# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Malcolm Chisholm'
'Judith Gallucci'
'Gulsah Yaman'
'Tanya Young'

_publ_contact_author_name        'Malcolm Chisholm'
_publ_contact_author_email       CHISHOLM@CHEMISTRY.OHIO-STATE.EDU

_publ_section_title              
;
On the Remarkable Structural Diversity and Kinetic
Lability of TpC*CaX Complexes ( X = NSi2Me6, OC6H4-p-Me, TpC*) where
TpC* = tris[3-(2-methoxy-1
;
_publ_requested_category         FM

# Attachment 'ca4.txt'

data_ChisholmCMC0525
_database_code_depnum_ccdc_archive 'CCDC 705806'

_audit_creation_date             2008-10-01T14:39:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C30 H58 B Ca N7 O3 Si2'
_chemical_formula_sum            'C30 H58 B Ca N7 O3 Si2'
_chemical_formula_weight         671.9
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   13.1496(5)
_cell_length_b                   15.5703(8)
_cell_length_c                   18.9206(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.351(2)
_cell_angle_gamma                90
_cell_volume                     3822.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    95(2)
_cell_measurement_wavelength     0.49595
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01

_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_special_details           
;Because of the small size of the crystal, a synchrotron data set was
collected at The Advanced Photon Source at the beamline
ChemMatCARS Sector 15 by Dr. Maren Pink of Indiana University.
All work was done at 95 K using a Bruker Smart6000 diffractometer.
The data collection strategy was set up to measure
a hemisphere of reciprocal space. Phi and omega scans with a frame
width of 0.5 degrees and an exposure time of 1 second were used. Data
integration was done with SAINT and scaling of the data was done
with SADABS.
;
_publ_section_acknowledgements   
; We thank Dr. Maren Pink of Indiana University for the data collection at
The Advanced Photon Source at the beamline ChemMatCARS, Sector 15.
ChemMatCARS Sector 15 is principally supported by the National Science
Foundation/Department of Energy under grant number CHE0087817 and by
the Illinois Board of Higher Education. The Advanced Photon Source is
supported by the U.S. Department of Energy, Basic Energy Sciences,
Office of Science, under Contract No. W-31-109-Eng-38.
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_process_details   'SADABS, version 2.10 (Sheldrick)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      95(2)
_diffrn_radiation_wavelength     0.49595
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_measurement_details      '0.5 degree frames measured for 1 second each'
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_number            42864
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         20.32
_diffrn_reflns_theta_full        20.32
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_reflns_number_total             10864
_reflns_number_gt                8923
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection       'SAINT, Bruker AXS, 2003'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;For the methyl groups, the hydrogen atoms were added at calculated positions
using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The torsion
angle, which defines the orientation of the methyl group about the C-C, O-C,
or Si-C bond, was refined. The remaining hydrogen atoms were
included in the model at calculated positions using a riding model with
U(H) = 1.2 * Ueq(attached atom).

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     
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.8539P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10864
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.086

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0007 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0003 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0018 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0039 0.0027 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0411 0.0336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1332 0.1518 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.30929(10) 0.32785(9) 0.82446(7) 0.0103(2) Uani 1 1 d . . .
C2 C 0.24889(11) 0.40201(9) 0.81222(8) 0.0133(3) Uani 1 1 d . . .
H2 H 0.2251 0.4377 0.8468 0.016 Uiso 1 1 calc R . .
C3 C 0.23140(10) 0.41189(9) 0.73855(8) 0.0118(3) Uani 1 1 d . . .
H3 H 0.1923 0.4565 0.7128 0.014 Uiso 1 1 calc R . .
C4 C 0.35115(11) 0.28640(10) 0.89564(7) 0.0141(3) Uani 1 1 d . . .
C5 C 0.42971(14) 0.34766(12) 0.93927(9) 0.0251(4) Uani 1 1 d . . .
H5A H 0.4867 0.3584 0.9128 0.038 Uiso 1 1 calc R . .
H5B H 0.4566 0.3214 0.9856 0.038 Uiso 1 1 calc R . .
H5C H 0.3958 0.4021 0.9471 0.038 Uiso 1 1 calc R . .
C6 C 0.26269(12) 0.26998(11) 0.93752(8) 0.0193(3) Uani 1 1 d . . .
H6A H 0.2276 0.3243 0.944 0.029 Uiso 1 1 calc R . .
H6B H 0.2903 0.2456 0.9845 0.029 Uiso 1 1 calc R . .
H6C H 0.2136 0.2296 0.9109 0.029 Uiso 1 1 calc R . .
C7 C 0.40972(12) 0.20379(11) 0.88541(8) 0.0182(3) Uani 1 1 d . . .
H7A H 0.4679 0.2177 0.8602 0.022 Uiso 1 1 calc R . .
H7B H 0.439 0.1805 0.9331 0.022 Uiso 1 1 calc R . .
C8 C 0.31781(16) 0.06893(12) 0.88782(11) 0.0313(4) Uani 1 1 d . . .
H8A H 0.3796 0.0385 0.911 0.047 Uiso 1 1 calc R . .
H8B H 0.2733 0.0291 0.8568 0.047 Uiso 1 1 calc R . .
H8C H 0.2803 0.0917 0.9245 0.047 Uiso 1 1 calc R . .
C9 C 0.19789(10) 0.51631(9) 0.53684(7) 0.0113(3) Uani 1 1 d . . .
C10 C 0.12125(11) 0.46277(10) 0.49916(8) 0.0147(3) Uani 1 1 d . . .
H10 H 0.0678 0.4784 0.4613 0.018 Uiso 1 1 calc R . .
C11 C 0.14092(10) 0.38290(9) 0.52923(8) 0.0126(3) Uani 1 1 d . . .
H11 H 0.1024 0.3322 0.516 0.015 Uiso 1 1 calc R . .
C12 C 0.20992(11) 0.61249(9) 0.53273(8) 0.0144(3) Uani 1 1 d . . .
C13 C 0.32412(12) 0.63741(11) 0.54654(9) 0.0205(3) Uani 1 1 d . . .
H13A H 0.355 0.6195 0.5949 0.031 Uiso 1 1 calc R . .
H13B H 0.3306 0.6998 0.5421 0.031 Uiso 1 1 calc R . .
H13C H 0.3598 0.6089 0.5114 0.031 Uiso 1 1 calc R . .
C14 C 0.15473(14) 0.65394(11) 0.58982(9) 0.0222(3) Uani 1 1 d . . .
H14A H 0.0811 0.6402 0.5796 0.033 Uiso 1 1 calc R . .
H14B H 0.1638 0.7164 0.5891 0.033 Uiso 1 1 calc R . .
H14C H 0.1841 0.6317 0.6372 0.033 Uiso 1 1 calc R . .
C15 C 0.15772(11) 0.64672(10) 0.46029(8) 0.0165(3) Uani 1 1 d . . .
H15A H 0.0839 0.6306 0.4524 0.02 Uiso 1 1 calc R . .
H15B H 0.1622 0.7102 0.4601 0.02 Uiso 1 1 calc R . .
C16 C 0.15241(14) 0.63877(13) 0.33624(9) 0.0273(4) Uani 1 1 d . . .
H16A H 0.0795 0.623 0.3319 0.041 Uiso 1 1 calc R . .
H16B H 0.1827 0.6101 0.2985 0.041 Uiso 1 1 calc R . .
H16C H 0.1585 0.7011 0.3313 0.041 Uiso 1 1 calc R . .
C17 C 0.52595(10) 0.22357(9) 0.63587(7) 0.0109(2) Uani 1 1 d . . .
C18 C 0.55175(11) 0.30423(10) 0.61147(8) 0.0140(3) Uani 1 1 d . . .
H18 H 0.6176 0.3234 0.6036 0.017 Uiso 1 1 calc R . .
C19 C 0.46035(11) 0.34987(9) 0.60142(7) 0.0119(3) Uani 1 1 d . . .
H19 H 0.4518 0.4075 0.5851 0.014 Uiso 1 1 calc R . .
C20 C 0.59559(10) 0.14719(10) 0.65628(8) 0.0132(3) Uani 1 1 d . . .
C21 C 0.66239(13) 0.13185(12) 0.59796(9) 0.0227(3) Uani 1 1 d . . .
H21A H 0.6182 0.115 0.5533 0.034 Uiso 1 1 calc R . .
H21B H 0.7122 0.086 0.6133 0.034 Uiso 1 1 calc R . .
H21C H 0.6993 0.1848 0.5901 0.034 Uiso 1 1 calc R . .
C22 C 0.66562(12) 0.16545(11) 0.72804(9) 0.0215(3) Uani 1 1 d . . .
H22A H 0.7061 0.2175 0.7237 0.032 Uiso 1 1 calc R . .
H22B H 0.7123 0.1168 0.7407 0.032 Uiso 1 1 calc R . .
H22C H 0.6231 0.1737 0.7655 0.032 Uiso 1 1 calc R . .
C23 C 0.53351(11) 0.06548(10) 0.66143(8) 0.0147(3) Uani 1 1 d . . .
H23A H 0.4843 0.058 0.6163 0.018 Uiso 1 1 calc R . .
H23B H 0.5809 0.0157 0.6665 0.018 Uiso 1 1 calc R . .
C24 C 0.51341(12) 0.00322(11) 0.77485(9) 0.0216(3) Uani 1 1 d . . .
H24A H 0.5138 -0.0536 0.7526 0.032 Uiso 1 1 calc R . .
H24B H 0.4678 0.0023 0.811 0.032 Uiso 1 1 calc R . .
H24C H 0.5835 0.0181 0.7977 0.032 Uiso 1 1 calc R . .
C25 C 0.07248(13) -0.09863(11) 0.61303(10) 0.0255(4) Uani 1 1 d . . .
H25A H 0.0674 -0.1284 0.6579 0.038 Uiso 1 1 calc R . .
H25B H 0.0799 -0.1409 0.5758 0.038 Uiso 1 1 calc R . .
H25C H 0.01 -0.0646 0.5982 0.038 Uiso 1 1 calc R . .
C26 C 0.20640(16) 0.01288(14) 0.53545(10) 0.0322(4) Uani 1 1 d . . .
H26A H 0.147 0.0477 0.5146 0.048 Uiso 1 1 calc R . .
H26B H 0.2125 -0.0367 0.5045 0.048 Uiso 1 1 calc R . .
H26C H 0.2692 0.0476 0.5397 0.048 Uiso 1 1 calc R . .
C27 C 0.30235(13) -0.09701(12) 0.65735(11) 0.0273(4) Uani 1 1 d . . .
H27A H 0.3661 -0.065 0.6555 0.041 Uiso 1 1 calc R . .
H27B H 0.2993 -0.1472 0.6259 0.041 Uiso 1 1 calc R . .
H27C H 0.3011 -0.1159 0.7066 0.041 Uiso 1 1 calc R . .
C28 C 0.08906(12) 0.20542(11) 0.74766(10) 0.0235(3) Uani 1 1 d . . .
H28A H 0.1362 0.1946 0.7925 0.035 Uiso 1 1 calc R . .
H28B H 0.0229 0.2261 0.7585 0.035 Uiso 1 1 calc R . .
H28C H 0.1189 0.2489 0.7197 0.035 Uiso 1 1 calc R . .
C29 C -0.01280(14) 0.03706(12) 0.74637(12) 0.0309(4) Uani 1 1 d . . .
H29A H -0.028 -0.0183 0.7223 0.046 Uiso 1 1 calc R . .
H29B H -0.0774 0.0674 0.749 0.046 Uiso 1 1 calc R . .
H29C H 0.0245 0.0274 0.7949 0.046 Uiso 1 1 calc R . .
C30 C -0.01566(15) 0.13391(13) 0.60770(11) 0.0320(4) Uani 1 1 d . . .
H30A H 0.0202 0.1765 0.5826 0.048 Uiso 1 1 calc R . .
H30B H -0.0805 0.1583 0.6177 0.048 Uiso 1 1 calc R . .
H30C H -0.0303 0.0827 0.5776 0.048 Uiso 1 1 calc R . .
B B 0.27464(11) 0.31934(10) 0.63050(8) 0.0094(3) Uani 1 1 d . . .
H1B H 0.2321 0.266 0.6221 0.011 Uiso 1 1 calc R . .
N1 N 0.27904(9) 0.34773(7) 0.70954(6) 0.0095(2) Uani 1 1 d . . .
N2 N 0.32675(9) 0.29437(7) 0.76237(6) 0.0096(2) Uani 1 1 d . . .
N3 N 0.22468(9) 0.38907(8) 0.58094(6) 0.0110(2) Uani 1 1 d . . .
N4 N 0.26075(9) 0.47170(8) 0.58600(6) 0.0126(2) Uani 1 1 d . . .
N5 N 0.38557(9) 0.29893(7) 0.61860(6) 0.0095(2) Uani 1 1 d . . .
N6 N 0.42526(9) 0.22035(8) 0.64009(6) 0.0099(2) Uani 1 1 d . . .
N7 N 0.18185(9) 0.05768(8) 0.68360(7) 0.0130(2) Uani 1 1 d . . .
O1 O 0.34743(9) 0.13846(7) 0.84562(6) 0.0174(2) Uani 1 1 d . . .
O2 O 0.20539(9) 0.61283(8) 0.40432(6) 0.0201(2) Uani 1 1 d . . .
O3 O 0.47695(8) 0.06610(7) 0.72091(6) 0.0156(2) Uani 1 1 d . . .
Si1 Si 0.06831(3) 0.10332(3) 0.69464(2) 0.01483(9) Uani 1 1 d . . .
Si2 Si 0.18808(3) -0.02561(3) 0.62682(2) 0.01536(9) Uani 1 1 d . . .
Ca Ca 0.32234(2) 0.145681(18) 0.718839(15) 0.00966(7) Uani 1 1 d . . .

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
C1 0.0101(6) 0.0110(6) 0.0100(6) -0.0004(5) 0.0017(5) -0.0022(5)
C2 0.0158(6) 0.0115(6) 0.0134(6) -0.0015(5) 0.0050(5) -0.0007(5)
C3 0.0124(6) 0.0095(6) 0.0143(6) 0.0000(5) 0.0042(5) 0.0012(5)
C4 0.0158(6) 0.0179(7) 0.0082(6) 0.0011(5) 0.0008(5) -0.0021(5)
C5 0.0272(8) 0.0312(9) 0.0148(7) 0.0000(6) -0.0033(6) -0.0080(7)
C6 0.0245(7) 0.0218(8) 0.0132(7) 0.0020(6) 0.0077(6) -0.0009(6)
C7 0.0173(7) 0.0237(8) 0.0128(7) 0.0053(6) 0.0001(5) 0.0022(6)
C8 0.0499(11) 0.0182(8) 0.0315(9) 0.0117(7) 0.0235(8) 0.0034(8)
C9 0.0103(6) 0.0128(6) 0.0111(6) 0.0019(5) 0.0023(5) 0.0028(5)
C10 0.0121(6) 0.0166(7) 0.0142(6) 0.0024(5) -0.0014(5) 0.0008(5)
C11 0.0102(6) 0.0142(7) 0.0128(6) 0.0003(5) 0.0002(5) 0.0002(5)
C12 0.0157(6) 0.0126(7) 0.0143(7) 0.0043(5) 0.0008(5) 0.0016(5)
C13 0.0179(7) 0.0184(8) 0.0234(8) 0.0071(6) -0.0022(6) -0.0051(6)
C14 0.0304(8) 0.0154(7) 0.0211(8) -0.0013(6) 0.0053(6) 0.0048(6)
C15 0.0164(6) 0.0142(7) 0.0183(7) 0.0054(6) 0.0010(5) 0.0035(5)
C16 0.0328(9) 0.0303(9) 0.0169(8) 0.0069(7) -0.0016(7) 0.0012(7)
C17 0.0108(6) 0.0144(6) 0.0075(6) -0.0002(5) 0.0018(4) 0.0016(5)
C18 0.0125(6) 0.0154(7) 0.0147(6) 0.0018(5) 0.0039(5) -0.0007(5)
C19 0.0154(6) 0.0111(6) 0.0099(6) 0.0009(5) 0.0036(5) -0.0005(5)
C20 0.0099(6) 0.0160(7) 0.0139(6) 0.0023(5) 0.0027(5) 0.0037(5)
C21 0.0194(7) 0.0273(9) 0.0238(8) 0.0054(7) 0.0106(6) 0.0111(6)
C22 0.0164(7) 0.0241(8) 0.0214(8) 0.0036(6) -0.0049(6) 0.0003(6)
C23 0.0153(6) 0.0144(7) 0.0147(7) 0.0000(5) 0.0033(5) 0.0045(5)
C24 0.0229(7) 0.0212(8) 0.0215(8) 0.0110(6) 0.0062(6) 0.0101(6)
C25 0.0218(8) 0.0168(8) 0.0367(10) -0.0071(7) 0.0014(7) -0.0040(6)
C26 0.0423(10) 0.0346(10) 0.0212(8) -0.0028(8) 0.0098(7) -0.0025(8)
C27 0.0214(8) 0.0200(8) 0.0401(10) -0.0047(7) 0.0036(7) 0.0042(6)
C28 0.0169(7) 0.0204(8) 0.0349(9) -0.0093(7) 0.0095(6) -0.0030(6)
C29 0.0239(8) 0.0223(9) 0.0513(12) 0.0006(8) 0.0205(8) -0.0042(7)
C30 0.0269(9) 0.0291(10) 0.0354(10) -0.0040(8) -0.0085(7) 0.0093(7)
B 0.0102(6) 0.0089(7) 0.0087(6) 0.0014(5) 0.0005(5) 0.0011(5)
N1 0.0105(5) 0.0082(5) 0.0096(5) 0.0019(4) 0.0014(4) 0.0015(4)
N2 0.0109(5) 0.0089(5) 0.0088(5) 0.0025(4) 0.0007(4) 0.0006(4)
N3 0.0113(5) 0.0093(5) 0.0117(5) 0.0012(4) 0.0003(4) 0.0014(4)
N4 0.0142(5) 0.0103(6) 0.0127(5) 0.0019(4) 0.0002(4) 0.0000(4)
N5 0.0115(5) 0.0087(5) 0.0081(5) 0.0007(4) 0.0010(4) 0.0009(4)
N6 0.0106(5) 0.0094(5) 0.0096(5) 0.0014(4) 0.0018(4) 0.0031(4)
N7 0.0111(5) 0.0118(6) 0.0161(6) -0.0019(5) 0.0018(4) -0.0015(4)
O1 0.0251(5) 0.0130(5) 0.0150(5) 0.0050(4) 0.0063(4) 0.0010(4)
O2 0.0203(5) 0.0254(6) 0.0147(5) 0.0074(4) 0.0034(4) 0.0051(5)
O3 0.0146(5) 0.0143(5) 0.0189(5) 0.0075(4) 0.0059(4) 0.0059(4)
Si1 0.00962(17) 0.01314(19) 0.0216(2) -0.00239(16) 0.00214(14) -0.00184(14)
Si2 0.01575(18) 0.0125(2) 0.0178(2) -0.00299(15) 0.00274(15) -0.00153(15)
Ca 0.00903(12) 0.00778(12) 0.01246(13) 0.00074(10) 0.00265(9) 0.00023(9)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.3387(17) . ?
C1 C2 1.399(2) . ?
C1 C4 1.5141(19) . ?
C2 C3 1.384(2) . ?
C2 H2 0.95 . ?
C3 N1 1.3429(17) . ?
C3 H3 0.95 . ?
C4 C7 1.528(2) . ?
C4 C6 1.532(2) . ?
C4 C5 1.543(2) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 O1 1.4394(19) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 O1 1.4361(19) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 N4 1.3345(17) . ?
C9 C10 1.409(2) . ?
C9 C12 1.509(2) . ?
C10 C11 1.375(2) . ?
C10 H10 0.95 . ?
C11 N3 1.3524(17) . ?
C11 H11 0.95 . ?
C12 C15 1.526(2) . ?
C12 C13 1.532(2) . ?
C12 C14 1.538(2) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 O2 1.4172(19) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 O2 1.4199(19) . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 N6 1.3403(17) . ?
C17 C18 1.399(2) . ?
C17 C20 1.5123(19) . ?
C18 C19 1.382(2) . ?
C18 H18 0.95 . ?
C19 N5 1.3437(18) . ?
C19 H19 0.95 . ?
C20 C23 1.523(2) . ?
C20 C21 1.537(2) . ?
C20 C22 1.538(2) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 O3 1.4462(17) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 O3 1.4391(18) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 Si2 1.8821(17) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 Si2 1.8817(19) . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 Si2 1.8829(17) . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C28 Si1 1.8759(17) . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 Si1 1.8708(18) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 Si1 1.8872(19) . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
B N3 1.5131(18) . ?
B N5 1.5448(18) . ?
B N1 1.5514(18) . ?
B Ca 3.1871(15) . ?
B H1B 1 . ?
N1 N2 1.3709(15) . ?
N2 Ca 2.4548(12) . ?
N3 N4 1.3692(17) . ?
N5 N6 1.3660(16) . ?
N6 Ca 2.4614(12) . ?
N7 Si2 1.6944(13) . ?
N7 Si1 1.6967(12) . ?
N7 Ca 2.3097(12) . ?
O1 Ca 2.3703(11) . ?
O3 Ca 2.3757(10) . ?
Si1 Ca 3.3624(5) . ?
Si2 Ca 3.5017(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
N2 C1 C2 110.47(12) . . ?
N2 C1 C4 121.68(12) . . ?
C2 C1 C4 127.85(13) . . ?
C3 C2 C1 104.80(12) . . ?
C3 C2 H2 127.6 . . ?
C1 C2 H2 127.6 . . ?
N1 C3 C2 108.47(12) . . ?
N1 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
C1 C4 C7 111.35(12) . . ?
C1 C4 C6 109.54(12) . . ?
C7 C4 C6 111.47(13) . . ?
C1 C4 C5 109.10(13) . . ?
C7 C4 C5 106.31(13) . . ?
C6 C4 C5 108.98(13) . . ?
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 . . ?
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 . . ?
O1 C7 C4 113.93(12) . . ?
O1 C7 H7A 108.8 . . ?
C4 C7 H7A 108.8 . . ?
O1 C7 H7B 108.8 . . ?
C4 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 110.85(13) . . ?
N4 C9 C12 119.61(12) . . ?
C10 C9 C12 129.29(13) . . ?
C11 C10 C9 104.76(12) . . ?
C11 C10 H10 127.6 . . ?
C9 C10 H10 127.6 . . ?
N3 C11 C10 108.15(13) . . ?
N3 C11 H11 125.9 . . ?
C10 C11 H11 125.9 . . ?
C9 C12 C15 110.93(12) . . ?
C9 C12 C13 110.53(12) . . ?
C15 C12 C13 110.50(12) . . ?
C9 C12 C14 108.35(12) . . ?
C15 C12 C14 106.83(12) . . ?
C13 C12 C14 109.60(13) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 C12 110.61(12) . . ?
O2 C15 H15A 109.5 . . ?
C12 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 C18 110.38(12) . . ?
N6 C17 C20 121.22(12) . . ?
C18 C17 C20 128.40(12) . . ?
C19 C18 C17 104.76(12) . . ?
C19 C18 H18 127.6 . . ?
C17 C18 H18 127.6 . . ?
N5 C19 C18 108.50(13) . . ?
N5 C19 H19 125.7 . . ?
C18 C19 H19 125.7 . . ?
C17 C20 C23 111.38(11) . . ?
C17 C20 C21 109.38(12) . . ?
C23 C20 C21 106.91(13) . . ?
C17 C20 C22 109.33(12) . . ?
C23 C20 C22 110.37(12) . . ?
C21 C20 C22 109.43(12) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C20 113.14(12) . . ?
O3 C23 H23A 109 . . ?
C20 C23 H23A 109 . . ?
O3 C23 H23B 109 . . ?
C20 C23 H23B 109 . . ?
H23A C23 H23B 107.8 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 B N5 112.48(11) . . ?
N3 B N1 109.72(11) . . ?
N5 B N1 108.11(10) . . ?
N3 B Ca 164.24(9) . . ?
N5 B Ca 77.99(7) . . ?
N1 B Ca 76.28(7) . . ?
N3 B H1B 108.8 . . ?
N5 B H1B 108.8 . . ?
N1 B H1B 108.8 . . ?
Ca B H1B 55.6 . . ?
C3 N1 N2 109.96(11) . . ?
C3 N1 B 131.23(11) . . ?
N2 N1 B 118.12(11) . . ?
C1 N2 N1 106.29(11) . . ?
C1 N2 Ca 131.58(9) . . ?
N1 N2 Ca 110.11(8) . . ?
C11 N3 N4 110.46(11) . . ?
C11 N3 B 128.16(12) . . ?
N4 N3 B 121.35(11) . . ?
C9 N4 N3 105.78(11) . . ?
C19 N5 N6 109.97(11) . . ?
C19 N5 B 131.25(12) . . ?
N6 N5 B 117.71(11) . . ?
C17 N6 N5 106.39(11) . . ?
C17 N6 Ca 134.38(9) . . ?
N5 N6 Ca 112.47(8) . . ?
Si2 N7 Si1 122.19(7) . . ?
Si2 N7 Ca 121.21(6) . . ?
Si1 N7 Ca 113.23(6) . . ?
C8 O1 C7 115.12(13) . . ?
C8 O1 Ca 126.35(11) . . ?
C7 O1 Ca 118.01(8) . . ?
C15 O2 C16 111.13(12) . . ?
C24 O3 C23 113.15(11) . . ?
C24 O3 Ca 123.51(9) . . ?
C23 O3 Ca 122.52(8) . . ?
N7 Si1 C29 114.91(8) . . ?
N7 Si1 C28 111.49(7) . . ?
C29 Si1 C28 103.49(9) . . ?
N7 Si1 C30 113.60(8) . . ?
C29 Si1 C30 107.01(10) . . ?
C28 Si1 C30 105.43(9) . . ?
C29 Si1 Ca 132.47(7) . . ?
C28 Si1 Ca 72.91(5) . . ?
C30 Si1 Ca 119.79(7) . . ?
N7 Si2 C26 111.43(8) . . ?
N7 Si2 C25 115.41(7) . . ?
C26 Si2 C25 106.62(9) . . ?
N7 Si2 C27 112.07(7) . . ?
C26 Si2 C27 104.77(9) . . ?
C25 Si2 C27 105.79(8) . . ?
C26 Si2 Ca 94.86(6) . . ?
C25 Si2 Ca 149.27(6) . . ?
C27 Si2 Ca 89.11(6) . . ?
N7 Ca O1 103.72(4) . . ?
N7 Ca O3 109.73(4) . . ?
O1 Ca O3 88.89(4) . . ?
N7 Ca N2 129.09(4) . . ?
O1 Ca N2 73.34(4) . . ?
O3 Ca N2 120.86(4) . . ?
N7 Ca N6 126.74(4) . . ?
O1 Ca N6 129.43(4) . . ?
O3 Ca N6 72.73(4) . . ?
N2 Ca N6 76.84(4) . . ?
N7 Ca B 105.78(4) . . ?
O1 Ca B 123.65(4) . . ?
O3 Ca B 123.10(4) . . ?
N2 Ca B 50.78(4) . . ?
N6 Ca B 50.40(4) . . ?
N7 Ca Si1 27.63(3) . . ?
O1 Ca Si1 95.76(3) . . ?
O3 Ca Si1 136.76(3) . . ?
N2 Ca Si1 101.50(3) . . ?
N6 Ca Si1 129.94(3) . . ?
B Ca Si1 89.34(3) . . ?
N7 Ca Si2 24.45(3) . . ?
O1 Ca Si2 116.30(3) . . ?
O3 Ca Si2 88.39(3) . . ?
N2 Ca Si2 150.18(3) . . ?
N6 Ca Si2 109.95(3) . . ?
B Ca Si2 110.18(3) . . ?
Si1 Ca Si2 51.203(11) . . ?

