8669 -0.0864 0.8174 0.097 Uiso 1 1 calc R . .
C12 C 0.8120(3) 0.00235(17) 0.9474(2) 0.0784(9) Uani 1 1 d . . .
H12A H 0.8858 0.0262 0.9496 0.118 Uiso 1 1 calc R . .
H12B H 0.8247 -0.0403 0.9771 0.118 Uiso 1 1 calc R . .
H12C H 0.7555 0.0272 0.9805 0.118 Uiso 1 1 calc R . .
N2 N 0.64959(13) 0.15271(7) 0.62532(10) 0.0266(3) Uani 1 1 d . . .
C13 C 0.72338(17) 0.17972(9) 0.55965(13) 0.0298(4) Uani 1 1 d . . .
C14 C 0.83993(18) 0.15748(10) 0.56327(14) 0.0346(4) Uani 1 1 d . . .
C15 C 0.88586(18) 0.10756(11) 0.63501(15) 0.0386(5) Uani 1 1 d . . .
H15 H 0.8172 0.0823 0.6537 0.046 Uiso 1 1 calc R . .
C16 C 0.9413(3) 0.14000(15) 0.7222(2) 0.0785(10) Uani 1 1 d . . .
H16A H 0.9694 0.1065 0.7670 0.118 Uiso 1 1 calc R . .
H16B H 0.8834 0.1674 0.7497 0.118 Uiso 1 1 calc R . .
H16C H 1.0067 0.1671 0.7061 0.118 Uiso 1 1 calc R . .
C17 C 0.9691(2) 0.05870(13) 0.59658(19) 0.0528(6) Uani 1 1 d . . .
H17A H 0.9953 0.0276 0.6455 0.079 Uiso 1 1 calc R . .
H17B H 1.0365 0.0818 0.5754 0.079 Uiso 1 1 calc R . .
H17C H 0.9290 0.0352 0.5442 0.079 Uiso 1 1 calc R . .
C18 C 0.9132(2) 0.18247(12) 0.50013(17) 0.0460(5) Uani 1 1 d . . .
H18 H 0.9918 0.1682 0.5024 0.055 Uiso 1 1 calc R . .
C19 C 0.8735(2) 0.22793(13) 0.43385(17) 0.0515(6) Uani 1 1 d . . .
H19 H 0.9253 0.2455 0.3923 0.062 Uiso 1 1 calc R . .
C20 C 0.7594(2) 0.24756(11) 0.42835(16) 0.0467(5) Uani 1 1 d . . .
H20 H 0.7325 0.2778 0.3816 0.056 Uiso 1 1 calc R . .
C21 C 0.68146(19) 0.22397(10) 0.49013(14) 0.0354(4) Uani 1 1 d . . .
C22 C 0.5546(2) 0.24428(10) 0.47563(15) 0.0395(5) Uani 1 1 d . . .
H22 H 0.5122 0.2252 0.5270 0.047 Uiso 1 1 calc R . .
C23 C 0.5001(2) 0.21712(12) 0.38298(16) 0.0468(5) Uani 1 1 d . . .
H23A H 0.4183 0.2304 0.3742 0.070 Uiso 1 1 calc R . .
H23B H 0.5050 0.1694 0.3838 0.070 Uiso 1 1 calc R . .
H23C H 0.5423 0.2342 0.3318 0.070 Uiso 1 1 calc R . .
C24 C 0.5389(3) 0.31885(11) 0.47716(18) 0.0554(6) Uani 1 1 d . . .
H24A H 0.4559 0.3295 0.4678 0.083 Uiso 1 1 calc R . .
H24B H 0.5802 0.3385 0.4273 0.083 Uiso 1 1 calc R . .
H24C H 0.5708 0.3360 0.5374 0.083 Uiso 1 1 calc R . .
N3 N 0.61207(16) -0.04765(9) 0.52546(12) 0.0384(4) Uani 1 1 d . . .
H3A H 0.598(3) -0.0766(16) 0.578(2) 0.079(10) Uiso 1 1 d . . .
C25 C 0.7264(2) -0.06968(11) 0.50058(16) 0.0431(5) Uani 1 1 d . . .
H25A H 0.7830 -0.0649 0.5556 0.052 Uiso 1 1 calc R . .
H25B H 0.7521 -0.0409 0.4511 0.052 Uiso 1 1 calc R . .
C26 C 0.72888(17) -0.13944(10) 0.46719(15) 0.0369(4) Uani 1 1 d . . .
C27 C 0.6858(2) -0.15576(12) 0.37747(16) 0.0474(5) Uani 1 1 d . . .
H27 H 0.6575 -0.1225 0.3357 0.057 Uiso 1 1 calc R . .
C28 C 0.6837(3) -0.22050(14) 0.3480(2) 0.0613(7) Uani 1 1 d . . .
H28 H 0.6544 -0.2313 0.2865 0.074 Uiso 1 1 calc R . .
C29 C 0.7246(3) -0.26927(14) 0.4092(2) 0.0669(8) Uani 1 1 d . . .
H29 H 0.7216 -0.3136 0.3901 0.080 Uiso 1 1 calc R . .
C30 C 0.7692(3) -0.25312(14) 0.4972(2) 0.0650(8) Uani 1 1 d . . .
H30 H 0.7989 -0.2862 0.5387 0.078 Uiso 1 1 calc R . .
C31 C 0.7712(2) -0.18928(12) 0.52530(18) 0.0497(6) Uani 1 1 d . . .
H31 H 0.8024 -0.1789 0.5865 0.060 Uiso 1 1 calc R . .
C32 C 0.55085(17) 0.09759(9) 0.80440(13) 0.0306(4) Uani 1 1 d . . .
C33 C 0.5211(2) 0.09022(11) 0.90470(15) 0.0462(6) Uani 1 1 d . . .
H33A H 0.4847 0.0476 0.9128 0.069 Uiso 1 1 calc R . .
H33B H 0.4670 0.1248 0.9196 0.069 Uiso 1 1 calc R . .
H33C H 0.5924 0.0935 0.9463 0.069 Uiso 1 1 calc R . .
C34 C 0.57746(18) 0.16178(9) 0.77820(13) 0.0310(4) Uani 1 1 d . . .
H34 H 0.5553 0.1943 0.8202 0.037 Uiso 1 1 calc R . .
C35 C 0.63102(17) 0.18642(8) 0.70093(13) 0.0283(4) Uani 1 1 d . . .
C36 C 0.6714(2) 0.25683(9) 0.71049(15) 0.0413(5) Uani 1 1 d . . .
H36A H 0.7567 0.2582 0.7164 0.062 Uiso 1 1 calc R . .
H36B H 0.6416 0.2762 0.7660 0.062 Uiso 1 1 calc R . .
H36C H 0.6420 0.2815 0.6553 0.062 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ca 0.0404(2) 0.02795(18) 0.02318(18) -0.00466(14) 0.00289(14) -0.00665(16)
N1 0.0377(9) 0.0248(7) 0.0253(7) -0.0002(6) 0.0034(6) 0.0017(6)
C1 0.0483(12) 0.0276(9) 0.0225(8) -0.0001(7) 0.0061(8) 0.0031(8)
C2 0.0503(12) 0.0325(9) 0.0306(10) 0.0006(8) 0.0107(9) -0.0019(9)
C3 0.0469(13) 0.0407(11) 0.0487(13) 0.0023(10) 0.0058(10) -0.0087(10)
C4 0.067(2) 0.175(4) 0.082(2) -0.026(3) 0.0029(19) 0.047(3)
C5 0.104(3) 0.0582(17) 0.098(3) -0.0067(17) -0.045(2) -0.0077(18)
C6 0.0666(16) 0.0346(11) 0.0430(12) 0.0030(9) 0.0172(11) -0.0074(10)
C7 0.0826(19) 0.0302(10) 0.0385(12) 0.0065(9) 0.0154(12) 0.0032(11)
C8 0.0708(17) 0.0338(11) 0.0350(11) 0.0054(9) 0.0040(11) 0.0112(11)
C9 0.0545(13) 0.0320(10) 0.0287(10) 0.0003(8) 0.0033(9) 0.0057(9)
C10 0.0537(14) 0.0406(12) 0.0497(13) 0.0051(10) -0.0097(11) 0.0068(10)
C11 0.0581(17) 0.0590(16) 0.077(2) 0.0089(14) 0.0110(14) 0.0061(13)
C12 0.083(2) 0.080(2) 0.0672(19) -0.0095(16) -0.0253(17) 0.0025(17)
N2 0.0283(8) 0.0264(7) 0.0251(7) -0.0022(6) 0.0021(6) -0.0006(6)
C13 0.0324(10) 0.0287(9) 0.0286(9) -0.0071(7) 0.0040(7) -0.0064(7)
C14 0.0317(10) 0.0370(10) 0.0354(10) -0.0087(8) 0.0053(8) -0.0057(8)
C15 0.0310(10) 0.0434(11) 0.0412(11) -0.0084(9) 0.0010(8) 0.0048(9)
C16 0.104(3) 0.0644(17) 0.0601(17) -0.0223(14) -0.0352(17) 0.0230(17)
C17 0.0446(13) 0.0534(14) 0.0616(15) -0.0080(12) 0.0114(11) 0.0086(11)
C18 0.0332(11) 0.0541(13) 0.0522(13) -0.0090(11) 0.0123(10) -0.0122(10)
C19 0.0520(15) 0.0574(14) 0.0476(13) -0.0006(11) 0.0186(11) -0.0228(12)
C20 0.0578(15) 0.0442(12) 0.0392(12) 0.0048(9) 0.0102(10) -0.0134(11)
C21 0.0435(12) 0.0323(10) 0.0308(10) -0.0006(8) 0.0051(8) -0.0061(9)