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
N2 C1 C2 C3 -0.48(16) . . . . ?
C4 C1 C2 C3 -179.82(13) . . . . ?
C1 C2 C3 N1 -0.28(15) . . . . ?
N2 C1 C4 C7 -1.79(18) . . . . ?
C2 C1 C4 C7 177.49(13) . . . . ?
N2 C1 C4 C6 -125.54(14) . . . . ?
C2 C1 C4 C6 53.74(19) . . . . ?
N2 C1 C4 C5 115.24(15) . . . . ?
C2 C1 C4 C5 -65.48(19) . . . . ?
C1 C4 C7 O1 -61.56(16) . . . . ?
C6 C4 C7 O1 61.09(16) . . . . ?
C5 C4 C7 O1 179.72(12) . . . . ?
N4 C9 C10 C11 0.70(16) . . . . ?
C12 C9 C10 C11 -173.45(14) . . . . ?
C9 C10 C11 N3 -0.58(16) . . . . ?
N4 C9 C12 C15 161.19(13) . . . . ?
C10 C9 C12 C15 -25.1(2) . . . . ?
N4 C9 C12 C13 38.26(18) . . . . ?
C10 C9 C12 C13 -148.03(15) . . . . ?
N4 C9 C12 C14 -81.84(16) . . . . ?
C10 C9 C12 C14 91.87(18) . . . . ?
C9 C12 C15 O2 -63.22(16) . . . . ?
C13 C12 C15 O2 59.73(17) . . . . ?
C14 C12 C15 O2 178.89(12) . . . . ?
N6 C17 C18 C19 0.22(16) . . . . ?
C20 C17 C18 C19 -179.45(13) . . . . ?
C17 C18 C19 N5 -0.23(16) . . . . ?
N6 C17 C20 C23 15.07(18) . . . . ?
C18 C17 C20 C23 -165.29(14) . . . . ?
N6 C17 C20 C21 133.03(14) . . . . ?
C18 C17 C20 C21 -47.3(2) . . . . ?
N6 C17 C20 C22 -107.17(15) . . . . ?
C18 C17 C20 C22 72.47(18) . . . . ?
C17 C20 C23 O3 -68.32(15) . . . . ?
C21 C20 C23 O3 172.24(11) . . . . ?
C22 C20 C23 O3 53.31(15) . . . . ?
C2 C3 N1 N2 0.92(15) . . . . ?
C2 C3 N1 B 170.95(13) . . . . ?
N3 B N1 C3 13.90(19) . . . . ?
N5 B N1 C3 136.90(14) . . . . ?
Ca B N1 C3 -150.87(14) . . . . ?
N3 B N1 N2 -176.73(11) . . . . ?
N5 B N1 N2 -53.73(15) . . . . ?
Ca B N1 N2 18.50(10) . . . . ?
C2 C1 N2 N1 1.02(15) . . . . ?
C4 C1 N2 N1 -179.59(12) . . . . ?
C2 C1 N2 Ca -136.55(11) . . . . ?
C4 C1 N2 Ca 42.84(18) . . . . ?
C3 N1 N2 C1 -1.20(15) . . . . ?
B N1 N2 C1 -172.71(11) . . . . ?
C3 N1 N2 Ca 146.29(9) . . . . ?
B N1 N2 Ca -25.22(13) . . . . ?
C10 C11 N3 N4 0.29(16) . . . . ?
C10 C11 N3 B 178.20(13) . . . . ?
N5 B N3 C11 116.22(15) . . . . ?
N1 B N3 C11 -123.40(14) . . . . ?
Ca B N3 C11 -13.4(4) . . . . ?
N5 B N3 N4 -66.07(16) . . . . ?
N1 B N3 N4 54.31(16) . . . . ?
Ca B N3 N4 164.3(3) . . . . ?
C10 C9 N4 N3 -0.53(16) . . . . ?
C12 C9 N4 N3 174.26(12) . . . . ?
C11 N3 N4 C9 0.15(15) . . . . ?
B N3 N4 C9 -177.93(12) . . . . ?
C18 C19 N5 N6 0.17(16) . . . . ?
C18 C19 N5 B 167.79(13) . . . . ?
N3 B N5 C19 35.65(19) . . . . ?
N1 B N5 C19 -85.66(16) . . . . ?
Ca B N5 C19 -156.71(14) . . . . ?
N3 B N5 N6 -157.51(11) . . . . ?
N1 B N5 N6 81.18(14) . . . . ?
Ca B N5 N6 10.13(10) . . . . ?
C18 C17 N6 N5 -0.12(15) . . . . ?
C20 C17 N6 N5 179.58(12) . . . . ?
C18 C17 N6 Ca -147.82(11) . . . . ?
C20 C17 N6 Ca 31.88(19) . . . . ?
C19 N5 N6 C17 -0.03(14) . . . . ?
B N5 N6 C17 -169.54(11) . . . . ?
C19 N5 N6 Ca 155.56(9) . . . . ?
B N5 N6 Ca -13.95(13) . . . . ?
C4 C7 O1 C8 -104.29(15) . . . . ?
C4 C7 O1 Ca 83.44(13) . . . . ?
C12 C15 O2 C16 175.35(13) . . . . ?
C20 C23 O3 C24 -113.63(14) . . . . ?
C20 C23 O3 Ca 76.44(13) . . . . ?
Si2 N7 Si1 C29 73.01(12) . . . . ?
Ca N7 Si1 C29 -127.50(9) . . . . ?
Si2 N7 Si1 C28 -169.65(9) . . . . ?
Ca N7 Si1 C28 -10.16(10) . . . . ?
Si2 N7 Si1 C30 -50.70(12) . . . . ?
Ca N7 Si1 C30 108.79(9) . . . . ?
Si2 N7 Si1 Ca -159.49(13) . . . . ?
Si1 N7 Si2 C26 92.29(11) . . . . ?
Ca N7 Si2 C26 -65.60(10) . . . . ?
Si1 N7 Si2 C25 -29.49(12) . . . . ?
Ca N7 Si2 C25 172.62(8) . . . . ?
Si1 N7 Si2 C27 -150.66(9) . . . . ?
Ca N7 Si2 C27 51.45(10) . . . . ?
Si1 N7 Si2 Ca 157.89(14) . . . . ?
Si2 N7 Ca O1 -124.39(7) . . . . ?
Si1 N7 Ca O1 75.89(7) . . . . ?
Si2 N7 Ca O3 -30.59(9) . . . . ?
Si1 N7 Ca O3 169.69(6) . . . . ?
Si2 N7 Ca N2 156.08(6) . . . . ?
Si1 N7 Ca N2 -3.64(9) . . . . ?
Si2 N7 Ca N6 52.17(9) . . . . ?
Si1 N7 Ca N6 -107.55(7) . . . . ?
Si2 N7 Ca B 104.17(7) . . . . ?
Si1 N7 Ca B -55.55(7) . . . . ?
Si2 N7 Ca Si1 159.72(13) . . . . ?
Si1 N7 Ca Si2 -159.72(13) . . . . ?
C8 O1 Ca N7 25.90(13) . . . . ?
C7 O1 Ca N7 -162.79(10) . . . . ?
C8 O1 Ca O3 -84.14(13) . . . . ?
C7 O1 Ca O3 87.17(10) . . . . ?
C8 O1 Ca N2 153.09(13) . . . . ?
C7 O1 Ca N2 -35.60(9) . . . . ?
C8 O1 Ca N6 -150.54(12) . . . . ?
C7 O1 Ca N6 20.78(12) . . . . ?
C8 O1 Ca B 145.82(12) . . . . ?
C7 O1 Ca B -42.87(11) . . . . ?
C8 O1 Ca Si1 52.77(13) . . . . ?
C7 O1 Ca Si1 -135.92(9) . . . . ?
C8 O1 Ca Si2 3.51(13) . . . . ?
C7 O1 Ca Si2 174.82(9) . . . . ?
C24 O3 Ca N7 -73.22(12) . . . . ?
C23 O3 Ca N7 95.67(10) . . . . ?
C24 O3 Ca O1 30.97(12) . . . . ?
C23 O3 Ca O1 -160.15(10) . . . . ?
C24 O3 Ca N2 100.75(12) . . . . ?
C23 O3 Ca N2 -90.36(11) . . . . ?
C24 O3 Ca N6 163.14(12) . . . . ?
C23 O3 Ca N6 -27.97(10) . . . . ?
C24 O3 Ca B 161.43(11) . . . . ?
C23 O3 Ca B -29.68(12) . . . . ?
C24 O3 Ca Si1 -66.26(12) . . . . ?
C23 O3 Ca Si1 102.62(10) . . . . ?
C24 O3 Ca Si2 -85.38(11) . . . . ?
C23 O3 Ca Si2 83.50(10) . . . . ?
C1 N2 Ca N7 72.23(13) . . . . ?
N1 N2 Ca N7 -64.18(10) . . . . ?
C1 N2 Ca O1 -22.13(11) . . . . ?
N1 N2 Ca O1 -158.53(9) . . . . ?
C1 N2 Ca O3 -100.46(12) . . . . ?
N1 N2 Ca O3 123.14(8) . . . . ?
C1 N2 Ca N6 -160.79(12) . . . . ?
N1 N2 Ca N6 62.80(8) . . . . ?
C1 N2 Ca B 150.06(13) . . . . ?
N1 N2 Ca B 13.66(7) . . . . ?
C1 N2 Ca Si1 70.50(12) . . . . ?
N1 N2 Ca Si1 -65.90(8) . . . . ?
C1 N2 Ca Si2 91.95(12) . . . . ?
N1 N2 Ca Si2 -44.45(11) . . . . ?
C17 N6 Ca N7 -126.19(13) . . . . ?
N5 N6 Ca N7 87.51(9) . . . . ?
C17 N6 Ca O1 49.49(14) . . . . ?
N5 N6 Ca O1 -96.81(9) . . . . ?
C17 N6 Ca O3 -24.12(13) . . . . ?
N5 N6 Ca O3 -170.43(9) . . . . ?
C17 N6 Ca N2 104.50(13) . . . . ?
N5 N6 Ca N2 -41.80(8) . . . . ?
C17 N6 Ca B 154.02(15) . . . . ?
N5 N6 Ca B 7.72(7) . . . . ?
C17 N6 Ca Si1 -161.40(11) . . . . ?
N5 N6 Ca Si1 52.30(10) . . . . ?
C17 N6 Ca Si2 -105.84(13) . . . . ?
N5 N6 Ca Si2 107.86(8) . . . . ?
N3 B Ca N7 1.9(4) . . . . ?
N5 B Ca N7 -131.40(7) . . . . ?
N1 B Ca N7 116.32(7) . . . . ?
N3 B Ca O1 -117.1(3) . . . . ?
N5 B Ca O1 109.64(7) . . . . ?
N1 B Ca O1 -2.64(9) . . . . ?
N3 B Ca O3 129.0(3) . . . . ?
N5 B Ca O3 -4.32(9) . . . . ?
N1 B Ca O3 -116.60(7) . . . . ?
N3 B Ca N2 -126.1(4) . . . . ?
N5 B Ca N2 100.64(8) . . . . ?
N1 B Ca N2 -11.64(6) . . . . ?
N3 B Ca N6 126.8(4) . . . . ?
N5 B Ca N6 -6.44(6) . . . . ?
N1 B Ca N6 -118.72(8) . . . . ?
N3 B Ca Si1 -20.6(3) . . . . ?
N5 B Ca Si1 -153.88(7) . . . . ?
N1 B Ca Si1 93.84(7) . . . . ?
N3 B Ca Si2 27.2(4) . . . . ?
N5 B Ca Si2 -106.09(7) . . . . ?
N1 B Ca Si2 141.63(6) . . . . ?
C29 Si1 Ca N7 77.29(11) . . . . ?
C28 Si1 Ca N7 170.11(10) . . . . ?
C30 Si1 Ca N7 -91.57(10) . . . . ?
N7 Si1 Ca O1 -108.75(7) . . . . ?
C29 Si1 Ca O1 -31.46(9) . . . . ?
C28 Si1 Ca O1 61.36(7) . . . . ?
C30 Si1 Ca O1 159.68(8) . . . . ?
N7 Si1 Ca O3 -14.24(8) . . . . ?
C29 Si1 Ca O3 63.05(10) . . . . ?
C28 Si1 Ca O3 155.88(7) . . . . ?
C30 Si1 Ca O3 -105.81(8) . . . . ?
N7 Si1 Ca N2 177.12(7) . . . . ?
C29 Si1 Ca N2 -105.59(9) . . . . ?
C28 Si1 Ca N2 -12.77(7) . . . . ?
C30 Si1 Ca N2 85.55(8) . . . . ?
N7 Si1 Ca N6 94.74(8) . . . . ?
C29 Si1 Ca N6 172.03(9) . . . . ?
C28 Si1 Ca N6 -95.15(7) . . . . ?
C30 Si1 Ca N6 3.16(8) . . . . ?
N7 Si1 Ca B 127.48(7) . . . . ?
C29 Si1 Ca B -155.23(9) . . . . ?
C28 Si1 Ca B -62.41(7) . . . . ?
C30 Si1 Ca B 35.91(8) . . . . ?
N7 Si1 Ca Si2 10.61(7) . . . . ?
C29 Si1 Ca Si2 87.89(9) . . . . ?
C28 Si1 Ca Si2 -179.28(6) . . . . ?
C30 Si1 Ca Si2 -80.97(7) . . . . ?
C26 Si2 Ca N7 121.70(10) . . . . ?
C25 Si2 Ca N7 -13.13(14) . . . . ?
C27 Si2 Ca N7 -133.55(10) . . . . ?
N7 Si2 Ca O1 63.40(8) . . . . ?
C26 Si2 Ca O1 -174.89(7) . . . . ?
C25 Si2 Ca O1 50.28(12) . . . . ?
C27 Si2 Ca O1 -70.14(7) . . . . ?
N7 Si2 Ca O3 151.37(8) . . . . ?
C26 Si2 Ca O3 -86.93(7) . . . . ?
C25 Si2 Ca O3 138.24(12) . . . . ?
C27 Si2 Ca O3 17.82(7) . . . . ?
N7 Si2 Ca N2 -39.27(10) . . . . ?
C26 Si2 Ca N2 82.44(9) . . . . ?
C25 Si2 Ca N2 -52.39(13) . . . . ?
C27 Si2 Ca N2 -172.81(8) . . . . ?
N7 Si2 Ca N6 -137.67(8) . . . . ?
C26 Si2 Ca N6 -15.97(7) . . . . ?
C25 Si2 Ca N6 -150.80(12) . . . . ?
C27 Si2 Ca N6 88.78(7) . . . . ?
N7 Si2 Ca B -83.76(8) . . . . ?
C26 Si2 Ca B 37.94(7) . . . . ?
C25 Si2 Ca B -96.89(12) . . . . ?
C27 Si2 Ca B 142.69(7) . . . . ?
N7 Si2 Ca Si1 -11.90(8) . . . . ?
C26 Si2 Ca Si1 109.80(7) . . . . ?
C25 Si2 Ca Si1 -25.03(12) . . . . ?
C27 Si2 Ca Si1 -145.45(6) . . . . ?

#===END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-09-29 at 17:44:51
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : shelxl dreduc import struct

data_Chisholm1547
_database_code_depnum_ccdc_archive 'CCDC 705807'

_audit_creation_date             2008-09-29T17:44:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Chisholm 1547'
_chemical_formula_moiety         'C31 H47 B1 Ca1 N6 O4, C7 H8'
_chemical_formula_sum            'C38 H55 B Ca N6 O4'
_chemical_formula_weight         710.77
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
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                   13.390(1)
_cell_length_b                   15.831(1)
_cell_length_c                   19.583(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.058(3)
_cell_angle_gamma                90
_cell_volume                     3923.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7185
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_special_details           
;All work was done at 150 K using an Oxford Cryosystems Cryostream
Cooler. The data collection strategy was set up to measure
a quadrant of reciprocal space with a redundancy factor
of 4.3, which means that 90% of the reflections were measured at least
4.3 times. A combination of phi and omega scans with a frame width
of 1.0\% was used. Data integration was done with Denzo, and
scaling and merging of the data was done with Scalepack.

The asymmetric unit consists of the Ca complex and one
molecule of toluene.
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.379508E-1
_diffrn_orient_matrix_ub_12      -0.248376E-1
_diffrn_orient_matrix_ub_13      0.315622E-1
_diffrn_orient_matrix_ub_21      0.689178E-1
_diffrn_orient_matrix_ub_22      -0.194571E-1
_diffrn_orient_matrix_ub_23      0.347848E-1
_diffrn_orient_matrix_ub_31      0.72793E-2
_diffrn_orient_matrix_ub_32      0.547216E-1
_diffrn_orient_matrix_ub_33      0.266941E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_number            63707
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             6918
_reflns_number_gt                5512
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
; Two of the three C-C-O-C chains of the Tp* ligand are disordered. Each
of these disordered chains is modeled with two orientations. Atoms C(5),
C(6) and C(7) comprise one orientation and C(5A), C(6A) and C(7A) make up
the second orientation for one chain. Atom C(8), located at the end of this
chain, is common to both orientations. The second disordered chain is
similarly modeled with C(13), C(14), C(15) and C(16) in one orientation and
C(13A), C(14A), C(15A) and C(16A) in the other. In this case, the
terminal carbon atom of this chain is disordered over two sites: C(16)
and C(16A) and both of these atoms are refined isotropically. SADI
restraints were used in the refinement of these disordered regions.

For the methyl groups, the hydrogen atoms were added at calculated
positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom).
The torsion angle, which defines the orientation of the methyl group
about the C-C OR O-C bond, was refined. In one instance, for the methyl
group bonded to the O-tolyl ligand, this torsion angle was not refined.
The other hydrogen atoms were included in the model
at calculated positions using a riding model with
U(H) = 1.2 * Ueq(attached atom).