C22 0.0462(12) 0.0371(10) 0.0348(11) 0.0058(8) 0.0012(9) 0.0023(9)
C23 0.0503(14) 0.0498(13) 0.0394(12) 0.0047(10) -0.0017(10) -0.0037(11)
C24 0.0722(18) 0.0400(12) 0.0526(14) 0.0005(10) -0.0029(13) 0.0056(12)
N3 0.0450(10) 0.0372(9) 0.0330(9) -0.0059(7) 0.0034(7) -0.0003(8)
C25 0.0391(12) 0.0483(12) 0.0412(12) -0.0045(9) -0.0015(9) -0.0038(10)
C26 0.0272(10) 0.0452(11) 0.0382(11) -0.0002(9) 0.0032(8) 0.0046(9)
C27 0.0467(13) 0.0574(14) 0.0382(12) -0.0025(10) 0.0039(10) 0.0094(11)
C28 0.0597(17) 0.0720(18) 0.0530(15) -0.0249(13) 0.0088(12) 0.0119(14)
C29 0.0593(17) 0.0536(15) 0.089(2) -0.0182(15) 0.0141(16) 0.0218(13)
C30 0.0519(16) 0.0547(15) 0.087(2) 0.0083(14) 0.0000(15) 0.0203(13)
C31 0.0385(12) 0.0587(14) 0.0510(13) 0.0075(11) -0.0021(10) 0.0094(11)
C32 0.0359(10) 0.0316(9) 0.0246(9) -0.0029(7) 0.0042(7) 0.0041(8)
C33 0.0733(17) 0.0372(11) 0.0305(10) -0.0022(9) 0.0177(10) 0.0012(11)
C34 0.0392(11) 0.0267(9) 0.0276(9) -0.0053(7) 0.0069(8) 0.0045(8)
C35 0.0328(10) 0.0234(8) 0.0284(9) -0.0034(7) 0.0008(7) 0.0012(7)
C36 0.0601(14) 0.0287(10) 0.0357(11) -0.0060(8) 0.0073(10) -0.0079(9)

_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
Ca N2 2.3464(15) . ?
Ca N1 2.3514(15) . ?
Ca N3 2.3802(17) . ?
Ca N3 2.4069(19) 3_656 ?
Ca Ca 3.4921(7) 3_656 ?
Ca H3A 2.73(3) . ?
N1 C32 1.329(2) . ?
N1 C1 1.435(2) . ?
C1 C2 1.408(3) . ?
C1 C9 1.411(3) . ?
C2 C6 1.397(3) . ?
C2 C3 1.522(3) . ?
C3 C5 1.501(4) . ?
C3 C4 1.515(4) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.387(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.369(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.399(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.522(3) . ?
C10 C11 1.521(4) . ?
C10 C12 1.534(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N2 C35 1.323(2) . ?
N2 C13 1.435(2) . ?
C13 C21 1.408(3) . ?
C13 C14 1.415(3) . ?
C14 C18 1.389(3) . ?
C14 C15 1.520(3) . ?
C15 C16 1.517(3) . ?
C15 C17 1.522(3) . ?
C15 H15 1.0000 . ?
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 C19 1.386(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.372(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.402(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.518(3) . ?
C22 C23 1.534(3) . ?
C22 C24 1.541(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N3 C25 1.465(3) . ?
N3 Ca 2.4069(19) 3_656 ?
N3 H3A 0.99(3) . ?
C25 C26 1.511(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.385(3) . ?
C26 C27 1.389(3) . ?
C27 C28 1.393(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.391(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.371(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C34 1.410(3) . ?
C32 C33 1.521(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.411(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.520(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
N2 Ca N1 82.20(5) . . ?
N2 Ca N3 134.84(6) . . ?
N1 Ca N3 109.32(6) . . ?
N2 Ca N3 122.68(6) . 3_656 ?