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     
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+2.0633P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6918
_refine_ls_number_parameters     521
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1025
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.042

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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
C1 C 0.04095(15) 0.32837(13) 0.11988(10) 0.0278(4) Uani 1 1 d . A .
C2 C 0.03502(16) 0.39908(13) 0.07563(11) 0.0338(5) Uani 1 1 d . . .
H2 H -0.0249 0.4337 0.0539 0.041 Uiso 1 1 calc R . .
C3 C 0.13385(16) 0.40756(12) 0.07045(10) 0.0300(5) Uani 1 1 d . . .
H3 H 0.1553 0.4501 0.0439 0.036 Uiso 1 1 calc R . .
C4 C -0.04699(15) 0.28813(13) 0.14161(10) 0.0320(5) Uani 1 1 d D . .
C5 C -0.0202(3) 0.3034(2) 0.22398(17) 0.0345(10) Uani 0.573(3) 1 d PD A 1
H1C5 H -0.0754 0.2783 0.2403 0.052 Uiso 0.573(3) 1 calc PR A 1
H2C5 H -0.0163 0.3642 0.2337 0.052 Uiso 0.573(3) 1 calc PR A 1
H3C5 H 0.048 0.2772 0.25 0.052 Uiso 0.573(3) 1 calc PR A 1
C6 C -0.1490(3) 0.3354(3) 0.1011(2) 0.0440(12) Uani 0.573(3) 1 d PD A 1
H1C6 H -0.1648 0.3279 0.049 0.066 Uiso 0.573(3) 1 calc PR A 1
H2C6 H -0.14 0.3957 0.113 0.066 Uiso 0.573(3) 1 calc PR A 1
H3C6 H -0.2073 0.3129 0.1155 0.066 Uiso 0.573(3) 1 calc PR A 1
C7 C -0.0554(3) 0.1986(2) 0.12115(18) 0.0311(9) Uani 0.573(3) 1 d PD A 1
H1C7 H -0.1226 0.1763 0.1246 0.037 Uiso 0.573(3) 1 calc PR A 1
H2C7 H -0.0589 0.1943 0.07 0.037 Uiso 0.573(3) 1 calc PR A 1
C5A C -0.1015(4) 0.3515(3) 0.1773(3) 0.0453(16) Uani 0.427(3) 1 d PD A 2
H4C5 H -0.1577 0.3228 0.1902 0.068 Uiso 0.427(3) 1 calc PR A 2
H5C5 H -0.1321 0.3975 0.1435 0.068 Uiso 0.427(3) 1 calc PR A 2
H6C5 H -0.0496 0.3746 0.221 0.068 Uiso 0.427(3) 1 calc PR A 2
C6A C -0.1357(4) 0.2507(3) 0.0736(2) 0.0388(14) Uani 0.427(3) 1 d PD A 2
H4C6 H -0.1055 0.2057 0.052 0.058 Uiso 0.427(3) 1 calc PR A 2
H5C6 H -0.1634 0.2956 0.0379 0.058 Uiso 0.427(3) 1 calc PR A 2
H6C6 H -0.1931 0.2276 0.0887 0.058 Uiso 0.427(3) 1 calc PR A 2
C7A C -0.0155(3) 0.2132(3) 0.1941(2) 0.0306(12) Uani 0.427(3) 1 d PD A 2
H3C7 H 0.0361 0.2324 0.2403 0.037 Uiso 0.427(3) 1 calc PR A 2
H4C7 H -0.0788 0.1919 0.2043 0.037 Uiso 0.427(3) 1 calc PR A 2
C8 C 0.00250(19) 0.07305(17) 0.19737(14) 0.0518(7) Uani 1 1 d . A .
H1C8 H -0.0264 0.0912 0.2349 0.078 Uiso 0.573(3) 1 calc PR A 1
H2C8 H 0.0653 0.0381 0.2191 0.078 Uiso 0.573(3) 1 calc PR A 1
H3C8 H -0.0507 0.0401 0.1608 0.078 Uiso 0.573(3) 1 calc PR A 1
H4C8 H 0.041 0.0236 0.1889 0.078 Uiso 0.427(3) 1 calc PR A 2
H5C8 H -0.0737 0.0631 0.1764 0.078 Uiso 0.427(3) 1 calc PR A 2
H6C8 H 0.0208 0.0827 0.2495 0.078 Uiso 0.427(3) 1 calc PR A 2
C9 C 0.28259(15) 0.10532(12) 0.04919(10) 0.0251(4) Uani 1 1 d . A .
C10 C 0.33540(16) 0.13792(13) 0.00418(11) 0.0310(5) Uani 1 1 d . . .
H10 H 0.3558 0.1084 -0.0314 0.037 Uiso 1 1 calc R . .
C11 C 0.35161(15) 0.22161(13) 0.02231(10) 0.0270(4) Uani 1 1 d . . .
H11 H 0.3854 0.2613 0.0008 0.032 Uiso 1 1 calc R . .
C12 C 0.23793(15) 0.01720(12) 0.04793(10) 0.0305(5) Uani 1 1 d D . .
C13 C 0.3263(3) -0.04585(19) 0.06566(19) 0.0409(9) Uani 0.672(3) 1 d PD B 3
H13A H 0.2971 -0.1031 0.0621 0.061 Uiso 0.672(3) 1 calc PR B 3
H13B H 0.3739 -0.036 0.1149 0.061 Uiso 0.672(3) 1 calc PR B 3
H13C H 0.3655 -0.0397 0.0316 0.061 Uiso 0.672(3) 1 calc PR B 3
C14 C 0.1638(3) 0.0031(2) -0.03113(16) 0.0410(9) Uani 0.672(3) 1 d PD B 3
H14A H 0.205 0.0073 -0.0642 0.062 Uiso 0.672(3) 1 calc PR B 3
H14B H 0.1082 0.0462 -0.0436 0.062 Uiso 0.672(3) 1 calc PR B 3
H14C H 0.1317 -0.0531 -0.0353 0.062 Uiso 0.672(3) 1 calc PR B 3
C15 C 0.1676(2) 0.01278(19) 0.09478(14) 0.0308(8) Uani 0.672(3) 1 d PD A 3
H15A H 0.1144 0.0586 0.0808 0.037 Uiso 0.672(3) 1 calc PR B 3
H15B H 0.1295 -0.0418 0.0866 0.037 Uiso 0.672(3) 1 calc PR B 3
C16 C 0.2385(3) -0.0528(2) 0.2135(2) 0.0421(11) Uiso 0.672(3) 1 d PD A 3
H16A H 0.2767 -0.0406 0.2645 0.063 Uiso 0.672(3) 1 calc PR B 3
H16B H 0.277 -0.0957 0.196 0.063 Uiso 0.672(3) 1 calc PR B 3
H16C H 0.1677 -0.0738 0.2086 0.063 Uiso 0.672(3) 1 calc PR B 3
C13A C 0.2764(6) -0.0471(4) 0.0026(3) 0.0382(18) Uani 0.328(3) 1 d PD B 4
H13D H 0.3538 -0.0488 0.0199 0.057 Uiso 0.328(3) 1 calc PR B 4
H13E H 0.2512 -0.03 -0.0482 0.057 Uiso 0.328(3) 1 calc PR B 4
H13F H 0.2487 -0.1032 0.0075 0.057 Uiso 0.328(3) 1 calc PR B 4
C14A C 0.1182(4) 0.0148(4) 0.0249(3) 0.0345(17) Uani 0.328(3) 1 d PD B 4
H14D H 0.0885 0.0355 -0.0247 0.052 Uiso 0.328(3) 1 calc PR B 4
H14E H 0.094 0.0506 0.0572 0.052 Uiso 0.328(3) 1 calc PR B 4
H14F H 0.0948 -0.0435 0.0275 0.052 Uiso 0.328(3) 1 calc PR B 4
C15A C 0.2746(4) -0.0283(3) 0.1248(3) 0.0274(15) Uani 0.328(3) 1 d PD A 4
H15C H 0.2479 -0.0871 0.1202 0.033 Uiso 0.328(3) 1 calc PR B 4
H15D H 0.3526 -0.0297 0.1451 0.033 Uiso 0.328(3) 1 calc PR B 4
C16A C 0.2480(6) -0.0378(4) 0.2357(4) 0.0272(18) Uiso 0.328(3) 1 d PD A 4
H16D H 0.1948 -0.0828 0.2228 0.041 Uiso 0.328(3) 1 calc PR B 4
H16E H 0.242 -0.0064 0.2773 0.041 Uiso 0.328(3) 1 calc PR B 4
H16F H 0.3187 -0.0626 0.248 0.041 Uiso 0.328(3) 1 calc PR B 4
C17 C 0.46935(15) 0.27803(12) 0.29733(10) 0.0248(4) Uani 1 1 d . A .
C18 C 0.53160(15) 0.34233(12) 0.28300(11) 0.0291(5) Uani 1 1 d . . .
H18 H 0.5976 0.3626 0.3141 0.035 Uiso 1 1 calc R . .
C19 C 0.47722(15) 0.36985(12) 0.21470(10) 0.0273(4) Uani 1 1 d . . .
H19 H 0.4993 0.4132 0.1893 0.033 Uiso 1 1 calc R . .
C20 C 0.49473(17) 0.22679(13) 0.36643(11) 0.0328(5) Uani 1 1 d . . .
C21 C 0.6145(2) 0.2091(2) 0.39393(17) 0.0777(11) Uani 1 1 d . . .
H21A H 0.6346 0.1795 0.3564 0.117 Uiso 1 1 calc R . .
H21B H 0.6321 0.174 0.4375 0.117 Uiso 1 1 calc R . .
H21C H 0.6531 0.2627 0.4054 0.117 Uiso 1 1 calc R . .
C22 C 0.4665(3) 0.27845(17) 0.42341(14) 0.0875(12) Uani 1 1 d . . .
H22A H 0.5065 0.3315 0.432 0.131 Uiso 1 1 calc R . .
H22B H 0.4844 0.2462 0.4685 0.131 Uiso 1 1 calc R . .
H22C H 0.3907 0.2909 0.4063 0.131 Uiso 1 1 calc R . .
C23 C 0.43295(16) 0.14395(13) 0.35954(10) 0.0311(5) Uani 1 1 d . A .
H23A H 0.4784 0.103 0.3941 0.037 Uiso 1 1 calc R . .
H23B H 0.3709 0.1549 0.3751 0.037 Uiso 1 1 calc R . .
C24 C 0.4781(2) 0.07201(18) 0.26665(15) 0.0598(8) Uani 1 1 d . A .
H24A H 0.5189 0.1189 0.2565 0.09 Uiso 1 1 calc R . .
H24B H 0.4472 0.0387 0.2226 0.09 Uiso 1 1 calc R . .
H24C H 0.5247 0.036 0.3044 0.09 Uiso 1 1 calc R . .
C25 C 0.16324(14) 0.16072(13) 0.36778(10) 0.0276(4) Uani 1 1 d . A .
C26 C 0.12630(15) 0.22570(13) 0.40211(10) 0.0291(5) Uani 1 1 d . . .
H26 H 0.1199 0.2812 0.3828 0.035 Uiso 1 1 calc R . .
C27 C 0.09894(15) 0.21096(13) 0.46334(10) 0.0295(5) Uani 1 1 d . . .
H27 H 0.0749 0.2568 0.4851 0.035 Uiso 1 1 calc R . .
C28 C 0.10552(15) 0.13140(14) 0.49381(10) 0.0297(5) Uani 1 1 d . . .
C29 C 0.14050(18) 0.06683(14) 0.45985(12) 0.0381(5) Uani 1 1 d . . .
H29 H 0.1458 0.0114 0.4793 0.046 Uiso 1 1 calc R . .
C30 C 0.16802(17) 0.08021(14) 0.39879(11) 0.0364(5) Uani 1 1 d . . .
H30 H 0.1909 0.0337 0.3771 0.044 Uiso 1 1 calc R . .
C31 C 0.0790(2) 0.11548(17) 0.56191(12) 0.0476(6) Uani 1 1 d . . .
H31A H 0.0181 0.0775 0.5512 0.071 Uiso 1 1 calc R . .
H31B H 0.062 0.1692 0.5805 0.071 Uiso 1 1 calc R . .
H31C H 0.1398 0.0895 0.5983 0.071 Uiso 1 1 calc R . .
C32 C 0.7676(2) 0.1013(2) 0.26814(15) 0.0654(9) Uani 1 1 d . . .
C33 C 0.7085(2) 0.1607(2) 0.21929(17) 0.0696(9) Uani 1 1 d . . .
H33 H 0.7193 0.2191 0.2301 0.083 Uiso 1 1 calc R . .
C34 C 0.6344(3) 0.1357(3) 0.1553(2) 0.0900(12) Uani 1 1 d . . .
H34 H 0.5953 0.1773 0.1223 0.108 Uiso 1 1 calc R . .
C35 C 0.6166(3) 0.0525(4) 0.13875(19) 0.0960(13) Uani 1 1 d . . .
H35 H 0.5644 0.0357 0.095 0.115 Uiso 1 1 calc R . .
C36 C 0.6739(3) -0.0059(3) 0.1853(2) 0.0881(11) Uani 1 1 d . . .
H36 H 0.6622 -0.0641 0.1737 0.106 Uiso 1 1 calc R . .
C37 C 0.7480(3) 0.0168(2) 0.24856(18) 0.0729(9) Uani 1 1 d . . .
H37 H 0.7874 -0.0259 0.2801 0.087 Uiso 1 1 calc R . .
C38 C 0.8472(2) 0.1258(3) 0.33774(18) 0.1003(13) Uani 1 1 d . . .
H38A H 0.8268 0.1029 0.3777 0.15 Uiso 1 1 calc R . .
H38B H 0.8511 0.1876 0.3414 0.15 Uiso 1 1 calc R . .
H38C H 0.9164 0.1033 0.3401 0.15 Uiso 1 1 calc R . .
B B 0.30930(17) 0.32468(14) 0.11173(11) 0.0238(5) Uani 1 1 d . . .
H1B H 0.3325 0.3689 0.0836 0.029 Uiso 1 1 calc R . .
N1 N 0.19582(12) 0.34572(10) 0.10914(8) 0.0246(4) Uani 1 1 d . A .
N2 N 0.13913(12) 0.29612(10) 0.14060(8) 0.0255(4) Uani 1 1 d . . .
N3 N 0.31175(12) 0.23816(10) 0.07556(8) 0.0226(3) Uani 1 1 d . A .
N4 N 0.26920(12) 0.16596(10) 0.09326(8) 0.0246(4) Uani 1 1 d . . .
N5 N 0.38715(12) 0.32502(9) 0.18958(8) 0.0221(3) Uani 1 1 d . A .
N6 N 0.38103(12) 0.26789(9) 0.24053(8) 0.0229(3) Uani 1 1 d . . .
O1 O 0.03066(10) 0.14524(8) 0.16444(7) 0.0297(3) Uani 1 1 d D . .
O2 O 0.23010(11) 0.02111(9) 0.17282(7) 0.0343(3) Uani 1 1 d D . .
O3 O 0.39618(10) 0.10440(8) 0.29034(7) 0.0293(3) Uani 1 1 d . . .
O4 O 0.19086(11) 0.17417(10) 0.31042(7) 0.0384(4) Uani 1 1 d . . .
Ca Ca 0.22815(3) 0.16834(2) 0.210337(19) 0.02143(11) Uani 1 1 d . A .

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
C1 0.0249(10) 0.0335(11) 0.0222(10) -0.0017(8) 0.0038(8) 0.0065(9)
C2 0.0305(11) 0.0340(12) 0.0321(11) 0.0063(9) 0.0037(9) 0.0116(9)
C3 0.0363(12) 0.0266(11) 0.0245(10) 0.0057(8) 0.0063(9) 0.0060(9)
C4 0.0243(10) 0.0389(12) 0.0317(11) 0.0040(9) 0.0077(9) 0.0063(9)
C5 0.032(2) 0.041(2) 0.035(2) 0.0008(17) 0.0172(17) 0.0030(17)
C6 0.0192(18) 0.057(3) 0.054(3) 0.014(2) 0.0089(17) 0.0047(18)
C7 0.0221(18) 0.040(2) 0.028(2) 0.0031(16) 0.0037(15) -0.0064(15)
C5A 0.039(3) 0.038(3) 0.069(4) -0.003(3) 0.031(3) 0.006(2)
C6A 0.027(3) 0.041(3) 0.043(3) 0.010(2) 0.003(2) -0.001(2)
C7A 0.023(2) 0.039(3) 0.032(3) -0.001(2) 0.012(2) 0.000(2)
C8 0.0360(13) 0.0663(17) 0.0509(15) 0.0237(13) 0.0110(11) -0.0142(12)
C9 0.0256(10) 0.0275(10) 0.0202(10) -0.0037(8) 0.0047(8) 0.0002(8)
C10 0.0354(11) 0.0364(12) 0.0246(10) -0.0053(9) 0.0142(9) 0.0031(9)
C11 0.0273(10) 0.0346(12) 0.0215(10) 0.0029(8) 0.0113(8) 0.0014(9)
C12 0.0365(11) 0.0264(11) 0.0267(11) -0.0087(8) 0.0079(9) -0.0020(9)
C13 0.055(2) 0.0249(17) 0.041(2) 0.0008(14) 0.0143(17) 0.0058(15)
C14 0.055(2) 0.0326(18) 0.0288(18) -0.0061(14) 0.0040(15) -0.0112(16)
C15 0.0362(18) 0.0248(16) 0.0270(17) -0.0021(13) 0.0044(13) -0.0089(13)
C13A 0.058(5) 0.026(4) 0.032(4) -0.005(3) 0.017(3) -0.002(3)
C14A 0.037(4) 0.034(4) 0.025(3) 0.000(3) 0.000(3) -0.007(3)
C15A 0.030(3) 0.021(3) 0.031(3) -0.006(3) 0.010(3) -0.003(3)
C17 0.0246(10) 0.0240(10) 0.0235(10) -0.0036(8) 0.0048(8) 0.0017(8)
C18 0.0233(10) 0.0311(11) 0.0305(11) -0.0053(9) 0.0056(8) -0.0052(8)
C19 0.0277(10) 0.0257(10) 0.0314(11) -0.0042(8) 0.0136(9) -0.0058(9)
C20 0.0380(12) 0.0294(11) 0.0236(10) -0.0014(9) 0.0000(9) -0.0017(9)
C21 0.0390(15) 0.088(2) 0.076(2) 0.0453(17) -0.0231(14) -0.0210(15)
C22 0.196(4) 0.0398(16) 0.0359(15) -0.0029(12) 0.050(2) 0.006(2)
C23 0.0322(11) 0.0356(12) 0.0227(10) 0.0041(9) 0.0052(8) 0.0023(9)
C24 0.0457(15) 0.0674(18) 0.0625(17) -0.0316(14) 0.0125(13) 0.0149(13)
C25 0.0176(9) 0.0446(13) 0.0196(10) -0.0017(9) 0.0047(8) -0.0008(9)
C26 0.0298(11) 0.0295(11) 0.0270(11) 0.0009(9) 0.0080(8) -0.0041(9)
C27 0.0277(11) 0.0345(12) 0.0278(11) -0.0074(9) 0.0113(9) 0.0011(9)
C28 0.0262(10) 0.0403(12) 0.0242(10) 0.0017(9) 0.0104(8) -0.0030(9)
C29 0.0496(14) 0.0304(12) 0.0366(12) 0.0057(9) 0.0171(10) 0.0037(10)
C30 0.0418(13) 0.0378(13) 0.0313(12) -0.0043(10) 0.0144(10) 0.0106(10)
C31 0.0499(14) 0.0639(17) 0.0368(13) 0.0084(12) 0.0247(11) 0.0019(12)
C32 0.0336(14) 0.117(3) 0.0521(17) 0.0111(18) 0.0231(12) 0.0004(16)
C33 0.0545(17) 0.090(2) 0.075(2) 0.0260(18) 0.0358(17) 0.0033(16)
C34 0.066(2) 0.144(4) 0.063(2) 0.042(2) 0.0249(18) 0.012(2)
C35 0.075(2) 0.165(4) 0.052(2) -0.003(3) 0.0270(18) -0.010(3)
C36 0.090(3) 0.121(3) 0.064(2) -0.009(2) 0.041(2) 0.004(2)
C37 0.070(2) 0.094(3) 0.066(2) 0.0135(19) 0.0370(17) 0.0196(19)
C38 0.0451(17) 0.182(4) 0.071(2) -0.004(2) 0.0149(16) -0.012(2)
B 0.0277(11) 0.0221(11) 0.0230(11) 0.0032(9) 0.0100(9) -0.0014(9)
N1 0.0279(9) 0.0234(9) 0.0224(8) 0.0029(7) 0.0080(7) 0.0015(7)
N2 0.0233(8) 0.0294(9) 0.0242(8) 0.0007(7) 0.0085(7) 0.0014(7)
N3 0.0247(8) 0.0249(9) 0.0188(8) 0.0017(6) 0.0077(6) -0.0009(7)
N4 0.0284(9) 0.0235(9) 0.0225(8) -0.0016(7) 0.0092(7) -0.0043(7)
N5 0.0250(8) 0.0204(8) 0.0222(8) 0.0008(6) 0.0096(7) -0.0019(7)
N6 0.0267(8) 0.0207(8) 0.0205(8) 0.0012(6) 0.0064(7) -0.0010(7)
O1 0.0255(7) 0.0295(8) 0.0343(8) 0.0020(6) 0.0100(6) -0.0026(6)
O2 0.0473(9) 0.0297(8) 0.0290(8) -0.0050(6) 0.0166(7) -0.0135(7)
O3 0.0304(7) 0.0248(7) 0.0300(7) -0.0032(6) 0.0064(6) 0.0012(6)
O4 0.0297(8) 0.0669(11) 0.0218(7) 0.0002(7) 0.0126(6) -0.0019(7)
Ca 0.0215(2) 0.0247(2) 0.0187(2) 0.00069(15) 0.00737(15) -0.00227(16)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.344(2) . ?
C1 C2 1.402(3) . ?
C1 C4 1.517(3) . ?
C2 C3 1.367(3) . ?
C2 H2 0.95 . ?
C3 N1 1.346(2) . ?
C3 H3 0.95 . ?
C4 C7 1.467(4) . ?
C4 C6 1.532(4) . ?
C4 C7A 1.536(4) . ?
C4 C5A 1.537(4) . ?
C4 C5 1.553(3) . ?
C4 C6A 1.582(4) . ?
C5 H1C5 0.98 . ?
C5 H2C5 0.98 . ?
C5 H3C5 0.98 . ?
C6 H1C6 0.98 . ?
C6 H2C6 0.98 . ?
C6 H3C6 0.98 . ?
C7 O1 1.457(3) . ?
C7 H1C7 0.99 . ?
C7 H2C7 0.99 . ?
C5A H4C5 0.98 . ?
C5A H5C5 0.98 . ?
C5A H6C5 0.98 . ?
C6A H4C6 0.98 . ?
C6A H5C6 0.98 . ?
C6A H6C6 0.98 . ?
C7A O1 1.454(4) . ?
C7A H3C7 0.99 . ?
C7A H4C7 0.99 . ?
C8 O1 1.422(3) . ?
C8 H1C8 0.98 . ?
C8 H2C8 0.98 . ?
C8 H3C8 0.98 . ?
C8 H4C8 0.98 . ?
C8 H5C8 0.98 . ?
C8 H6C8 0.98 . ?
C9 N4 1.341(2) . ?
C9 C10 1.397(3) . ?
C9 C12 1.515(3) . ?
C10 C11 1.370(3) . ?
C10 H10 0.95 . ?
C11 N3 1.343(2) . ?
C11 H11 0.95 . ?
C12 C13 1.499(3) . ?
C12 C15 1.516(3) . ?
C12 C14A 1.518(5) . ?
C12 C13A 1.545(5) . ?
C12 C14 1.558(3) . ?
C12 C15A 1.596(5) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 O2 1.489(3) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 O2 1.399(3) . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C13A H13D 0.98 . ?
C13A H13E 0.98 . ?
C13A H13F 0.98 . ?
C14A H14D 0.98 . ?
C14A H14E 0.98 . ?
C14A H14F 0.98 . ?
C15A O2 1.488(4) . ?
C15A H15C 0.99 . ?
C15A H15D 0.99 . ?
C16A O2 1.500(5) . ?
C16A H16D 0.98 . ?
C16A H16E 0.98 . ?
C16A H16F 0.98 . ?
C17 N6 1.343(2) . ?
C17 C18 1.401(3) . ?
C17 C20 1.518(3) . ?
C18 C19 1.369(3) . ?
C18 H18 0.95 . ?
C19 N5 1.346(2) . ?
C19 H19 0.95 . ?
C20 C22 1.527(3) . ?
C20 C23 1.533(3) . ?
C20 C21 1.542(3) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 O3 1.426(2) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C24 O3 1.419(3) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 O4 1.310(2) . ?
C25 C30 1.404(3) . ?
C25 C26 1.404(3) . ?
C26 C27 1.383(3) . ?
C26 H26 0.95 . ?
C27 C28 1.384(3) . ?
C27 H27 0.95 . ?
C28 C29 1.382(3) . ?
C28 C31 1.509(3) . ?
C29 C30 1.378(3) . ?
C29 H29 0.95 . ?
C30 H30 0.95 . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C32 C33 1.389(4) . ?
C32 C37 1.394(5) . ?
C32 C38 1.482(4) . ?
C33 C34 1.378(5) . ?
C33 H33 0.95 . ?
C34 C35 1.360(6) . ?
C34 H34 0.95 . ?
C35 C36 1.348(5) . ?
C35 H35 0.95 . ?
C36 C37 1.358(5) . ?
C36 H36 0.95 . ?
C37 H37 0.95 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
B N1 1.540(3) . ?
B N5 1.540(3) . ?
B N3 1.547(3) . ?
B H1B 1 . ?
N1 N2 1.370(2) . ?
N2 Ca 2.5129(16) . ?
N3 N4 1.371(2) . ?
N4 Ca 2.5264(16) . ?
N5 N6 1.369(2) . ?
N6 Ca 2.4966(15) . ?
O1 Ca 2.5263(13) . ?
O2 Ca 2.4465(14) . ?
O3 Ca 2.4979(13) . ?
O4 Ca 2.1768(14) . ?

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 C1 C2 110.03(18) . . ?
N2 C1 C4 121.89(17) . . ?
C2 C1 C4 128.04(17) . . ?
C3 C2 C1 105.28(17) . . ?
C3 C2 H2 127.4 . . ?
C1 C2 H2 127.4 . . ?
N1 C3 C2 108.70(18) . . ?
N1 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
C7 C4 C1 109.0(2) . . ?
C7 C4 C6 110.8(2) . . ?
C1 C4 C6 107.0(2) . . ?
C1 C4 C7A 116.4(2) . . ?
C1 C4 C5A 112.4(3) . . ?
C7A C4 C5A 105.4(3) . . ?
C7 C4 C5 113.9(2) . . ?
C1 C4 C5 106.80(19) . . ?
C6 C4 C5 109.0(3) . . ?
C1 C4 C6A 111.1(2) . . ?
C7A C4 C6A 103.9(3) . . ?
C5A C4 C6A 106.9(3) . . ?
C4 C5 H1C5 109.5 . . ?
C4 C5 H2C5 109.5 . . ?
C4 C5 H3C5 109.5 . . ?
C4 C6 H1C6 109.5 . . ?
C4 C6 H2C6 109.5 . . ?
C4 C6 H3C6 109.5 . . ?
O1 C7 C4 115.2(2) . . ?
O1 C7 H1C7 108.5 . . ?
C4 C7 H1C7 108.5 . . ?
O1 C7 H2C7 108.5 . . ?
C4 C7 H2C7 108.5 . . ?
H1C7 C7 H2C7 107.5 . . ?
C4 C5A H4C5 109.5 . . ?
C4 C5A H5C5 109.5 . . ?
H4C5 C5A H5C5 109.5 . . ?
C4 C5A H6C5 109.5 . . ?
H4C5 C5A H6C5 109.5 . . ?
H5C5 C5A H6C5 109.5 . . ?
C4 C6A H4C6 109.5 . . ?
C4 C6A H5C6 109.5 . . ?
H4C6 C6A H5C6 109.5 . . ?
C4 C6A H6C6 109.5 . . ?
H4C6 C6A H6C6 109.5 . . ?
H5C6 C6A H6C6 109.5 . . ?
O1 C7A C4 111.3(3) . . ?
O1 C7A H3C7 109.4 . . ?
C4 C7A H3C7 109.4 . . ?
O1 C7A H4C7 109.4 . . ?
C4 C7A H4C7 109.4 . . ?
H3C7 C7A H4C7 108 . . ?
O1 C8 H1C8 109.5 . . ?
O1 C8 H2C8 109.5 . . ?
O1 C8 H3C8 109.5 . . ?
O1 C8 H4C8 109.5 . . ?
O1 C8 H5C8 109.5 . . ?
H4C8 C8 H5C8 109.5 . . ?
O1 C8 H6C8 109.5 . . ?
H4C8 C8 H6C8 109.5 . . ?
H5C8 C8 H6C8 109.5 . . ?
N4 C9 C10 110.08(17) . . ?
N4 C9 C12 122.31(17) . . ?
C10 C9 C12 127.48(17) . . ?
C11 C10 C9 105.28(17) . . ?
C11 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
N3 C11 C10 108.68(17) . . ?
N3 C11 H11 125.7 . . ?
C10 C11 H11 125.7 . . ?
C13 C12 C9 109.38(19) . . ?
C13 C12 C15 115.4(2) . . ?
C9 C12 C15 110.65(18) . . ?
C9 C12 C14A 113.7(3) . . ?
C9 C12 C13A 114.3(3) . . ?
C14A C12 C13A 109.3(4) . . ?
C13 C12 C14 109.4(2) . . ?
C9 C12 C14 105.56(18) . . ?
C15 C12 C14 106.0(2) . . ?
C9 C12 C15A 113.7(2) . . ?
C14A C12 C15A 103.8(3) . . ?
C13A C12 C15A 100.8(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
O2 C15 C12 111.4(2) . . ?
O2 C15 H15A 109.3 . . ?
C12 C15 H15A 109.3 . . ?
O2 C15 H15B 109.3 . . ?
C12 C15 H15B 109.3 . . ?
H15A C15 H15B 108 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
C12 C13A H13D 109.5 . . ?
C12 C13A H13E 109.5 . . ?
C12 C13A H13F 109.5 . . ?
C12 C14A H14D 109.5 . . ?
C12 C14A H14E 109.5 . . ?
C12 C14A H14F 109.5 . . ?
O2 C15A C12 107.2(3) . . ?
O2 C15A H15C 110.3 . . ?
C12 C15A H15C 110.3 . . ?
O2 C15A H15D 110.3 . . ?
C12 C15A H15D 110.3 . . ?
H15C C15A H15D 108.5 . . ?
O2 C16A H16D 109.5 . . ?
O2 C16A H16E 109.5 . . ?
O2 C16A H16F 109.5 . . ?
N6 C17 C18 109.98(16) . . ?
N6 C17 C20 123.70(17) . . ?
C18 C17 C20 126.31(17) . . ?
C19 C18 C17 105.40(17) . . ?
C19 C18 H18 127.3 . . ?
C17 C18 H18 127.3 . . ?
N5 C19 C18 108.45(17) . . ?
N5 C19 H19 125.8 . . ?
C18 C19 H19 125.8 . . ?
C17 C20 C22 109.17(18) . . ?
C17 C20 C23 114.92(16) . . ?
C22 C20 C23 105.5(2) . . ?
C17 C20 C21 108.23(19) . . ?
C22 C20 C21 108.6(2) . . ?
C23 C20 C21 110.23(19) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C20 117.91(16) . . ?
O3 C23 H23A 107.8 . . ?
C20 C23 H23A 107.8 . . ?
O3 C23 H23B 107.8 . . ?
C20 C23 H23B 107.8 . . ?
H23A C23 H23B 107.2 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 C30 122.19(18) . . ?
O4 C25 C26 122.26(19) . . ?
C30 C25 C26 115.55(17) . . ?
C27 C26 C25 121.73(19) . . ?
C27 C26 H26 119.1 . . ?
C25 C26 H26 119.1 . . ?
C26 C27 C28 121.97(19) . . ?
C26 C27 H27 119 . . ?
C28 C27 H27 119 . . ?
C29 C28 C27 116.71(18) . . ?
C29 C28 C31 121.1(2) . . ?
C27 C28 C31 122.19(19) . . ?
C30 C29 C28 122.2(2) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C29 C30 C25 121.84(19) . . ?
C29 C30 H30 119.1 . . ?
C25 C30 H30 119.1 . . ?
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 . . ?
C33 C32 C37 116.5(3) . . ?
C33 C32 C38 122.2(4) . . ?
C37 C32 C38 121.3(3) . . ?
C34 C33 C32 120.8(4) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C35 C34 C33 120.8(4) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C34 119.1(4) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C37 121.4(4) . . ?
C35 C36 H36 119.3 . . ?
C37 C36 H36 119.3 . . ?
C36 C37 C32 121.4(3) . . ?
C36 C37 H37 119.3 . . ?
C32 C37 H37 119.3 . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 B N5 111.93(15) . . ?
N1 B N3 110.15(15) . . ?
N5 B N3 110.33(15) . . ?
N1 B H1B 108.1 . . ?
N5 B H1B 108.1 . . ?
N3 B H1B 108.1 . . ?
C3 N1 N2 109.87(16) . . ?
C3 N1 B 126.60(16) . . ?
N2 N1 B 123.14(15) . . ?
C1 N2 N1 106.11(15) . . ?
C1 N2 Ca 135.54(13) . . ?
N1 N2 Ca 118.13(11) . . ?
C11 N3 N4 109.68(15) . . ?
C11 N3 B 126.97(16) . . ?
N4 N3 B 123.33(14) . . ?
C9 N4 N3 106.26(15) . . ?
C9 N4 Ca 135.14(12) . . ?
N3 N4 Ca 116.65(10) . . ?
C19 N5 N6 109.98(15) . . ?
C19 N5 B 126.83(16) . . ?
N6 N5 B 122.47(14) . . ?
C17 N6 N5 106.18(14) . . ?
C17 N6 Ca 134.75(12) . . ?
N5 N6 Ca 118.95(10) . . ?
C8 O1 C7A 101.7(2) . . ?
C8 O1 C7 116.98(19) . . ?
C8 O1 Ca 110.89(12) . . ?
C7A O1 Ca 106.44(19) . . ?
C7 O1 Ca 131.30(15) . . ?
C16 O2 C15A 86.9(3) . . ?
C16 O2 C15 115.1(2) . . ?
C15A O2 C15 60.8(2) . . ?
C15A O2 C16A 101.6(4) . . ?
C15 O2 C16A 132.3(3) . . ?
C16 O2 Ca 129.2(2) . . ?
C15A O2 Ca 137.4(2) . . ?
C15 O2 Ca 109.57(14) . . ?
C16A O2 Ca 111.1(3) . . ?
C24 O3 C23 113.92(16) . . ?
C24 O3 Ca 125.13(14) . . ?
C23 O3 Ca 112.26(11) . . ?
C25 O4 Ca 167.80(14) . . ?
O4 Ca O2 109.81(5) . . ?
O4 Ca N6 99.87(5) . . ?
O2 Ca N6 125.74(5) . . ?
O4 Ca O3 82.93(5) . . ?
O2 Ca O3 72.94(5) . . ?
N6 Ca O3 66.81(5) . . ?
O4 Ca N2 104.34(6) . . ?
O2 Ca N2 130.80(5) . . ?
N6 Ca N2 80.06(5) . . ?
O3 Ca N2 146.86(5) . . ?
O4 Ca O1 78.77(5) . . ?
O2 Ca O1 82.40(5) . . ?
N6 Ca O1 149.06(5) . . ?
O3 Ca O1 142.03(5) . . ?
N2 Ca O1 70.58(5) . . ?
O4 Ca N4 178.29(6) . . ?
O2 Ca N4 71.72(5) . . ?
N6 Ca N4 79.62(5) . . ?
O3 Ca N4 98.33(5) . . ?
N2 Ca N4 73.98(5) . . ?
O1 Ca N4 100.81(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
N2 C1 C2 C3 0.3(2) . . . . ?
C4 C1 C2 C3 -177.61(19) . . . . ?
C1 C2 C3 N1 0.1(2) . . . . ?
N2 C1 C4 C7 -53.5(3) . . . . ?
C2 C1 C4 C7 124.1(2) . . . . ?
N2 C1 C4 C6 -173.4(2) . . . . ?
C2 C1 C4 C6 4.3(3) . . . . ?
N2 C1 C4 C7A 5.3(3) . . . . ?
C2 C1 C4 C7A -177.0(2) . . . . ?
N2 C1 C4 C5A 127.0(3) . . . . ?
C2 C1 C4 C5A -55.3(3) . . . . ?
N2 C1 C4 C5 70.0(3) . . . . ?
C2 C1 C4 C5 -112.4(2) . . . . ?
N2 C1 C4 C6A -113.3(3) . . . . ?
C2 C1 C4 C6A 64.4(3) . . . . ?
C1 C4 C7 O1 71.5(3) . . . . ?
C6 C4 C7 O1 -171.0(3) . . . . ?
C7A C4 C7 O1 -37.8(3) . . . . ?
C5A C4 C7 O1 -109.2(4) . . . . ?
C5 C4 C7 O1 -47.6(3) . . . . ?
C6A C4 C7 O1 174.6(4) . . . . ?
C7 C4 C7A O1 36.6(2) . . . . ?
C1 C4 C7A O1 -58.8(3) . . . . ?
C6 C4 C7A O1 119.4(4) . . . . ?
C5A C4 C7A O1 175.9(3) . . . . ?
C5 C4 C7A O1 -153.8(4) . . . . ?
C6A C4 C7A O1 63.7(4) . . . . ?
N4 C9 C10 C11 -1.0(2) . . . . ?
C12 C9 C10 C11 174.84(18) . . . . ?
C9 C10 C11 N3 0.5(2) . . . . ?
N4 C9 C12 C13 -121.0(2) . . . . ?
C10 C9 C12 C13 63.5(3) . . . . ?
N4 C9 C12 C15 7.1(3) . . . . ?
C10 C9 C12 C15 -168.3(2) . . . . ?
N4 C9 C12 C14A 62.6(3) . . . . ?
C10 C9 C12 C14A -112.8(3) . . . . ?
N4 C9 C12 C13A -170.8(3) . . . . ?
C10 C9 C12 C13A 13.7(4) . . . . ?
N4 C9 C12 C14 121.3(2) . . . . ?
C10 C9 C12 C14 -54.1(3) . . . . ?
N4 C9 C12 C15A -55.8(3) . . . . ?
C10 C9 C12 C15A 128.8(3) . . . . ?
C13 C12 C15 O2 55.9(3) . . . . ?
C9 C12 C15 O2 -68.9(2) . . . . ?
C14A C12 C15 O2 -173.2(4) . . . . ?
C13A C12 C15 O2 108.4(4) . . . . ?
C14 C12 C15 O2 177.1(2) . . . . ?
C15A C12 C15 O2 36.8(3) . . . . ?
C13 C12 C15A O2 164.1(4) . . . . ?
C9 C12 C15A O2 64.5(4) . . . . ?
C15 C12 C15A O2 -35.8(2) . . . . ?
C14A C12 C15A O2 -59.5(4) . . . . ?
C13A C12 C15A O2 -172.7(4) . . . . ?
C14 C12 C15A O2 -111.1(4) . . . . ?
N6 C17 C18 C19 -0.6(2) . . . . ?
C20 C17 C18 C19 -179.93(19) . . . . ?
C17 C18 C19 N5 0.3(2) . . . . ?
N6 C17 C20 C22 -99.2(3) . . . . ?
C18 C17 C20 C22 80.0(3) . . . . ?
N6 C17 C20 C23 19.0(3) . . . . ?
C18 C17 C20 C23 -161.71(19) . . . . ?
N6 C17 C20 C21 142.7(2) . . . . ?
C18 C17 C20 C21 -38.0(3) . . . . ?
C17 C20 C23 O3 26.6(3) . . . . ?
C22 C20 C23 O3 146.9(2) . . . . ?
C21 C20 C23 O3 -96.1(2) . . . . ?
O4 C25 C26 C27 -178.96(18) . . . . ?
C30 C25 C26 C27 1.4(3) . . . . ?
C25 C26 C27 C28 -0.6(3) . . . . ?
C26 C27 C28 C29 -0.3(3) . . . . ?
C26 C27 C28 C31 178.04(19) . . . . ?
C27 C28 C29 C30 0.2(3) . . . . ?
C31 C28 C29 C30 -178.1(2) . . . . ?
C28 C29 C30 C25 0.7(3) . . . . ?
O4 C25 C30 C29 178.89(19) . . . . ?
C26 C25 C30 C29 -1.5(3) . . . . ?
C37 C32 C33 C34 0.3(4) . . . . ?
C38 C32 C33 C34 -179.5(3) . . . . ?
C32 C33 C34 C35 0.7(5) . . . . ?
C33 C34 C35 C36 -1.2(5) . . . . ?
C34 C35 C36 C37 0.7(5) . . . . ?
C35 C36 C37 C32 0.4(5) . . . . ?
C33 C32 C37 C36 -0.9(4) . . . . ?
C38 C32 C37 C36 178.9(3) . . . . ?
C2 C3 N1 N2 -0.4(2) . . . . ?
C2 C3 N1 B 172.58(17) . . . . ?
N5 B N1 C3 124.87(19) . . . . ?
N3 B N1 C3 -112.0(2) . . . . ?
N5 B N1 N2 -63.1(2) . . . . ?
N3 B N1 N2 60.1(2) . . . . ?
C2 C1 N2 N1 -0.5(2) . . . . ?
C4 C1 N2 N1 177.55(16) . . . . ?
C2 C1 N2 Ca -174.80(14) . . . . ?
C4 C1 N2 Ca 3.3(3) . . . . ?
C3 N1 N2 C1 0.5(2) . . . . ?
B N1 N2 C1 -172.71(16) . . . . ?
C3 N1 N2 Ca 176.01(12) . . . . ?
B N1 N2 Ca 2.8(2) . . . . ?
C10 C11 N3 N4 0.1(2) . . . . ?
C10 C11 N3 B -178.23(17) . . . . ?
N1 B N3 C11 126.60(19) . . . . ?
N5 B N3 C11 -109.3(2) . . . . ?
N1 B N3 N4 -51.6(2) . . . . ?
N5 B N3 N4 72.5(2) . . . . ?
C10 C9 N4 N3 1.1(2) . . . . ?
C12 C9 N4 N3 -175.01(15) . . . . ?
C10 C9 N4 Ca -161.70(13) . . . . ?
C12 C9 N4 Ca 22.2(3) . . . . ?
C11 N3 N4 C9 -0.8(2) . . . . ?
B N3 N4 C9 177.65(16) . . . . ?
C11 N3 N4 Ca 165.74(12) . . . . ?
B N3 N4 Ca -15.8(2) . . . . ?
C18 C19 N5 N6 0.0(2) . . . . ?
C18 C19 N5 B -170.35(17) . . . . ?
N1 B N5 C19 -125.45(19) . . . . ?
N3 B N5 C19 111.5(2) . . . . ?
N1 B N5 N6 65.3(2) . . . . ?
N3 B N5 N6 -57.7(2) . . . . ?
C18 C17 N6 N5 0.6(2) . . . . ?
C20 C17 N6 N5 179.95(17) . . . . ?
C18 C17 N6 Ca 176.43(13) . . . . ?
C20 C17 N6 Ca -4.2(3) . . . . ?
C19 N5 N6 C17 -0.4(2) . . . . ?
B N5 N6 C17 170.48(16) . . . . ?
C19 N5 N6 Ca -176.99(11) . . . . ?
B N5 N6 Ca -6.1(2) . . . . ?
C4 C7A O1 C8 -150.6(3) . . . . ?
C4 C7A O1 C7 -35.9(2) . . . . ?
C4 C7A O1 Ca 93.2(3) . . . . ?
C4 C7 O1 C8 125.4(3) . . . . ?
C4 C7 O1 C7A 39.2(3) . . . . ?
C4 C7 O1 Ca -43.1(4) . . . . ?
C12 C15A O2 C16 156.4(4) . . . . ?
C12 C15A O2 C15 35.3(2) . . . . ?
C12 C15A O2 C16A 167.5(4) . . . . ?
C12 C15A O2 Ca -52.4(5) . . . . ?
C12 C15 O2 C16 -109.3(3) . . . . ?
C12 C15 O2 C15A -38.6(3) . . . . ?
C12 C15 O2 C16A -117.3(4) . . . . ?
C12 C15 O2 Ca 95.6(2) . . . . ?
C20 C23 O3 C24 67.9(2) . . . . ?
C20 C23 O3 Ca -81.63(18) . . . . ?
C30 C25 O4 Ca 25.6(7) . . . . ?
C26 C25 O4 Ca -154.0(5) . . . . ?
C25 O4 Ca O2 -11.5(6) . . . . ?
C25 O4 Ca N6 -145.4(6) . . . . ?
C25 O4 Ca O3 -80.5(6) . . . . ?
C25 O4 Ca N2 132.5(6) . . . . ?
C25 O4 Ca O1 66.1(6) . . . . ?
C16 O2 Ca O4 -18.3(3) . . . . ?
C15A O2 Ca O4 -159.9(3) . . . . ?
C15 O2 Ca O4 132.32(14) . . . . ?
C16A O2 Ca O4 -22.2(3) . . . . ?
C16 O2 Ca N6 100.7(2) . . . . ?
C15A O2 Ca N6 -41.0(3) . . . . ?
C15 O2 Ca N6 -108.76(14) . . . . ?
C16A O2 Ca N6 96.7(3) . . . . ?
C16 O2 Ca O3 57.4(2) . . . . ?
C15A O2 Ca O3 -84.2(3) . . . . ?
C15 O2 Ca O3 -152.01(14) . . . . ?
C16A O2 Ca O3 53.5(3) . . . . ?
C16 O2 Ca N2 -149.4(2) . . . . ?
C15A O2 Ca N2 68.9(3) . . . . ?
C15 O2 Ca N2 1.13(16) . . . . ?
C16A O2 Ca N2 -153.4(3) . . . . ?
C16 O2 Ca O1 -93.4(2) . . . . ?
C15A O2 Ca O1 125.0(3) . . . . ?
C15 O2 Ca O1 57.20(14) . . . . ?
C16A O2 Ca O1 -97.3(3) . . . . ?
C16 O2 Ca N4 162.5(3) . . . . ?
C15A O2 Ca N4 20.9(3) . . . . ?
C15 O2 Ca N4 -46.88(14) . . . . ?
C16A O2 Ca N4 158.6(3) . . . . ?
C17 N6 Ca O4 47.50(18) . . . . ?
N5 N6 Ca O4 -137.08(12) . . . . ?
C17 N6 Ca O2 -75.80(18) . . . . ?
N5 N6 Ca O2 99.62(12) . . . . ?
C17 N6 Ca O3 -30.35(16) . . . . ?
N5 N6 Ca O3 145.07(13) . . . . ?
C17 N6 Ca N2 150.49(18) . . . . ?
N5 N6 Ca N2 -34.09(12) . . . . ?
C17 N6 Ca O1 132.09(16) . . . . ?
N5 N6 Ca O1 -52.49(17) . . . . ?
C17 N6 Ca N4 -134.16(18) . . . . ?
N5 N6 Ca N4 41.26(12) . . . . ?
C24 O3 Ca O4 175.95(18) . . . . ?
C23 O3 Ca O4 -38.60(12) . . . . ?
C24 O3 Ca O2 62.67(17) . . . . ?
C23 O3 Ca O2 -151.88(12) . . . . ?
C24 O3 Ca N6 -80.10(17) . . . . ?
C23 O3 Ca N6 65.35(12) . . . . ?
C24 O3 Ca N2 -78.59(19) . . . . ?
C23 O3 Ca N2 66.86(15) . . . . ?
C24 O3 Ca O1 114.50(18) . . . . ?
C23 O3 Ca O1 -100.05(13) . . . . ?
C24 O3 Ca N4 -5.21(18) . . . . ?
C23 O3 Ca N4 140.23(12) . . . . ?
C1 N2 Ca O4 -52.78(18) . . . . ?
N1 N2 Ca O4 133.43(12) . . . . ?
C1 N2 Ca O2 80.26(19) . . . . ?
N1 N2 Ca O2 -93.53(13) . . . . ?
C1 N2 Ca N6 -150.53(18) . . . . ?
N1 N2 Ca N6 35.68(12) . . . . ?
C1 N2 Ca O3 -151.94(16) . . . . ?
N1 N2 Ca O3 34.27(17) . . . . ?
C1 N2 Ca O1 19.56(17) . . . . ?
N1 N2 Ca O1 -154.22(13) . . . . ?
C1 N2 Ca N4 127.51(18) . . . . ?
N1 N2 Ca N4 -46.28(12) . . . . ?
C8 O1 Ca O4 -58.60(15) . . . . ?
C7A O1 Ca O4 51.24(19) . . . . ?
C7 O1 Ca O4 110.5(2) . . . . ?
C8 O1 Ca O2 53.43(15) . . . . ?
C7A O1 Ca O2 163.27(19) . . . . ?
C7 O1 Ca O2 -137.5(2) . . . . ?
C8 O1 Ca N6 -149.10(15) . . . . ?
C7A O1 Ca N6 -39.3(2) . . . . ?
C7 O1 Ca N6 20.0(3) . . . . ?
C8 O1 Ca O3 4.12(18) . . . . ?
C7A O1 Ca O3 113.96(19) . . . . ?
C7 O1 Ca O3 173.2(2) . . . . ?
C8 O1 Ca N2 -168.34(15) . . . . ?
C7A O1 Ca N2 -58.49(19) . . . . ?
C7 O1 Ca N2 0.7(2) . . . . ?
C8 O1 Ca N4 123.09(15) . . . . ?
C7A O1 Ca N4 -127.07(19) . . . . ?
C7 O1 Ca N4 -67.8(2) . . . . ?
C9 N4 Ca O2 -1.75(17) . . . . ?
N3 N4 Ca O2 -163.26(13) . . . . ?
C9 N4 Ca N6 131.56(18) . . . . ?
N3 N4 Ca N6 -29.95(12) . . . . ?
C9 N4 Ca O3 67.11(17) . . . . ?
N3 N4 Ca O3 -94.40(12) . . . . ?
C9 N4 Ca N2 -145.91(18) . . . . ?
N3 N4 Ca N2 52.58(12) . . . . ?
C9 N4 Ca O1 -79.93(17) . . . . ?
N3 N4 Ca O1 118.56(12) . . . . ?