N1 Ca N3 126.26(6) . 3_656 ?
N3 Ca N3 86.32(7) . 3_656 ?
N2 Ca Ca 148.52(4) . 3_656 ?
N1 Ca Ca 129.28(4) . 3_656 ?
N3 Ca Ca 43.46(4) . 3_656 ?
N3 Ca Ca 42.86(4) 3_656 3_656 ?
N2 Ca H3A 140.6(7) . . ?
N1 Ca H3A 89.5(7) . . ?
N3 Ca H3A 20.8(7) . . ?
N3 Ca H3A 93.1(7) 3_656 . ?
Ca Ca H3A 53.2(7) 3_656 . ?
C32 N1 C1 118.56(15) . . ?
C32 N1 Ca 123.17(12) . . ?
C1 N1 Ca 118.24(11) . . ?
C2 C1 C9 120.35(18) . . ?
C2 C1 N1 120.12(18) . . ?
C9 C1 N1 119.46(19) . . ?
C6 C2 C1 118.6(2) . . ?
C6 C2 C3 120.1(2) . . ?
C1 C2 C3 121.33(18) . . ?
C5 C3 C4 109.3(3) . . ?
C5 C3 C2 114.5(2) . . ?
C4 C3 C2 111.8(2) . . ?
C5 C3 H3 106.9 . . ?
C4 C3 H3 106.9 . . ?
C2 C3 H3 106.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C2 121.3(2) . . ?
C7 C6 H6 119.3 . . ?
C2 C6 H6 119.3 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 121.6(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C1 118.5(2) . . ?
C8 C9 C10 119.2(2) . . ?
C1 C9 C10 122.28(18) . . ?
C11 C10 C9 110.2(2) . . ?
C11 C10 C12 110.2(2) . . ?
C9 C10 C12 112.4(2) . . ?
C11 C10 H10 108.0 . . ?
C9 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C35 N2 C13 119.12(15) . . ?
C35 N2 Ca 122.96(12) . . ?
C13 N2 Ca 117.70(11) . . ?
C21 C13 C14 120.23(18) . . ?
C21 C13 N2 122.10(18) . . ?
C14 C13 N2 117.57(17) . . ?
C18 C14 C13 118.9(2) . . ?
C18 C14 C15 119.9(2) . . ?
C13 C14 C15 121.27(18) . . ?
C16 C15 C14 111.63(19) . . ?
C16 C15 C17 110.8(2) . . ?
C14 C15 C17 112.98(19) . . ?
C16 C15 H15 107.0 . . ?
C14 C15 H15 107.0 . . ?
C17 C15 H15 107.0 . . ?
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 . . ?
C19 C18 C14 121.1(2) . . ?
C19 C18 H18 119.5 . . ?
C14 C18 H18 119.5 . . ?
C20 C19 C18 119.9(2) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 121.5(2) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C13 118.3(2) . . ?
C20 C21 C22 118.50(19) . . ?
C13 C21 C22 123.07(18) . . ?
C21 C22 C23 109.97(18) . . ?
C21 C22 C24 112.5(2) . . ?
C23 C22 C24 109.45(18) . . ?
C21 C22 H22 108.3 . . ?
C23 C22 H22 108.3 . . ?
C24 C22 H22 108.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 N3 Ca 130.12(14) . . ?
C25 N3 Ca 120.18(13) . 3_656 ?
Ca N3 Ca 93.68(7) . 3_656 ?
C25 N3 H3A 102.2(19) . . ?
Ca N3 H3A 100.2(19) . . ?
Ca N3 H3A 107.9(19) 3_656 . ?
N3 C25 C26 114.25(18) . . ?
N3 C25 H25A 108.7 . . ?
C26 C25 H25A 108.7 . . ?
N3 C25 H25B 108.7 . . ?
C26 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C31 C26 C27 117.9(2) . . ?
C31 C26 C25 121.4(2) . . ?
C27 C26 C25 120.7(2) . . ?
C26 C27 C28 120.6(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 119.7(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.1(3) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C26 122.0(2) . . ?
C30 C31 H31 119.0 . . ?
C26 C31 H31 119.0 . . ?
N1 C32 C34 124.58(17) . . ?
N1 C32 C33 120.68(17) . . ?
C34 C32 C33 114.74(17) . . ?
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 C35 131.67(17) . . ?
C32 C34 H34 114.2 . . ?
C35 C34 H34 114.2 . . ?
N2 C35 C34 125.05(16) . . ?
N2 C35 C36 120.15(17) . . ?
C34 C35 C36 114.78(16) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.046