#===END

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-09-30 at 17:41:51
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : shelxl dreduc import struct

data_Chisholm1492a
_database_code_depnum_ccdc_archive 'CCDC 705808'

_audit_creation_date             2008-09-30T17:41:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Chisholm 1492a'
_chemical_formula_moiety         'C24 H40 B1 N6 O3, C24 H40 B1 Ca1 N6 O3'
_chemical_formula_sum            'C48 H80 B2 Ca N12 O6'
_chemical_formula_weight         982.94
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.2546(2)
_cell_length_b                   16.7217(3)
_cell_length_c                   24.6146(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.840(1)
_cell_angle_gamma                90
_cell_volume                     5720.45(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    7697
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      22.465
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       'rectangular rod'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2120
_exptl_special_details           
;All work was done at 230 K. The data collection strategy was set
up to measure a quadrant of reciprocal space with a redundancy factor
of 2.8, which means that 90% of the reflections were measured at
least 2.8 times. Omega scans with a frame width of 1.0 degree
were used. Data integration was done with Denzo, and scaling
and merging of the data was done with Scalepack. Merging the data
and averaging the symmetry equivalent reflections resulted in an
Rint value of 0.085. This was a weakly diffracting crystal, and the
data set was measured only to a maximum two theta value of
45 degrees.

The asymmetric unit consists of a Ca(Tp)* complex and
a free Tp* molecule. One of the branches of the free Tp* molecule is
disordered and this was modeled with two sets of atoms: C(45), C(46),
C(47), O(5), C(48) and C(45A), C(46A), C(47A), O(5A) and C(48A).
These two sets of atoms were refined only isotropically and DFIX
restraints were used.
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.340732E-1
_diffrn_orient_matrix_ub_12      -0.503023E-1
_diffrn_orient_matrix_ub_13      -0.62267E-2
_diffrn_orient_matrix_ub_21      0.530064E-1
_diffrn_orient_matrix_ub_22      0.323423E-1
_diffrn_orient_matrix_ub_23      -0.96708E-2
_diffrn_orient_matrix_ub_31      0.347339E-1
_diffrn_orient_matrix_ub_32      -0.111E-4
_diffrn_orient_matrix_ub_33      0.400493E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega scans'
_diffrn_reflns_av_R_equivalents  0.085
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_number            51480
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         22.45
_diffrn_reflns_theta_full        22.45
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             7420
_reflns_number_gt                4516
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;For the methyl groups, the hydrogen atoms were added at calculated
positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom).
The torsion angle, which defines the orientation of the methyl group
about the O-C bond, was refined. For the other methyl groups, i.e.,
the ones bonded to carbon atoms, and for the methyl groups in the
disordered region, these torsion angles were not refined. The remaining
hydrogen atoms were included in the model at calculated positions using
a riding model with U(H) = 1.2 * Ueq(attached atom).

The final difference electron density map contains maximum and minimum
peak heights of 0.99 and -0.47 e/Ang**3. The largest peak in the map is
in the vicinity of another branch of the free Tp* molecule. Many attempts
were made to model this region as another disordered branch, but a reasonable
disorder model could not be obtained.

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     
'w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+19.3301P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7420
_refine_ls_number_parameters     622
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1502
_refine_ls_R_factor_gt           0.0885
_refine_ls_wR_factor_ref         0.2589
_refine_ls_wR_factor_gt          0.2301
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.003
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1 C 0.2995(5) 0.4960(4) 0.2292(3) 0.0458(17) Uani 1 1 d . . .
C2 C 0.2709(5) 0.5096(5) 0.2788(3) 0.059(2) Uani 1 1 d . . .
H2 H 0.2077 0.5136 0.2839 0.071 Uiso 1 1 calc R . .
C3 C 0.3533(6) 0.5160(4) 0.3183(3) 0.056(2) Uani 1 1 d . . .
H3 H 0.3573 0.5245 0.3565 0.067 Uiso 1 1 calc R . .
C4 C 0.2367(5) 0.4835(4) 0.1711(3) 0.0503(19) Uani 1 1 d . . .
C5 C 0.1504(5) 0.4330(5) 0.1750(3) 0.078(3) Uani 1 1 d . . .
H5A H 0.1137 0.4598 0.1985 0.118 Uiso 1 1 calc R . .
H5B H 0.1719 0.3814 0.191 0.118 Uiso 1 1 calc R . .
H5C H 0.1101 0.4254 0.1381 0.118 Uiso 1 1 calc R . .
C6 C 0.2024(6) 0.5666(5) 0.1468(3) 0.074(2) Uani 1 1 d . . .
H6A H 0.1686 0.5936 0.1716 0.112 Uiso 1 1 calc R . .
H6B H 0.1596 0.56 0.1105 0.112 Uiso 1 1 calc R . .
H6C H 0.2577 0.5982 0.1431 0.112 Uiso 1 1 calc R . .
C7 C 0.2895(5) 0.4397(4) 0.1343(3) 0.055(2) Uani 1 1 d . . .
H7A H 0.3189 0.392 0.1543 0.066 Uiso 1 1 calc R . .
H7B H 0.2425 0.4213 0.1014 0.066 Uiso 1 1 calc R . .
C8 C 0.3353(5) 0.5074(5) 0.0579(3) 0.065(2) Uani 1 1 d . . .
H8A H 0.3281 0.4602 0.0344 0.098 Uiso 1 1 calc R . .
H8B H 0.3843 0.542 0.0489 0.098 Uiso 1 1 calc R . .
H8C H 0.2745 0.5359 0.0517 0.098 Uiso 1 1 calc R . .
C9 C 0.6203(4) 0.6752(4) 0.2455(3) 0.0406(17) Uani 1 1 d . . .
C10 C 0.6596(5) 0.6997(4) 0.2996(3) 0.0520(19) Uani 1 1 d . . .
H10 H 0.6968 0.7458 0.3104 0.062 Uiso 1 1 calc R . .
C11 C 0.6337(5) 0.6439(4) 0.3339(3) 0.0497(19) Uani 1 1 d . . .
H11 H 0.6497 0.645 0.3731 0.06 Uiso 1 1 calc R . .
C12 C 0.6271(5) 0.7127(4) 0.1916(3) 0.0466(18) Uani 1 1 d . . .
C13 C 0.6227(6) 0.8037(4) 0.1975(4) 0.076(2) Uani 1 1 d . . .
H13A H 0.6274 0.8288 0.1626 0.113 Uiso 1 1 calc R . .
H13B H 0.6756 0.8214 0.2269 0.113 Uiso 1 1 calc R . .
H13C H 0.5622 0.8185 0.2065 0.113 Uiso 1 1 calc R . .
C14 C 0.7215(5) 0.6894(5) 0.1768(3) 0.065(2) Uani 1 1 d . . .
H14A H 0.7258 0.7146 0.1419 0.097 Uiso 1 1 calc R . .
H14B H 0.7241 0.6318 0.1729 0.097 Uiso 1 1 calc R . .
H14C H 0.7748 0.707 0.2061 0.097 Uiso 1 1 calc R . .
C15 C 0.5410(5) 0.6910(4) 0.1439(3) 0.0514(19) Uani 1 1 d . . .
H15A H 0.4814 0.6996 0.1567 0.062 Uiso 1 1 calc R . .
H15B H 0.5402 0.7271 0.1125 0.062 Uiso 1 1 calc R . .
C16 C 0.5646(5) 0.6053(4) 0.0703(3) 0.0539(19) Uani 1 1 d . . .
H16A H 0.5186 0.6375 0.0443 0.081 Uiso 1 1 calc R . .
H16B H 0.5605 0.5501 0.0578 0.081 Uiso 1 1 calc R . .
H16C H 0.6291 0.6254 0.0721 0.081 Uiso 1 1 calc R . .
C17 C 0.6469(4) 0.3466(4) 0.2611(3) 0.0417(17) Uani 1 1 d . . .
C18 C 0.6741(5) 0.3252(5) 0.3163(3) 0.059(2) Uani 1 1 d . . .
H18 H 0.7103 0.2802 0.3311 0.07 Uiso 1 1 calc R . .
C19 C 0.6373(5) 0.3834(5) 0.3455(3) 0.057(2) Uani 1 1 d . . .
H19 H 0.6443 0.3852 0.3843 0.068 Uiso 1 1 calc R . .
C20 C 0.6668(5) 0.3043(4) 0.2103(3) 0.0460(18) Uani 1 1 d . . .
C21 C 0.5863(6) 0.2431(5) 0.1906(4) 0.078(3) Uani 1 1 d . . .
H21A H 0.5843 0.206 0.2206 0.117 Uiso 1 1 calc R . .
H21B H 0.5986 0.214 0.1589 0.117 Uiso 1 1 calc R . .
H21C H 0.5251 0.2707 0.18 0.117 Uiso 1 1 calc R . .
C22 C 0.7652(6) 0.2624(5) 0.2261(3) 0.074(2) Uani 1 1 d . . .
H22A H 0.7648 0.224 0.2556 0.111 Uiso 1 1 calc R . .
H22B H 0.8151 0.3018 0.2389 0.111 Uiso 1 1 calc R . .
H22C H 0.7778 0.2349 0.1937 0.111 Uiso 1 1 calc R . .
C23 C 0.6748(5) 0.3630(4) 0.1649(3) 0.0439(17) Uani 1 1 d . . .
H23A H 0.7189 0.406 0.1811 0.053 Uiso 1 1 calc R . .
H23B H 0.7028 0.3356 0.1371 0.053 Uiso 1 1 calc R . .
C24 C 0.5515(6) 0.3741(5) 0.0808(3) 0.072(2) Uani 1 1 d . . .
H24A H 0.5988 0.3903 0.06 0.108 Uiso 1 1 calc R . .
H24B H 0.4902 0.3991 0.0647 0.108 Uiso 1 1 calc R . .
H24C H 0.5443 0.3164 0.079 0.108 Uiso 1 1 calc R . .
B1 B 0.5368(6) 0.5122(5) 0.3219(3) 0.048(2) Uani 1 1 d . . .
H1 H 0.5437 0.5157 0.3627 0.058 Uiso 1 1 calc R . .
Ca Ca 0.51345(9) 0.50067(8) 0.18032(5) 0.0383(4) Uani 1 1 d . . .
N1 N 0.4283(4) 0.5082(3) 0.2941(2) 0.0442(14) Uani 1 1 d . . .
N2 N 0.3953(4) 0.4960(3) 0.2381(2) 0.0428(13) Uani 1 1 d . . .
N3 N 0.5816(4) 0.5873(3) 0.3024(2) 0.0416(14) Uani 1 1 d . . .
N4 N 0.5732(4) 0.6053(3) 0.2472(2) 0.0406(14) Uani 1 1 d . . .
N5 N 0.5900(4) 0.4366(3) 0.3090(2) 0.0444(14) Uani 1 1 d . . .
N6 N 0.5949(4) 0.4145(3) 0.2559(2) 0.0401(13) Uani 1 1 d . . .
O1 O 0.3634(3) 0.4836(3) 0.11581(17) 0.0492(12) Uani 1 1 d . . .
O2 O 0.5430(3) 0.6098(3) 0.12502(17) 0.0459(12) Uani 1 1 d . . .
O3 O 0.5825(3) 0.3983(3) 0.13703(17) 0.0497(12) Uani 1 1 d . . .
C25 C 0.9266(5) 0.5409(4) 0.2468(3) 0.0497(19) Uani 1 1 d . . .
C26 C 0.9766(5) 0.5984(4) 0.2235(3) 0.056(2) Uani 1 1 d . . .
H26 H 1.0233 0.6342 0.2425 0.067 Uiso 1 1 calc R . .
C27 C 0.9434(5) 0.5915(4) 0.1667(3) 0.0543(19) Uani 1 1 d . . .
H27 H 0.9636 0.6221 0.1394 0.065 Uiso 1 1 calc R . .
C28 C 0.9319(5) 0.5183(4) 0.3069(3) 0.0532(19) Uani 1 1 d . . .
C29 C 0.8325(6) 0.5258(6) 0.3199(4) 0.086(3) Uani 1 1 d . . .
H29A H 0.8364 0.5121 0.3587 0.13 Uiso 1 1 calc R . .
H29B H 0.7882 0.4896 0.2962 0.13 Uiso 1 1 calc R . .
H29C H 0.8096 0.5803 0.3132 0.13 Uiso 1 1 calc R . .
C30 C 1.0024(7) 0.5736(6) 0.3460(3) 0.098(3) Uani 1 1 d . . .
H30A H 1.0657 0.569 0.3379 0.146 Uiso 1 1 calc R . .
H30B H 1.0057 0.5582 0.3843 0.146 Uiso 1 1 calc R . .
H30C H 0.9803 0.6285 0.3403 0.146 Uiso 1 1 calc R . .
C31 C 0.9624(6) 0.4326(5) 0.3156(3) 0.076(3) Uani 1 1 d . . .
H31A H 0.9645 0.4174 0.3543 0.091 Uiso 1 1 calc R . .
H31B H 0.915 0.3984 0.2913 0.091 Uiso 1 1 calc R . .
C32 C 1.0709(10) 0.3366(7) 0.2973(5) 0.151(6) Uani 1 1 d . . .
H32A H 1.0611 0.3074 0.3296 0.226 Uiso 1 1 calc R . .
H32B H 1.1367 0.3295 0.2936 0.226 Uiso 1 1 calc R . .
H32C H 1.0271 0.3165 0.2641 0.226 Uiso 1 1 calc R . .
C33 C 0.8383(5) 0.6689(4) 0.0099(3) 0.0432(17) Uani 1 1 d . . .
C34 C 0.9096(5) 0.6207(5) -0.0022(3) 0.0541(19) Uani 1 1 d . . .
H34 H 0.9513 0.6329 -0.0257 0.065 Uiso 1 1 calc R . .
C35 C 0.9073(5) 0.5515(4) 0.0272(3) 0.0523(19) Uani 1 1 d . . .
H35 H 0.948 0.5071 0.0277 0.063 Uiso 1 1 calc R . .
C36 C 0.8082(5) 0.7517(4) -0.0076(3) 0.057(2) Uani 1 1 d . . .
C37 C 0.8421(6) 0.7755(5) -0.0603(3) 0.078(3) Uani 1 1 d . . .
H37A H 0.8227 0.8301 -0.0703 0.116 Uiso 1 1 calc R . .
H37B H 0.8135 0.7399 -0.0906 0.116 Uiso 1 1 calc R . .
H37C H 0.9117 0.7714 -0.0533 0.116 Uiso 1 1 calc R . .
C38 C 0.8514(9) 0.8105(6) 0.0389(4) 0.122(4) Uani 1 1 d . . .
H38A H 0.8327 0.8646 0.0269 0.182 Uiso 1 1 calc R . .
H38B H 0.921 0.8062 0.0473 0.182 Uiso 1 1 calc R . .
H38C H 0.828 0.798 0.072 0.182 Uiso 1 1 calc R . .
C39 C 0.6993(7) 0.7586(5) -0.0172(5) 0.103(4) Uani 1 1 d . . .
H39A H 0.6687 0.7294 -0.051 0.124 Uiso 1 1 calc R . .
H39B H 0.6774 0.7352 0.0143 0.124 Uiso 1 1 calc R . .
O6 O 0.6720(6) 0.8431(5) -0.0231(3) 0.130(3) Uani 1 1 d . . .
C40 C 0.5713(11) 0.8575(9) -0.0166(8) 0.202(8) Uani 1 1 d . . .
H40A H 0.5567 0.9142 -0.0206 0.303 Uiso 1 1 calc R . .
H40B H 0.5654 0.8398 0.0201 0.303 Uiso 1 1 calc R . .
H40C H 0.5266 0.8279 -0.0449 0.303 Uiso 1 1 calc R . .
C41 C 0.8216(5) 0.3025(4) 0.0506(3) 0.0471(18) Uani 1 1 d . A .
C42 C 0.8977(5) 0.2950(4) 0.0980(3) 0.0530(19) Uani 1 1 d . . .
H42 H 0.9344 0.2491 0.1101 0.064 Uiso 1 1 calc R . .
C43 C 0.9065(5) 0.3682(4) 0.1221(3) 0.0449(17) Uani 1 1 d . . .
H43 H 0.9512 0.3826 0.1547 0.054 Uiso 1 1 calc R . .
C44 C 0.7813(5) 0.2400(4) 0.0072(3) 0.064(2) Uani 1 1 d D . .
B2 B 0.8138(5) 0.5048(4) 0.1012(3) 0.0408(19) Uani 1 1 d . . .
H2A H 0.7448 0.5089 0.1018 0.049 Uiso 1 1 calc R . .
N7 N 0.8768(4) 0.5333(3) 0.1575(2) 0.0418(14) Uani 1 1 d . . .
N8 N 0.8648(4) 0.5020(3) 0.2064(2) 0.0449(14) Uani 1 1 d . . .
N9 N 0.8363(4) 0.5581(3) 0.0554(2) 0.0408(14) Uani 1 1 d . . .
N10 N 0.7934(4) 0.6307(3) 0.0448(2) 0.0427(14) Uani 1 1 d . . .
N11 N 0.8400(4) 0.4167(3) 0.0912(2) 0.0402(13) Uani 1 1 d . A .
N12 N 0.7877(4) 0.3760(3) 0.0468(2) 0.0456(14) Uani 1 1 d . . .
O4 O 1.0525(5) 0.4204(4) 0.3039(3) 0.108(2) Uani 1 1 d . . .
O5 O 0.7178(11) 0.1107(8) -0.0055(6) 0.116(5) Uiso 0.556(14) 1 d PD A 3
C45 C 0.6996(9) 0.2732(8) -0.0388(5) 0.067(5) Uiso 0.556(14) 1 d PD A 3
H45A H 0.6525 0.2996 -0.0221 0.1 Uiso 0.556(14) 1 calc PR A 3
H45B H 0.6691 0.2296 -0.0622 0.1 Uiso 0.556(14) 1 calc PR A 3
H45C H 0.7257 0.3112 -0.0613 0.1 Uiso 0.556(14) 1 calc PR A 3
C46 C 0.8580(11) 0.2008(13) -0.0175(8) 0.157(10) Uiso 0.556(14) 1 d PD A 3
H46A H 0.8284 0.1615 -0.0451 0.236 Uiso 0.556(14) 1 calc PR A 3
H46B H 0.9047 0.1746 0.0118 0.236 Uiso 0.556(14) 1 calc PR A 3
H46C H 0.8901 0.2411 -0.0352 0.236 Uiso 0.556(14) 1 calc PR A 3
C47 C 0.7366(13) 0.1751(8) 0.0391(5) 0.105(7) Uiso 0.556(14) 1 d PD A 3
H47A H 0.7819 0.1572 0.0728 0.127 Uiso 0.556(14) 1 calc PR A 3
H47B H 0.677 0.1936 0.0486 0.127 Uiso 0.556(14) 1 calc PR A 3
C48 C 0.721(3) 0.0301(14) 0.0215(14) 0.238(17) Uiso 0.556(14) 1 d PD A 3
H48A H 0.7104 -0.011 -0.007 0.356 Uiso 0.556(14) 1 calc PR A 3
H48B H 0.6717 0.0269 0.0428 0.356 Uiso 0.556(14) 1 calc PR A 3
H48C H 0.7838 0.0223 0.0461 0.356 Uiso 0.556(14) 1 calc PR A 3
O5A O 0.7846(14) 0.1061(10) -0.0197(6) 0.115(7) Uiso 0.444(14) 1 d PD A 4
C45A C 0.6745(7) 0.2525(11) -0.0179(8) 0.072(6) Uiso 0.444(14) 1 d PD A 4
H45D H 0.6646 0.3056 -0.034 0.108 Uiso 0.444(14) 1 calc PR A 4
H45E H 0.6384 0.247 0.011 0.108 Uiso 0.444(14) 1 calc PR A 4
H45F H 0.6526 0.2129 -0.0467 0.108 Uiso 0.444(14) 1 calc PR A 4
C46A C 0.8366(12) 0.2496(12) -0.0413(7) 0.088(7) Uiso 0.444(14) 1 d PD A 4
H46D H 0.8267 0.3032 -0.0565 0.133 Uiso 0.444(14) 1 calc PR A 4
H46E H 0.8123 0.2109 -0.0703 0.133 Uiso 0.444(14) 1 calc PR A 4
H46F H 0.9048 0.2406 -0.0267 0.133 Uiso 0.444(14) 1 calc PR A 4
C47A C 0.8023(14) 0.1575(7) 0.0311(6) 0.084(7) Uiso 0.444(14) 1 d PD A 4
H47C H 0.869 0.153 0.0521 0.101 Uiso 0.444(14) 1 calc PR A 4
H47D H 0.759 0.1434 0.0554 0.101 Uiso 0.444(14) 1 calc PR A 4
C48A C 0.822(5) 0.024(2) -0.002(3) 0.36(4) Uiso 0.444(14) 1 d PD A 4
H48D H 0.8095 -0.0115 -0.0338 0.539 Uiso 0.444(14) 1 calc PR A 4
H48E H 0.7895 0.0038 0.0261 0.539 Uiso 0.444(14) 1 calc PR A 4
H48F H 0.8905 0.0266 0.0137 0.539 Uiso 0.444(14) 1 calc PR A 4

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
C1 0.038(4) 0.040(4) 0.060(5) 0.005(4) 0.012(4) -0.001(3)
C2 0.038(4) 0.072(6) 0.069(5) -0.005(4) 0.013(4) 0.007(4)
C3 0.063(5) 0.054(5) 0.058(5) -0.004(4) 0.028(5) 0.001(4)
C4 0.035(4) 0.053(5) 0.061(5) 0.001(4) 0.006(4) -0.002(4)
C5 0.048(5) 0.105(7) 0.079(6) -0.011(5) 0.008(4) -0.029(5)
C6 0.056(5) 0.083(6) 0.080(6) 0.006(5) 0.007(4) 0.024(5)
C7 0.044(4) 0.047(5) 0.065(5) 0.001(4) -0.003(4) -0.015(4)
C8 0.053(5) 0.081(6) 0.053(5) 0.007(4) -0.005(4) -0.007(4)
C9 0.029(4) 0.031(4) 0.059(5) -0.009(4) 0.004(3) 0.003(3)
C10 0.045(4) 0.045(4) 0.063(5) -0.009(4) 0.006(4) -0.006(4)
C11 0.040(4) 0.057(5) 0.045(4) -0.012(4) -0.004(4) 0.002(4)
C12 0.046(4) 0.031(4) 0.063(5) -0.004(4) 0.014(4) -0.001(3)
C13 0.099(7) 0.042(5) 0.084(6) 0.004(4) 0.015(5) 0.000(4)
C14 0.047(5) 0.075(6) 0.075(6) 0.000(5) 0.020(4) -0.008(4)
C15 0.049(4) 0.045(5) 0.062(5) 0.003(4) 0.014(4) -0.004(4)
C16 0.044(4) 0.065(5) 0.049(5) 0.011(4) 0.003(4) 0.005(4)
C17 0.036(4) 0.036(4) 0.051(5) 0.007(4) 0.006(3) 0.000(3)
C18 0.069(5) 0.050(5) 0.054(5) 0.014(4) 0.009(4) 0.016(4)
C19 0.067(5) 0.057(5) 0.042(4) 0.014(4) 0.003(4) 0.003(4)
C20 0.042(4) 0.036(4) 0.061(5) 0.005(4) 0.013(4) 0.001(3)
C21 0.094(6) 0.052(5) 0.095(7) -0.011(5) 0.036(5) -0.018(5)
C22 0.074(6) 0.067(6) 0.080(6) 0.010(5) 0.018(5) 0.026(5)
C23 0.042(4) 0.041(4) 0.048(4) 0.000(4) 0.009(3) 0.001(3)
C24 0.073(6) 0.088(6) 0.047(5) -0.014(4) -0.005(4) 0.027(5)
B1 0.054(5) 0.055(6) 0.031(4) 0.003(4) 0.001(4) 0.000(4)
Ca 0.0377(8) 0.0354(8) 0.0387(8) -0.0006(7) 0.0021(6) -0.0013(6)
N1 0.045(3) 0.045(3) 0.042(3) -0.001(3) 0.009(3) -0.002(3)
N2 0.038(3) 0.045(3) 0.044(4) 0.004(3) 0.007(3) -0.004(3)
N3 0.040(3) 0.047(4) 0.035(3) -0.003(3) 0.005(3) -0.001(3)
N4 0.040(3) 0.039(3) 0.041(4) -0.005(3) 0.007(3) -0.003(3)
N5 0.046(3) 0.042(4) 0.042(4) 0.009(3) 0.002(3) 0.003(3)
N6 0.041(3) 0.042(4) 0.035(3) 0.001(3) 0.006(3) 0.000(3)
O1 0.042(3) 0.059(3) 0.040(3) -0.003(2) -0.005(2) -0.004(2)
O2 0.052(3) 0.043(3) 0.041(3) 0.003(2) 0.007(2) -0.005(2)
O3 0.055(3) 0.049(3) 0.040(3) -0.007(2) 0.000(2) 0.010(2)
C25 0.044(4) 0.043(4) 0.060(5) -0.015(4) 0.007(4) 0.004(4)
C26 0.043(4) 0.048(5) 0.073(6) -0.017(4) 0.004(4) -0.009(4)
C27 0.048(4) 0.042(5) 0.071(6) 0.000(4) 0.010(4) -0.007(4)
C28 0.050(4) 0.060(5) 0.045(5) -0.016(4) 0.002(3) 0.003(4)
C29 0.067(6) 0.124(8) 0.072(6) 0.010(6) 0.023(5) 0.027(5)
C30 0.116(8) 0.109(8) 0.058(6) -0.029(5) -0.001(5) -0.026(6)
C31 0.071(6) 0.091(7) 0.064(6) 0.016(5) 0.011(5) 0.021(5)
C32 0.204(14) 0.129(11) 0.137(10) 0.051(9) 0.077(10) 0.109(10)
C33 0.044(4) 0.043(4) 0.040(4) 0.007(3) 0.003(3) -0.003(4)
C34 0.047(5) 0.061(5) 0.058(5) 0.007(4) 0.019(4) 0.003(4)
C35 0.047(4) 0.051(5) 0.061(5) 0.009(4) 0.018(4) 0.011(4)
C36 0.061(5) 0.043(5) 0.065(5) 0.017(4) 0.011(4) 0.000(4)
C37 0.073(6) 0.075(6) 0.085(6) 0.023(5) 0.016(5) 0.004(5)
C38 0.191(12) 0.060(6) 0.109(8) 0.004(6) 0.023(8) 0.001(7)
C39 0.089(7) 0.054(6) 0.173(10) 0.062(6) 0.043(7) 0.029(5)
O6 0.143(7) 0.107(6) 0.137(7) 0.024(5) 0.026(5) 0.019(5)
C40 0.156(13) 0.167(14) 0.31(2) 0.097(14) 0.101(14) 0.087(12)
C41 0.042(4) 0.042(5) 0.051(5) -0.006(4) -0.001(4) 0.003(3)
C42 0.046(4) 0.041(5) 0.066(5) -0.001(4) -0.001(4) 0.013(3)
C43 0.038(4) 0.038(4) 0.054(4) -0.006(4) 0.000(3) -0.001(3)
C44 0.054(5) 0.056(5) 0.074(5) -0.021(4) -0.002(4) 0.008(4)
B2 0.033(4) 0.037(5) 0.050(5) -0.002(4) 0.002(4) 0.002(4)
N7 0.040(3) 0.032(3) 0.051(4) -0.002(3) 0.004(3) -0.001(3)
N8 0.044(3) 0.045(3) 0.043(3) -0.010(3) 0.005(3) -0.004(3)
N9 0.040(3) 0.031(3) 0.049(3) 0.002(3) 0.007(3) 0.004(3)
N10 0.041(3) 0.037(3) 0.048(3) 0.004(3) 0.003(3) 0.005(3)
N11 0.038(3) 0.036(3) 0.042(3) -0.002(3) 0.001(3) 0.002(3)
N12 0.041(3) 0.036(4) 0.054(4) -0.011(3) -0.003(3) 0.009(3)
O4 0.094(5) 0.120(6) 0.117(5) 0.029(4) 0.036(4) 0.055(4)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.334(8) . ?
C1 C2 1.390(10) . ?
C1 C4 1.523(9) . ?
C2 C3 1.351(10) . ?
C2 H2 0.94 . ?
C3 N1 1.341(8) . ?
C3 H3 0.94 . ?
C4 C7 1.492(10) . ?
C4 C5 1.513(10) . ?
C4 C6 1.548(10) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C5 H5C 0.97 . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C6 H6C 0.97 . ?
C7 O1 1.439(8) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C8 O1 1.448(8) . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C8 H8C 0.97 . ?
C9 N4 1.352(8) . ?
C9 C10 1.386(9) . ?
C9 C12 1.492(9) . ?
C10 C11 1.365(9) . ?
C10 H10 0.94 . ?
C11 N3 1.340(8) . ?
C11 H11 0.94 . ?
C12 C14 1.520(9) . ?
C12 C13 1.531(10) . ?
C12 C15 1.540(9) . ?
C13 H13A 0.97 . ?
C13 H13B 0.97 . ?
C13 H13C 0.97 . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C14 H14C 0.97 . ?
C15 O2 1.438(8) . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C16 O2 1.449(8) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C16 H16C 0.97 . ?
C17 N6 1.345(8) . ?
C17 C18 1.375(9) . ?
C17 C20 1.517(9) . ?
C18 C19 1.380(10) . ?
C18 H18 0.94 . ?
C19 N5 1.336(8) . ?
C19 H19 0.94 . ?
C20 C23 1.511(9) . ?
C20 C21 1.534(10) . ?
C20 C22 1.539(9) . ?
C21 H21A 0.97 . ?
C21 H21B 0.97 . ?
C21 H21C 0.97 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 H22C 0.97 . ?
C23 O3 1.466(7) . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C24 O3 1.416(8) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 H24C 0.97 . ?
B1 N3 1.534(9) . ?
B1 N5 1.543(10) . ?
B1 N1 1.547(9) . ?
B1 H1 0.99 . ?
Ca O3 2.346(4) . ?
Ca O2 2.369(4) . ?
Ca O1 2.380(4) . ?
Ca N4 2.423(5) . ?
Ca N6 2.434(5) . ?
Ca N2 2.436(5) . ?
N1 N2 1.369(7) . ?
N3 N4 1.370(7) . ?
N5 N6 1.376(7) . ?
C25 N8 1.342(8) . ?
C25 C26 1.394(10) . ?
C25 C28 1.512(10) . ?
C26 C27 1.376(10) . ?
C26 H26 0.94 . ?
C27 N7 1.342(8) . ?
C27 H27 0.94 . ?
C28 C31 1.500(11) . ?
C28 C29 1.526(10) . ?
C28 C30 1.536(10) . ?
C29 H29A 0.97 . ?
C29 H29B 0.97 . ?
C29 H29C 0.97 . ?
C30 H30A 0.97 . ?
C30 H30B 0.97 . ?
C30 H30C 0.97 . ?
C31 O4 1.392(9) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C32 O4 1.441(12) . ?
C32 H32A 0.97 . ?
C32 H32B 0.97 . ?
C32 H32C 0.97 . ?
C33 N10 1.343(8) . ?
C33 C34 1.382(9) . ?
C33 C36 1.483(9) . ?
C34 C35 1.369(9) . ?
C34 H34 0.94 . ?
C35 N9 1.353(8) . ?
C35 H35 0.94 . ?
C36 C39 1.523(11) . ?
C36 C38 1.531(12) . ?
C36 C37 1.534(10) . ?
C37 H37A 0.97 . ?
C37 H37B 0.97 . ?
C37 H37C 0.97 . ?
C38 H38A 0.97 . ?
C38 H38B 0.97 . ?
C38 H38C 0.97 . ?
C39 O6 1.464(10) . ?
C39 H39A 0.98 . ?
C39 H39B 0.98 . ?
O6 C40 1.499(14) . ?
C40 H40A 0.97 . ?
C40 H40B 0.97 . ?
C40 H40C 0.97 . ?
C41 N12 1.317(8) . ?
C41 C42 1.410(9) . ?
C41 C44 1.513(9) . ?
C42 C43 1.354(9) . ?
C42 H42 0.94 . ?
C43 N11 1.347(8) . ?
C43 H43 0.94 . ?
C44 C47A 1.504(8) . ?
C44 C46 1.516(9) . ?
C44 C45A 1.524(8) . ?
C44 C45 1.536(8) . ?
C44 C47 1.556(8) . ?
C44 C46A 1.578(8) . ?
B2 N9 1.524(9) . ?
B2 N7 1.552(9) . ?
B2 N11 1.552(9) . ?
B2 H2A 0.99 . ?
N7 N8 1.357(7) . ?
N9 N10 1.359(7) . ?
N11 N12 1.363(7) . ?
O5 C48 1.498(10) . ?
O5 C47 1.517(9) . ?
C45 H45A 0.97 . ?
C45 H45B 0.97 . ?
C45 H45C 0.97 . ?
C46 H46A 0.97 . ?
C46 H46B 0.97 . ?
C46 H46C 0.97 . ?
C47 H47A 0.98 . ?
C47 H47B 0.98 . ?
C48 H48A 0.97 . ?
C48 H48B 0.97 . ?
C48 H48C 0.97 . ?
O5A C47A 1.492(10) . ?
O5A C48A 1.503(10) . ?
C45A H45D 0.97 . ?
C45A H45E 0.97 . ?
C45A H45F 0.97 . ?
C46A H46D 0.97 . ?
C46A H46E 0.97 . ?
C46A H46F 0.97 . ?
C47A H47C 0.98 . ?
C47A H47D 0.98 . ?
C48A H48D 0.97 . ?
C48A H48E 0.97 . ?
C48A H48F 0.97 . ?

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 C1 C2 110.1(6) . . ?
N2 C1 C4 121.5(6) . . ?
C2 C1 C4 128.4(6) . . ?
C3 C2 C1 105.5(6) . . ?
C3 C2 H2 127.2 . . ?
C1 C2 H2 127.2 . . ?
N1 C3 C2 108.9(7) . . ?
N1 C3 H3 125.5 . . ?
C2 C3 H3 125.5 . . ?
C7 C4 C5 107.0(6) . . ?
C7 C4 C1 111.5(6) . . ?
C5 C4 C1 109.5(6) . . ?
C7 C4 C6 111.4(6) . . ?
C5 C4 C6 109.5(6) . . ?
C1 C4 C6 108.0(6) . . ?
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 . . ?
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 . . ?
O1 C7 C4 116.4(6) . . ?
O1 C7 H7A 108.2 . . ?
C4 C7 H7A 108.2 . . ?
O1 C7 H7B 108.2 . . ?
C4 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 108.9(6) . . ?
N4 C9 C12 121.4(6) . . ?
C10 C9 C12 129.6(6) . . ?
C11 C10 C9 106.6(6) . . ?
C11 C10 H10 126.7 . . ?
C9 C10 H10 126.7 . . ?
N3 C11 C10 108.4(6) . . ?
N3 C11 H11 125.8 . . ?
C10 C11 H11 125.8 . . ?
C9 C12 C14 109.9(6) . . ?
C9 C12 C13 108.8(6) . . ?
C14 C12 C13 109.6(6) . . ?
C9 C12 C15 112.3(5) . . ?
C14 C12 C15 110.8(6) . . ?
C13 C12 C15 105.3(6) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 C12 113.5(5) . . ?
O2 C15 H15A 108.9 . . ?
C12 C15 H15A 108.9 . . ?
O2 C15 H15B 108.9 . . ?
C12 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
O2 C16 H16A 109.5 . . ?
O2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 C18 110.0(6) . . ?
N6 C17 C20 121.0(6) . . ?
C18 C17 C20 129.0(6) . . ?
C17 C18 C19 106.0(6) . . ?
C17 C18 H18 127 . . ?
C19 C18 H18 127 . . ?
N5 C19 C18 108.2(6) . . ?
N5 C19 H19 125.9 . . ?
C18 C19 H19 125.9 . . ?
C23 C20 C17 111.4(5) . . ?
C23 C20 C21 112.0(6) . . ?
C17 C20 C21 107.9(6) . . ?
C23 C20 C22 105.5(6) . . ?
C17 C20 C22 109.4(6) . . ?
C21 C20 C22 110.6(6) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 C20 113.6(5) . . ?
O3 C23 H23A 108.9 . . ?
C20 C23 H23A 108.9 . . ?
O3 C23 H23B 108.9 . . ?
C20 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 B1 N5 110.4(6) . . ?
N3 B1 N1 110.0(5) . . ?
N5 B1 N1 111.2(6) . . ?
N3 B1 H1 108.4 . . ?
N5 B1 H1 108.4 . . ?
N1 B1 H1 108.4 . . ?
O3 Ca O2 98.91(16) . . ?
O3 Ca O1 90.86(15) . . ?
O2 Ca O1 87.54(15) . . ?
O3 Ca N4 135.72(17) . . ?
O2 Ca N4 75.74(17) . . ?
O1 Ca N4 131.88(17) . . ?
O3 Ca N6 74.78(17) . . ?
O2 Ca N6 141.21(16) . . ?
O1 Ca N6 130.09(17) . . ?
N4 Ca N6 82.70(18) . . ?
O3 Ca N2 131.01(18) . . ?
O2 Ca N2 126.51(17) . . ?
O1 Ca N2 75.56(17) . . ?
N4 Ca N2 79.10(18) . . ?
N6 Ca N2 78.99(18) . . ?
C3 N1 N2 109.3(5) . . ?
C3 N1 B1 128.1(6) . . ?
N2 N1 B1 122.5(5) . . ?
C1 N2 N1 106.1(5) . . ?
C1 N2 Ca 135.9(4) . . ?
N1 N2 Ca 117.1(4) . . ?
C11 N3 N4 109.6(5) . . ?
C11 N3 B1 127.8(6) . . ?
N4 N3 B1 122.7(5) . . ?
C9 N4 N3 106.6(5) . . ?
C9 N4 Ca 134.8(4) . . ?
N3 N4 Ca 117.0(4) . . ?
C19 N5 N6 109.6(6) . . ?
C19 N5 B1 127.3(6) . . ?
N6 N5 B1 123.2(5) . . ?
C17 N6 N5 106.2(5) . . ?
C17 N6 Ca 137.0(4) . . ?
N5 N6 Ca 116.8(4) . . ?
C7 O1 C8 112.9(5) . . ?
C7 O1 Ca 117.5(4) . . ?
C8 O1 Ca 129.4(4) . . ?
C15 O2 C16 111.9(5) . . ?
C15 O2 Ca 121.5(4) . . ?
C16 O2 Ca 126.6(4) . . ?
C24 O3 C23 113.3(5) . . ?
C24 O3 Ca 125.5(4) . . ?
C23 O3 Ca 120.3(3) . . ?
N8 C25 C26 109.9(6) . . ?
N8 C25 C28 119.1(6) . . ?
C26 C25 C28 131.0(7) . . ?
C27 C26 C25 105.6(6) . . ?
C27 C26 H26 127.2 . . ?
C25 C26 H26 127.2 . . ?
N7 C27 C26 107.6(7) . . ?
N7 C27 H27 126.2 . . ?
C26 C27 H27 126.2 . . ?
C31 C28 C25 109.2(6) . . ?
C31 C28 C29 107.6(7) . . ?
C25 C28 C29 109.8(6) . . ?
C31 C28 C30 110.9(7) . . ?
C25 C28 C30 110.2(6) . . ?
C29 C28 C30 109.2(7) . . ?
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 . . ?
O4 C31 C28 111.2(7) . . ?
O4 C31 H31A 109.4 . . ?
C28 C31 H31A 109.4 . . ?
O4 C31 H31B 109.4 . . ?
C28 C31 H31B 109.4 . . ?
H31A C31 H31B 108 . . ?
O4 C32 H32A 109.5 . . ?
O4 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O4 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N10 C33 C34 109.7(6) . . ?
N10 C33 C36 118.8(6) . . ?
C34 C33 C36 131.4(7) . . ?
C35 C34 C33 105.9(6) . . ?
C35 C34 H34 127 . . ?
C33 C34 H34 127 . . ?
N9 C35 C34 108.1(6) . . ?
N9 C35 H35 125.9 . . ?
C34 C35 H35 125.9 . . ?
C33 C36 C39 109.6(6) . . ?
C33 C36 C38 109.9(6) . . ?
C39 C36 C38 107.1(8) . . ?
C33 C36 C37 111.2(7) . . ?
C39 C36 C37 110.5(7) . . ?
C38 C36 C37 108.4(7) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O6 C39 C36 109.2(7) . . ?
O6 C39 H39A 109.8 . . ?
C36 C39 H39A 109.8 . . ?
O6 C39 H39B 109.8 . . ?
C36 C39 H39B 109.8 . . ?
H39A C39 H39B 108.3 . . ?
C39 O6 C40 112.6(9) . . ?
O6 C40 H40A 109.5 . . ?
O6 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O6 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N12 C41 C42 110.2(6) . . ?
N12 C41 C44 121.2(6) . . ?
C42 C41 C44 128.6(6) . . ?
C43 C42 C41 105.1(6) . . ?
C43 C42 H42 127.4 . . ?
C41 C42 H42 127.4 . . ?
N11 C43 C42 108.3(6) . . ?
N11 C43 H43 125.9 . . ?
C42 C43 H43 125.9 . . ?
C47A C44 C41 110.3(7) . . ?
C41 C44 C46 112.9(10) . . ?
C47A C44 C45A 112.2(7) . . ?
C41 C44 C45A 112.4(8) . . ?
C41 C44 C45 112.3(7) . . ?
C46 C44 C45 110.8(7) . . ?
C41 C44 C47 105.0(7) . . ?
C46 C44 C47 108.2(7) . . ?
C45 C44 C47 107.2(7) . . ?
C47A C44 C46A 107.4(7) . . ?
C41 C44 C46A 106.8(9) . . ?
C45A C44 C46A 107.5(7) . . ?
N9 B2 N7 107.8(5) . . ?
N9 B2 N11 109.9(5) . . ?
N7 B2 N11 108.7(5) . . ?
N9 B2 H2A 110.1 . . ?
N7 B2 H2A 110.1 . . ?
N11 B2 H2A 110.1 . . ?
C27 N7 N8 110.8(5) . . ?
C27 N7 B2 128.4(6) . . ?
N8 N7 B2 120.7(5) . . ?
C25 N8 N7 106.1(5) . . ?
C35 N9 N10 109.3(5) . . ?
C35 N9 B2 129.5(6) . . ?
N10 N9 B2 120.3(5) . . ?
C33 N10 N9 106.9(5) . . ?
C43 N11 N12 110.0(5) . . ?
C43 N11 B2 130.4(5) . . ?
N12 N11 B2 119.5(5) . . ?
C41 N12 N11 106.4(5) . . ?
C31 O4 C32 111.4(9) . . ?
C48 O5 C47 109.6(17) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.4 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O5 C47 C44 99.1(9) . . ?
O5 C47 H47A 112 . . ?
C44 C47 H47A 112 . . ?
O5 C47 H47B 111.9 . . ?
C44 C47 H47B 111.9 . . ?
H47A C47 H47B 109.6 . . ?
O5 C48 H48A 109.5 . . ?
O5 C48 H48B 109.4 . . ?
H48A C48 H48B 109.5 . . ?
O5 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47A O5A C48A 107(3) . . ?
C44 C45A H45D 109.4 . . ?
C44 C45A H45E 109.5 . . ?
H45D C45A H45E 109.5 . . ?
C44 C45A H45F 109.5 . . ?
H45D C45A H45F 109.5 . . ?
H45E C45A H45F 109.5 . . ?
C44 C46A H46D 109.5 . . ?
C44 C46A H46E 109.5 . . ?
H46D C46A H46E 109.5 . . ?
C44 C46A H46F 109.4 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?
O5A C47A C44 102.7(10) . . ?
O5A C47A H47C 111.3 . . ?
C44 C47A H47C 111.3 . . ?
O5A C47A H47D 111.2 . . ?
C44 C47A H47D 111.2 . . ?
H47C C47A H47D 109.1 . . ?
O5A C48A H48D 109.5 . . ?
O5A C48A H48E 109.3 . . ?
H48D C48A H48E 109.5 . . ?
O5A C48A H48F 109.6 . . ?
H48D C48A H48F 109.5 . . ?
H48E C48A H48F 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
N2 C1 C2 C3 -1.4(8) . . . . ?
C4 C1 C2 C3 179.5(7) . . . . ?
C1 C2 C3 N1 1.1(8) . . . . ?
N2 C1 C4 C7 23.7(9) . . . . ?
C2 C1 C4 C7 -157.3(7) . . . . ?
N2 C1 C4 C5 141.8(7) . . . . ?
C2 C1 C4 C5 -39.1(10) . . . . ?
N2 C1 C4 C6 -99.0(7) . . . . ?
C2 C1 C4 C6 80.1(9) . . . . ?
C5 C4 C7 O1 168.1(6) . . . . ?
C1 C4 C7 O1 -72.2(7) . . . . ?
C6 C4 C7 O1 48.5(8) . . . . ?
N4 C9 C10 C11 -1.0(7) . . . . ?
C12 C9 C10 C11 -178.9(6) . . . . ?
C9 C10 C11 N3 0.5(7) . . . . ?
N4 C9 C12 C14 -95.7(7) . . . . ?
C10 C9 C12 C14 81.9(8) . . . . ?
N4 C9 C12 C13 144.3(6) . . . . ?
C10 C9 C12 C13 -38.1(9) . . . . ?
N4 C9 C12 C15 28.2(8) . . . . ?
C10 C9 C12 C15 -154.2(6) . . . . ?
C9 C12 C15 O2 -72.8(7) . . . . ?
C14 C12 C15 O2 50.6(8) . . . . ?
C13 C12 C15 O2 169.0(6) . . . . ?
N6 C17 C18 C19 -0.5(8) . . . . ?
C20 C17 C18 C19 -179.6(6) . . . . ?
C17 C18 C19 N5 0.3(8) . . . . ?
N6 C17 C20 C23 32.2(8) . . . . ?
C18 C17 C20 C23 -148.9(7) . . . . ?
N6 C17 C20 C21 -91.2(7) . . . . ?
C18 C17 C20 C21 87.8(8) . . . . ?
N6 C17 C20 C22 148.5(6) . . . . ?
C18 C17 C20 C22 -32.6(9) . . . . ?
C17 C20 C23 O3 -72.2(7) . . . . ?
C21 C20 C23 O3 48.8(8) . . . . ?
C22 C20 C23 O3 169.2(5) . . . . ?
C2 C3 N1 N2 -0.5(8) . . . . ?
C2 C3 N1 B1 179.2(7) . . . . ?
N3 B1 N1 C3 -112.0(7) . . . . ?
N5 B1 N1 C3 125.3(7) . . . . ?
N3 B1 N1 N2 67.6(8) . . . . ?
N5 B1 N1 N2 -55.1(8) . . . . ?
C2 C1 N2 N1 1.1(7) . . . . ?
C4 C1 N2 N1 -179.7(6) . . . . ?
C2 C1 N2 Ca -167.3(5) . . . . ?
C4 C1 N2 Ca 12.0(10) . . . . ?
C3 N1 N2 C1 -0.4(7) . . . . ?
B1 N1 N2 C1 180.0(6) . . . . ?
C3 N1 N2 Ca 170.5(4) . . . . ?
B1 N1 N2 Ca -9.1(7) . . . . ?
O3 Ca N2 C1 -86.8(6) . . . . ?
O2 Ca N2 C1 67.2(7) . . . . ?
O1 Ca N2 C1 -8.6(6) . . . . ?
N4 Ca N2 C1 130.1(6) . . . . ?
N6 Ca N2 C1 -145.3(6) . . . . ?
O3 Ca N2 N1 105.8(4) . . . . ?
O2 Ca N2 N1 -100.2(4) . . . . ?
O1 Ca N2 N1 -176.0(4) . . . . ?
N4 Ca N2 N1 -37.3(4) . . . . ?
N6 Ca N2 N1 47.3(4) . . . . ?
C10 C11 N3 N4 0.2(7) . . . . ?
C10 C11 N3 B1 179.7(6) . . . . ?
N5 B1 N3 C11 -109.8(7) . . . . ?
N1 B1 N3 C11 127.1(7) . . . . ?
N5 B1 N3 N4 69.7(7) . . . . ?
N1 B1 N3 N4 -53.4(8) . . . . ?
C10 C9 N4 N3 1.1(6) . . . . ?
C12 C9 N4 N3 179.2(5) . . . . ?
C10 C9 N4 Ca -163.5(4) . . . . ?
C12 C9 N4 Ca 14.6(9) . . . . ?
C11 N3 N4 C9 -0.8(6) . . . . ?
B1 N3 N4 C9 179.6(5) . . . . ?
C11 N3 N4 Ca 167.0(4) . . . . ?
B1 N3 N4 Ca -12.6(7) . . . . ?
O3 Ca N4 C9 72.4(6) . . . . ?
O2 Ca N4 C9 -15.8(5) . . . . ?
O1 Ca N4 C9 -89.1(6) . . . . ?
N6 Ca N4 C9 131.7(6) . . . . ?
N2 Ca N4 C9 -148.2(6) . . . . ?
O3 Ca N4 N3 -91.0(4) . . . . ?
O2 Ca N4 N3 -179.2(4) . . . . ?
O1 Ca N4 N3 107.5(4) . . . . ?
N6 Ca N4 N3 -31.7(4) . . . . ?
N2 Ca N4 N3 48.4(4) . . . . ?
C18 C19 N5 N6 0.0(8) . . . . ?
C18 C19 N5 B1 -179.9(6) . . . . ?
N3 B1 N5 C19 119.0(7) . . . . ?
N1 B1 N5 C19 -118.6(7) . . . . ?
N3 B1 N5 N6 -60.9(8) . . . . ?
N1 B1 N5 N6 61.5(8) . . . . ?
C18 C17 N6 N5 0.5(7) . . . . ?
C20 C17 N6 N5 179.6(5) . . . . ?
C18 C17 N6 Ca -179.4(5) . . . . ?
C20 C17 N6 Ca -0.2(9) . . . . ?
C19 N5 N6 C17 -0.3(7) . . . . ?
B1 N5 N6 C17 179.6(6) . . . . ?
C19 N5 N6 Ca 179.6(4) . . . . ?
B1 N5 N6 Ca -0.5(7) . . . . ?
O3 Ca N6 C17 -0.6(6) . . . . ?
O2 Ca N6 C17 -85.9(6) . . . . ?
O1 Ca N6 C17 77.3(6) . . . . ?
N4 Ca N6 C17 -142.1(6) . . . . ?
N2 Ca N6 C17 137.6(6) . . . . ?
O3 Ca N6 N5 179.5(4) . . . . ?
O2 Ca N6 N5 94.2(4) . . . . ?
O1 Ca N6 N5 -102.5(4) . . . . ?
N4 Ca N6 N5 38.0(4) . . . . ?
N2 Ca N6 N5 -42.3(4) . . . . ?
C4 C7 O1 C8 -105.6(7) . . . . ?
C4 C7 O1 Ca 77.6(6) . . . . ?
O3 Ca O1 C7 101.4(4) . . . . ?
O2 Ca O1 C7 -159.7(4) . . . . ?
N4 Ca O1 C7 -91.4(5) . . . . ?
N6 Ca O1 C7 30.7(5) . . . . ?
N2 Ca O1 C7 -31.0(4) . . . . ?
O3 Ca O1 C8 -74.7(5) . . . . ?
O2 Ca O1 C8 24.2(5) . . . . ?
N4 Ca O1 C8 92.5(6) . . . . ?
N6 Ca O1 C8 -145.4(5) . . . . ?
N2 Ca O1 C8 152.9(6) . . . . ?
C12 C15 O2 C16 -108.7(6) . . . . ?
C12 C15 O2 Ca 71.3(6) . . . . ?
O3 Ca O2 C15 -160.9(4) . . . . ?
O1 Ca O2 C15 108.6(4) . . . . ?
N4 Ca O2 C15 -25.8(4) . . . . ?
N6 Ca O2 C15 -84.1(5) . . . . ?
N2 Ca O2 C15 38.7(5) . . . . ?
O3 Ca O2 C16 19.1(5) . . . . ?
O1 Ca O2 C16 -71.4(4) . . . . ?
N4 Ca O2 C16 154.2(5) . . . . ?
N6 Ca O2 C16 95.9(5) . . . . ?
N2 Ca O2 C16 -141.4(4) . . . . ?
C20 C23 O3 C24 -112.5(7) . . . . ?
C20 C23 O3 Ca 77.4(6) . . . . ?
O2 Ca O3 C24 -62.1(6) . . . . ?
O1 Ca O3 C24 25.5(6) . . . . ?
N4 Ca O3 C24 -140.8(5) . . . . ?
N6 Ca O3 C24 157.1(6) . . . . ?
N2 Ca O3 C24 97.0(6) . . . . ?
O2 Ca O3 C23 106.7(4) . . . . ?
O1 Ca O3 C23 -165.7(4) . . . . ?
N4 Ca O3 C23 28.0(5) . . . . ?
N6 Ca O3 C23 -34.1(4) . . . . ?
N2 Ca O3 C23 -94.2(4) . . . . ?
N8 C25 C26 C27 -1.0(8) . . . . ?
C28 C25 C26 C27 179.1(7) . . . . ?
C25 C26 C27 N7 0.4(8) . . . . ?
N8 C25 C28 C31 61.4(8) . . . . ?
C26 C25 C28 C31 -118.8(8) . . . . ?
N8 C25 C28 C29 -56.3(9) . . . . ?
C26 C25 C28 C29 123.6(8) . . . . ?
N8 C25 C28 C30 -176.6(7) . . . . ?
C26 C25 C28 C30 3.3(11) . . . . ?
C25 C28 C31 O4 60.3(8) . . . . ?
C29 C28 C31 O4 179.3(7) . . . . ?
C30 C28 C31 O4 -61.3(9) . . . . ?
N10 C33 C34 C35 -0.5(8) . . . . ?
C36 C33 C34 C35 177.5(7) . . . . ?
C33 C34 C35 N9 0.5(8) . . . . ?
N10 C33 C36 C39 -39.2(9) . . . . ?
C34 C33 C36 C39 143.0(8) . . . . ?
N10 C33 C36 C38 78.3(9) . . . . ?
C34 C33 C36 C38 -99.6(10) . . . . ?
N10 C33 C36 C37 -161.7(6) . . . . ?
C34 C33 C36 C37 20.5(11) . . . . ?
C33 C36 C39 O6 168.4(7) . . . . ?
C38 C36 C39 O6 49.3(10) . . . . ?
C37 C36 C39 O6 -68.7(10) . . . . ?
C36 C39 O6 C40 -163.8(10) . . . . ?
N12 C41 C42 C43 0.4(8) . . . . ?
C44 C41 C42 C43 178.6(7) . . . . ?
C41 C42 C43 N11 -0.1(8) . . . . ?
N12 C41 C44 C47A -158.0(10) . . . . ?
C42 C41 C44 C47A 24.0(12) . . . . ?
N12 C41 C44 C46 125.8(10) . . . . ?
C42 C41 C44 C46 -52.3(12) . . . . ?
N12 C41 C44 C45A -32.0(11) . . . . ?
C42 C41 C44 C45A 150.0(10) . . . . ?
N12 C41 C44 C45 -0.4(11) . . . . ?
C42 C41 C44 C45 -178.4(9) . . . . ?
N12 C41 C44 C47 -116.5(9) . . . . ?
C42 C41 C44 C47 65.4(11) . . . . ?
N12 C41 C44 C46A 85.7(10) . . . . ?
C42 C41 C44 C46A -92.4(10) . . . . ?
C26 C27 N7 N8 0.4(7) . . . . ?
C26 C27 N7 B2 176.7(6) . . . . ?
N9 B2 N7 C27 -2.8(9) . . . . ?
N11 B2 N7 C27 116.3(7) . . . . ?
N9 B2 N7 N8 173.2(5) . . . . ?
N11 B2 N7 N8 -67.7(7) . . . . ?
C26 C25 N8 N7 1.3(7) . . . . ?
C28 C25 N8 N7 -178.9(5) . . . . ?
C27 N7 N8 C25 -1.0(7) . . . . ?
B2 N7 N8 C25 -177.6(5) . . . . ?
C34 C35 N9 N10 -0.4(7) . . . . ?
C34 C35 N9 B2 -169.0(6) . . . . ?
N7 B2 N9 C35 85.3(8) . . . . ?
N11 B2 N9 C35 -33.0(9) . . . . ?
N7 B2 N9 N10 -82.3(6) . . . . ?
N11 B2 N9 N10 159.4(5) . . . . ?
C34 C33 N10 N9 0.3(7) . . . . ?
C36 C33 N10 N9 -178.0(5) . . . . ?
C35 N9 N10 C33 0.0(7) . . . . ?
B2 N9 N10 C33 169.9(5) . . . . ?
C42 C43 N11 N12 -0.2(7) . . . . ?
C42 C43 N11 B2 176.0(6) . . . . ?
N9 B2 N11 C43 115.7(7) . . . . ?
N7 B2 N11 C43 -2.0(9) . . . . ?
N9 B2 N11 N12 -68.4(7) . . . . ?
N7 B2 N11 N12 173.8(5) . . . . ?
C42 C41 N12 N11 -0.5(8) . . . . ?
C44 C41 N12 N11 -178.9(6) . . . . ?
C43 N11 N12 C41 0.4(7) . . . . ?
B2 N11 N12 C41 -176.2(6) . . . . ?
C28 C31 O4 C32 -164.2(8) . . . . ?
C48 O5 C47 C44 152.0(19) . . . . ?
C47A C44 C47 O5 -65.7(13) . . . . ?
C41 C44 C47 O5 -169.4(9) . . . . ?
C46 C44 C47 O5 -48.6(13) . . . . ?
C45A C44 C47 O5 80.1(11) . . . . ?
C45 C44 C47 O5 71.0(11) . . . . ?
C46A C44 C47 O5 -24.8(17) . . . . ?
C48A O5A C47A C44 169(3) . . . . ?
C41 C44 C47A O5A -164.1(11) . . . . ?
C46 C44 C47A O5A -56.3(13) . . . . ?
C45A C44 C47A O5A 69.8(14) . . . . ?
C45 C44 C47A O5A 44.3(15) . . . . ?
C47 C44 C47A O5A 106.5(16) . . . . ?
C46A C44 C47A O5A -48.1(14) . . . . ?

#===END OF CIF

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-10-02 at 11:19:39
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : shelxl dreduc import struct

data_Chisholm1571
_database_code_depnum_ccdc_archive 'CCDC 705809'

_audit_creation_date             2008-10-02T11:19:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_name_common            'Chisholm 1571'
_chemical_formula_moiety         'C24 H40 B1 N6 O3, C24 H40 B1 Mg1 N6 O3'
_chemical_formula_sum            'C48 H80 B2 Mg N12 O6'
_chemical_formula_weight         967.17
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.3126(1)
_cell_length_b                   14.5131(2)
_cell_length_c                   14.9368(2)
_cell_angle_alpha                97.536(1)
_cell_angle_beta                 115.884(1)
_cell_angle_gamma                99.546(1)
_cell_volume                     2679.34(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9294
_cell_measurement_theta_min      2.037
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       chunk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_special_details           
;All work was done at 150 K using an Oxford Cryosystems Cryostream
Cooler. The data collection strategy was set
up to measure a hemisphere of reciprocal space with a redundancy factor
of 2.3, which means that 90% of the reflections were measured at
least 2.3 times. Phi and omega scans with a frame width of 1.0\%
were used. Data integration was done with Denzo, and scaling
and merging of the data was done with Scalepack. This was a weakly
diffracting crystal, and the data set was measured only to a maximum
two theta value of 50 degrees.

The asymmetric unit consists of a Mg(Tp)* complex and
a free Tp* molecule. One of the branches of the free Tp* molecule is
disordered and this was modeled with two sets of atoms: O(3B) with
C(24B) and O(3C) with C(24C). DFIX and SADI restraints were used for
refining this disordered region.
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.09
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.756482E-1
_diffrn_orient_matrix_ub_12      0.161521E-1
_diffrn_orient_matrix_ub_13      0.114618E-1
_diffrn_orient_matrix_ub_21      0.242829E-1
_diffrn_orient_matrix_ub_22      -0.212255E-1
_diffrn_orient_matrix_ub_23      0.658637E-1
_diffrn_orient_matrix_ub_31      -0.11009E-1
_diffrn_orient_matrix_ub_32      -0.666463E-1
_diffrn_orient_matrix_ub_33      -0.37091E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_number            47258
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             9449
_reflns_number_gt                6822
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;For most of the methyl groups, the hydrogen atoms were added at calculated
positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom).
The torsion angle, which defines the orientation of the methyl group
about the O-C or C-C bond, was refined. For the methyl groups in the
disordered region (C(24B) and C(24C)), these torsion angles were not
refined. The remaining hydrogen atoms were included in the model at
calculated positions using a riding model with
U(H) = 1.2 * Ueq(attached atom).

The ten largest peaks in the final difference electron density map are
in the vicinity of the free Tp* molecule, but no additional disorder model
could be developed to account for any of these peaks. The structure
was also solved and refined in space group P1, but the same problem
persisted, i.e., the two Mg(Tp)* complexes were well-behaved, but
the two free Tp* groups contained disordered regions and large
residual electron density peaks. It is most likely that the correct
space group is P-1.

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     
'w=1/[\s^2^(Fo^2^)+(0.1718P)^2^+3.3880P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9449
_refine_ls_number_parameters     658
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0912
_refine_ls_wR_factor_ref         0.2891
_refine_ls_wR_factor_gt          0.2644
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         1.551
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.078

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
C1A C 0.9368(3) 0.2992(3) 0.1989(3) 0.0432(9) Uani 1 1 d . . .
C1B C 0.9456(4) 0.9239(3) 0.2874(4) 0.0649(13) Uani 1 1 d . . .
C2A C 1.0356(3) 0.2764(3) 0.2464(3) 0.0489(10) Uani 1 1 d . . .
H2A H 1.049 0.2144 0.2419 0.059 Uiso 1 1 calc R . .
C2B C 0.8951(4) 0.9769(4) 0.3288(4) 0.0697(13) Uani 1 1 d . . .
H2B H 0.9281 1.0284 0.3877 0.084 Uiso 1 1 calc R . .
C3A C 1.1091(3) 0.3626(3) 0.3007(3) 0.0451(9) Uani 1 1 d . . .
H3A H 1.1841 0.3714 0.3415 0.054 Uiso 1 1 calc R . .
C3B C 0.7867(4) 0.9382(3) 0.2657(4) 0.0659(13) Uani 1 1 d . . .
H3B H 0.7301 0.9578 0.2737 0.079 Uiso 1 1 calc R . .
C4A C 0.8277(4) 0.2311(3) 0.1312(3) 0.0511(10) Uani 1 1 d . . .
C4B C 1.0649(4) 0.9332(4) 0.3261(5) 0.0861(19) Uani 1 1 d . . .
C5A C 0.8342(4) 0.1605(3) 0.0490(4) 0.0647(12) Uani 1 1 d . . .
H5A1 H 0.8613 0.1966 0.0105 0.097 Uiso 1 1 calc R . .
H5A2 H 0.7626 0.119 0.0022 0.097 Uiso 1 1 calc R . .
H5A3 H 0.8828 0.1211 0.0818 0.097 Uiso 1 1 calc R . .
C5B C 1.0896(6) 0.8434(6) 0.3679(6) 0.121(3) Uani 1 1 d . . .
H5B1 H 1.0683 0.8395 0.4216 0.181 Uiso 1 1 calc R . .
H5B2 H 1.1667 0.848 0.3963 0.181 Uiso 1 1 calc R . .
H5B3 H 1.0497 0.7858 0.3123 0.181 Uiso 1 1 calc R . .
C6A C 0.7941(4) 0.1748(4) 0.1966(4) 0.0716(14) Uani 1 1 d . . .
H6A1 H 0.8447 0.1358 0.226 0.107 Uiso 1 1 calc R . .
H6A2 H 0.7219 0.1328 0.1539 0.107 Uiso 1 1 calc R . .
H6A3 H 0.7943 0.2196 0.2517 0.107 Uiso 1 1 calc R . .
C6B C 1.1291(5) 1.0260(6) 0.4105(7) 0.145(4) Uani 1 1 d . . .
H6B1 H 1.1167 1.0819 0.3806 0.217 Uiso 1 1 calc R . .
H6B2 H 1.2057 1.0281 0.4413 0.217 Uiso 1 1 calc R . .
H6B3 H 1.1055 1.0271 0.4631 0.217 Uiso 1 1 calc R . .
C7A C 0.7478(3) 0.2858(3) 0.0729(3) 0.0551(11) Uani 1 1 d . . .
H7A1 H 0.7727 0.3163 0.029 0.066 Uiso 1 1 calc R . .
H7A2 H 0.6779 0.2394 0.0274 0.066 Uiso 1 1 calc R . .
C7B C 1.0909(5) 0.9380(5) 0.2365(6) 0.101(2) Uani 1 1 d . . .
H7B1 H 1.1673 0.9395 0.2589 0.121 Uiso 1 1 calc R . .
H7B2 H 1.0461 0.8813 0.1794 0.121 Uiso 1 1 calc R . .
C8A C 0.6392(5) 0.3246(4) 0.1503(7) 0.103(2) Uani 1 1 d . . .
H8A1 H 0.5739 0.3115 0.0849 0.154 Uiso 1 1 calc R . .
H8A2 H 0.6364 0.3736 0.2003 0.154 Uiso 1 1 calc R . .
H8A3 H 0.6448 0.2655 0.1752 0.154 Uiso 1 1 calc R . .
C8B C 1.0551(12) 1.0116(9) 0.1061(12) 0.186(6) Uani 1 1 d . . .
H8B1 H 1.1194 0.9995 0.1037 0.278 Uiso 1 1 calc R . .
H8B2 H 1.043 1.0717 0.0853 0.278 Uiso 1 1 calc R . .
H8B3 H 0.993 0.9585 0.0596 0.278 Uiso 1 1 calc R . .
C9A C 0.9862(3) 0.6364(3) 0.1077(3) 0.0396(8) Uani 1 1 d . . .
C9B C 0.4997(4) 0.8528(3) 0.2057(4) 0.0667(13) Uani 1 1 d . . .
C10A C 1.0935(3) 0.6819(3) 0.1427(3) 0.0478(9) Uani 1 1 d . . .
H10A H 1.1221 0.7232 0.1116 0.057 Uiso 1 1 calc R . .
C10B C 0.4819(4) 0.9194(4) 0.1473(4) 0.0722(14) Uani 1 1 d . . .
H10B H 0.4421 0.9658 0.1464 0.087 Uiso 1 1 calc R . .
C11A C 1.1491(3) 0.6542(3) 0.2316(3) 0.0460(9) Uani 1 1 d . . .
H11A H 1.2247 0.6731 0.2737 0.055 Uiso 1 1 calc R . .
C11B C 0.5339(4) 0.9046(3) 0.0903(4) 0.0697(14) Uani 1 1 d . . .
H11B H 0.5379 0.9404 0.0426 0.084 Uiso 1 1 calc R . .
C12A C 0.8887(3) 0.6377(3) 0.0107(3) 0.0421(9) Uani 1 1 d . . .
C12B C 0.4688(4) 0.8370(4) 0.2904(4) 0.0697(14) Uani 1 1 d . . .
C13A C 0.8839(4) 0.5693(3) -0.0792(3) 0.0559(11) Uani 1 1 d . . .
H13A H 0.9478 0.5917 -0.087 0.084 Uiso 1 1 calc R . .
H13B H 0.8195 0.5676 -0.142 0.084 Uiso 1 1 calc R . .
H13C H 0.8812 0.5047 -0.0662 0.084 Uiso 1 1 calc R . .
C13B C 0.5581(6) 0.8979(7) 0.3939(6) 0.137(3) Uani 1 1 d . . .
H13D H 0.5412 0.8837 0.4483 0.206 Uiso 1 1 calc R . .
H13E H 0.564 0.9661 0.3937 0.206 Uiso 1 1 calc R . .
H13F H 0.6264 0.883 0.406 0.206 Uiso 1 1 calc R . .
C14A C 0.8954(4) 0.7405(3) -0.0078(3) 0.0572(11) Uani 1 1 d . . .
H14A H 0.896 0.7834 0.049 0.086 Uiso 1 1 calc R . .
H14B H 0.8331 0.7398 -0.0718 0.086 Uiso 1 1 calc R . .
H14C H 0.9612 0.7633 -0.0123 0.086 Uiso 1 1 calc R . .
C14B C 0.3630(6) 0.8655(6) 0.2657(7) 0.115(3) Uani 1 1 d . . .
H14D H 0.3395 0.8507 0.316 0.172 Uiso 1 1 calc R . .
H14E H 0.308 0.8296 0.1971 0.172 Uiso 1 1 calc R . .
H14F H 0.3739 0.9345 0.2684 0.172 Uiso 1 1 calc R . .
C15A C 0.7880(3) 0.6115(3) 0.0232(3) 0.0454(9) Uani 1 1 d . . .
H15A H 0.7982 0.6547 0.0855 0.054 Uiso 1 1 calc R . .
H15B H 0.7267 0.6224 -0.036 0.054 Uiso 1 1 calc R . .
C15B C 0.4562(6) 0.7323(5) 0.2978(5) 0.0856(17) Uani 1 1 d . . .
H15C H 0.4016 0.6912 0.2305 0.103 Uiso 1 1 calc R . .
H15D H 0.5251 0.7153 0.3138 0.103 Uiso 1 1 calc R . .
C16A C 0.6769(4) 0.4507(4) -0.0631(4) 0.0766(15) Uani 1 1 d . . .
H16A H 0.6214 0.4845 -0.0952 0.115 Uiso 1 1 calc R . .
H16B H 0.6456 0.3929 -0.0485 0.115 Uiso 1 1 calc R . .
H16C H 0.7059 0.4325 -0.1095 0.115 Uiso 1 1 calc R . .
C16B C 0.4259(6) 0.6177(5) 0.3846(5) 0.098(2) Uani 1 1 d . . .
H16D H 0.3725 0.572 0.3209 0.148 Uiso 1 1 calc R . .
H16E H 0.408 0.6087 0.4396 0.148 Uiso 1 1 calc R . .
H16F H 0.4971 0.6068 0.4025 0.148 Uiso 1 1 calc R . .
C17A C 0.9141(3) 0.6149(3) 0.4163(3) 0.0400(8) Uani 1 1 d . . .
C17B C 0.6257(4) 0.8020(3) -0.1630(4) 0.0585(11) Uani 1 1 d . . .
C18A C 1.0055(3) 0.6405(3) 0.5121(3) 0.0477(9) Uani 1 1 d . . .
H18A H 1.0117 0.6709 0.5754 0.057 Uiso 1 1 calc R . .
C18B C 0.6946(4) 0.8952(4) -0.1133(4) 0.0731(14) Uani 1 1 d . . .
H18B H 0.7199 0.9402 -0.1435 0.088 Uiso 1 1 calc R . .
C19A C 1.0835(3) 0.6126(3) 0.4953(3) 0.0451(9) Uani 1 1 d . . .
H19A H 1.1554 0.6207 0.5459 0.054 Uiso 1 1 calc R . .
C19B C 0.7173(4) 0.9071(3) -0.0129(4) 0.0673(13) Uani 1 1 d . . .
H19B H 0.7612 0.9631 0.0395 0.081 Uiso 1 1 calc R . .
C20A C 0.8056(3) 0.6360(3) 0.3862(3) 0.0470(9) Uani 1 1 d . . .
C21A C 0.8205(4) 0.7331(4) 0.4528(4) 0.0663(13) Uani 1 1 d . . .
H21A H 0.8537 0.7302 0.5249 0.099 Uiso 1 1 calc R . .
H21B H 0.7504 0.7472 0.4333 0.099 Uiso 1 1 calc R . .
H21C H 0.8668 0.7838 0.4425 0.099 Uiso 1 1 calc R . .
C22A C 0.7304(4) 0.5559(4) 0.3987(4) 0.0612(12) Uani 1 1 d . . .
H22A H 0.72 0.4948 0.3545 0.092 Uiso 1 1 calc R . .
H22B H 0.661 0.5713 0.3796 0.092 Uiso 1 1 calc R . .
H22C H 0.7622 0.5505 0.4701 0.092 Uiso 1 1 calc R . .
C23A C 0.7579(3) 0.6490(3) 0.2772(3) 0.0480(9) Uani 1 1 d . . .
H23A H 0.6941 0.6747 0.2625 0.058 Uiso 1 1 calc R . .
H23B H 0.8111 0.6967 0.2704 0.058 Uiso 1 1 calc R . .
C20B C 0.5785(4) 0.7539(4) -0.2705(4) 0.0695(14) Uani 1 1 d . A .
C24A C 0.6145(3) 0.5352(4) 0.1297(4) 0.0650(12) Uani 1 1 d . . .
H24A H 0.5715 0.5244 0.1653 0.098 Uiso 1 1 calc R . .
H24B H 0.5977 0.4767 0.0788 0.098 Uiso 1 1 calc R . .
H24C H 0.5978 0.5879 0.0953 0.098 Uiso 1 1 calc R . .
C21B C 0.5507(6) 0.6425(4) -0.2843(5) 0.0943(19) Uani 1 1 d . . .
H21D H 0.4906 0.6227 -0.27 0.141 Uiso 1 1 calc R . .
H21E H 0.6133 0.6235 -0.2368 0.141 Uiso 1 1 calc R . .
H21F H 0.5306 0.6114 -0.3546 0.141 Uiso 1 1 calc R . .
C22B C 0.6672(7) 0.7734(7) -0.3076(6) 0.120(3) Uani 1 1 d . . .
H22D H 0.639 0.7351 -0.3772 0.18 Uiso 1 1 calc R . .
H22E H 0.7314 0.7554 -0.2616 0.18 Uiso 1 1 calc R . .
H22F H 0.6857 0.8417 -0.3069 0.18 Uiso 1 1 calc R . .
C23B C 0.4963(7) 0.7899(6) -0.3368(7) 0.133(3) Uani 1 1 d D . .
H23C H 0.5238 0.8599 -0.3251 0.159 Uiso 0.684(13) 1 calc PR A 1
H23D H 0.478 0.7606 -0.408 0.159 Uiso 0.684(13) 1 calc PR A 1
H23E H 0.466 0.8189 -0.2953 0.159 Uiso 0.316(13) 1 calc PR A 2
H23F H 0.5322 0.8437 -0.3544 0.159 Uiso 0.316(13) 1 calc PR A 2
C24B C 0.3303(8) 0.8209(11) -0.3921(12) 0.130(6) Uani 0.684(13) 1 d PD A 1
H24D H 0.2664 0.8075 -0.3822 0.194 Uiso 0.684(13) 1 calc PR A 1
H24E H 0.3102 0.7958 -0.464 0.194 Uiso 0.684(13) 1 calc PR A 1
H24F H 0.361 0.8903 -0.3735 0.194 Uiso 0.684(13) 1 calc PR A 1
C24C C 0.3342(15) 0.7863(17) -0.4766(18) 0.099(8) Uani 0.316(13) 1 d PD A 2
H24G H 0.278 0.7398 -0.5382 0.148 Uiso 0.316(13) 1 calc PR A 2
H24H H 0.3652 0.8406 -0.4961 0.148 Uiso 0.316(13) 1 calc PR A 2
H24I H 0.3032 0.8093 -0.4337 0.148 Uiso 0.316(13) 1 calc PR A 2
B1A B 1.1010(3) 0.5411(3) 0.3357(3) 0.0387(9) Uani 1 1 d . . .
H1A H 1.1799 0.5559 0.3827 0.046 Uiso 1 1 calc R . .
B1B B 0.6714(4) 0.8036(4) 0.0981(4) 0.0526(12) Uani 1 1 d . . .
H1B H 0.6688 0.7342 0.0971 0.063 Uiso 1 1 calc R . .
Mg Mg 0.84558(9) 0.49641(8) 0.18582(8) 0.0365(3) Uani 1 1 d . . .
N1A N 1.0566(2) 0.4326(2) 0.2864(2) 0.0390(7) Uani 1 1 d . . .
N1B N 0.7756(3) 0.8677(2) 0.1906(3) 0.0560(9) Uani 1 1 d . . .
N2A N 0.9496(2) 0.3948(2) 0.2234(2) 0.0390(7) Uani 1 1 d . . .
N2B N 0.8741(3) 0.8573(3) 0.2057(3) 0.0604(10) Uani 1 1 d . . .
N3A N 1.0789(2) 0.5961(2) 0.2493(2) 0.0386(7) Uani 1 1 d . . .
N3B N 0.5779(3) 0.8306(3) 0.1138(3) 0.0627(10) Uani 1 1 d . . .
N4A N 0.9769(2) 0.5841(2) 0.1729(2) 0.0368(7) Uani 1 1 d . . .
N4B N 0.5569(3) 0.7978(3) 0.1861(3) 0.0577(9) Uani 1 1 d . . .
N5A N 1.0425(2) 0.5714(2) 0.3952(2) 0.0393(7) Uani 1 1 d . . .
N5B N 0.6671(3) 0.8262(2) -0.0009(3) 0.0556(9) Uani 1 1 d . . .
N6A N 0.9360(2) 0.5712(2) 0.3459(2) 0.0376(7) Uani 1 1 d . . .
N6B N 0.6121(3) 0.7601(3) -0.0926(3) 0.0556(9) Uani 1 1 d . . .
O1A O 0.7321(2) 0.35898(19) 0.1364(2) 0.0528(7) Uani 1 1 d . . .
O1B O 1.0694(5) 1.0191(4) 0.2068(7) 0.147(2) Uani 1 1 d . . .
O2A O 0.7616(2) 0.51251(19) 0.03059(18) 0.0455(6) Uani 1 1 d . . .
O2B O 0.4263(3) 0.7128(3) 0.3712(3) 0.0849(11) Uani 1 1 d . . .
O3A O 0.7271(2) 0.5599(2) 0.20274(19) 0.0482(7) Uani 1 1 d . . .
O3B O 0.4091(6) 0.7747(5) -0.3277(5) 0.097(3) Uani 0.684(13) 1 d PD A 1
O3C O 0.4158(13) 0.7415(10) -0.4210(10) 0.126(8) Uani 0.316(13) 1 d PD A 2

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
C1A 0.052(2) 0.038(2) 0.0355(19) 0.0092(16) 0.0176(17) 0.0112(17)
C1B 0.055(3) 0.052(2) 0.059(3) 0.001(2) 0.002(2) 0.019(2)
C2A 0.063(3) 0.044(2) 0.041(2) 0.0098(18) 0.023(2) 0.021(2)
C2B 0.065(3) 0.059(3) 0.061(3) -0.003(2) 0.012(2) 0.018(2)
C3A 0.051(2) 0.052(2) 0.0349(19) 0.0130(17) 0.0188(18) 0.0224(19)
C3B 0.066(3) 0.058(3) 0.064(3) 0.005(2) 0.022(2) 0.024(2)
C4A 0.060(3) 0.036(2) 0.049(2) 0.0075(17) 0.021(2) 0.0044(18)
C4B 0.048(3) 0.076(3) 0.084(4) -0.026(3) -0.003(3) 0.021(3)
C5A 0.071(3) 0.042(2) 0.061(3) -0.005(2) 0.023(2) 0.000(2)
C5B 0.086(4) 0.143(7) 0.094(5) 0.015(4) -0.004(4) 0.075(5)
C6A 0.075(3) 0.065(3) 0.077(3) 0.026(3) 0.037(3) 0.007(3)
C6B 0.055(4) 0.134(6) 0.144(7) -0.079(6) -0.004(4) 0.004(4)
C7A 0.049(2) 0.042(2) 0.054(2) 0.0013(19) 0.013(2) 0.0007(18)
C7B 0.061(3) 0.075(4) 0.128(6) -0.022(4) 0.022(4) 0.016(3)
C8A 0.090(4) 0.056(3) 0.182(7) 0.012(4) 0.092(5) 0.000(3)
C8B 0.248(15) 0.151(10) 0.264(16) 0.081(10) 0.190(14) 0.091(10)
C9A 0.043(2) 0.0368(19) 0.0369(19) 0.0094(15) 0.0165(16) 0.0111(16)
C9B 0.050(3) 0.059(3) 0.063(3) -0.009(2) 0.005(2) 0.020(2)
C10A 0.044(2) 0.050(2) 0.050(2) 0.0205(19) 0.0209(19) 0.0108(18)
C10B 0.054(3) 0.056(3) 0.089(4) 0.000(3) 0.021(3) 0.019(2)
C11A 0.0339(19) 0.048(2) 0.050(2) 0.0113(18) 0.0154(17) 0.0054(17)
C11B 0.073(3) 0.046(3) 0.075(3) 0.011(2) 0.020(3) 0.022(2)
C12A 0.046(2) 0.047(2) 0.0333(19) 0.0161(16) 0.0149(17) 0.0161(17)
C12B 0.045(3) 0.066(3) 0.076(3) -0.014(2) 0.022(2) 0.002(2)
C13A 0.064(3) 0.067(3) 0.039(2) 0.015(2) 0.023(2) 0.024(2)
C13B 0.102(5) 0.152(7) 0.094(5) -0.047(5) 0.037(4) -0.044(5)
C14A 0.060(3) 0.053(2) 0.055(3) 0.028(2) 0.018(2) 0.018(2)
C14B 0.087(5) 0.118(6) 0.179(8) 0.059(6) 0.082(5) 0.049(4)
C15A 0.044(2) 0.048(2) 0.0348(19) 0.0112(16) 0.0082(16) 0.0168(18)
C15B 0.109(5) 0.095(4) 0.069(3) 0.015(3) 0.050(3) 0.046(4)
C16A 0.063(3) 0.073(3) 0.046(3) 0.010(2) -0.008(2) -0.005(2)
C16B 0.090(4) 0.115(5) 0.096(5) 0.039(4) 0.036(4) 0.049(4)
C17A 0.046(2) 0.0384(19) 0.0316(18) 0.0088(15) 0.0141(16) 0.0118(16)
C17B 0.059(3) 0.046(2) 0.064(3) 0.018(2) 0.022(2) 0.013(2)
C18A 0.053(2) 0.053(2) 0.0318(19) 0.0055(17) 0.0146(18) 0.0180(19)
C18B 0.080(3) 0.055(3) 0.074(3) 0.027(3) 0.024(3) 0.016(3)
C19A 0.045(2) 0.045(2) 0.0287(19) 0.0041(16) 0.0045(16) 0.0105(17)
C19B 0.075(3) 0.043(2) 0.069(3) 0.017(2) 0.020(3) 0.012(2)
C20A 0.051(2) 0.052(2) 0.038(2) 0.0120(17) 0.0165(18) 0.0236(19)
C21A 0.079(3) 0.071(3) 0.049(3) 0.009(2) 0.022(2) 0.044(3)
C22A 0.056(3) 0.083(3) 0.060(3) 0.032(2) 0.032(2) 0.031(2)
C23A 0.048(2) 0.051(2) 0.041(2) 0.0116(18) 0.0145(18) 0.0187(18)
C20B 0.059(3) 0.080(3) 0.053(3) 0.034(2) 0.009(2) 0.008(2)
C24A 0.037(2) 0.063(3) 0.070(3) 0.012(2) 0.007(2) 0.007(2)
C21B 0.135(6) 0.072(4) 0.063(3) 0.007(3) 0.038(4) 0.024(4)
C22B 0.127(6) 0.141(7) 0.087(5) 0.017(5) 0.059(5) 0.002(5)
C23B 0.107(6) 0.118(6) 0.106(6) 0.020(5) -0.005(5) 0.019(5)
C24B 0.064(6) 0.167(12) 0.141(12) 0.092(10) 0.015(7) 0.037(7)
C24C 0.073(12) 0.126(18) 0.069(13) 0.043(13) 0.005(10) 0.018(12)
B1A 0.034(2) 0.044(2) 0.030(2) 0.0094(17) 0.0083(17) 0.0102(18)
B1B 0.048(3) 0.045(3) 0.056(3) 0.014(2) 0.014(2) 0.019(2)
Mg 0.0341(6) 0.0364(6) 0.0301(6) 0.0064(5) 0.0087(5) 0.0057(5)
N1A 0.0386(16) 0.0415(17) 0.0318(15) 0.0089(13) 0.0118(13) 0.0106(13)
N1B 0.052(2) 0.0462(19) 0.055(2) 0.0077(17) 0.0113(17) 0.0190(16)
N2A 0.0390(16) 0.0357(16) 0.0341(16) 0.0081(13) 0.0109(13) 0.0065(13)
N2B 0.044(2) 0.056(2) 0.059(2) 0.0016(18) 0.0064(17) 0.0186(17)
N3A 0.0341(16) 0.0386(16) 0.0362(16) 0.0093(13) 0.0108(13) 0.0074(13)
N3B 0.054(2) 0.062(2) 0.064(2) 0.0137(19) 0.0171(19) 0.0278(19)
N4A 0.0348(16) 0.0384(16) 0.0301(15) 0.0086(12) 0.0092(13) 0.0079(13)
N4B 0.047(2) 0.056(2) 0.062(2) 0.0092(18) 0.0181(18) 0.0165(17)
N5A 0.0355(16) 0.0418(16) 0.0311(15) 0.0076(13) 0.0076(13) 0.0098(13)
N5B 0.051(2) 0.047(2) 0.054(2) 0.0110(17) 0.0104(17) 0.0137(16)
N6A 0.0365(16) 0.0404(16) 0.0302(15) 0.0084(13) 0.0099(13) 0.0118(13)
N6B 0.047(2) 0.0475(19) 0.053(2) 0.0113(17) 0.0077(17) 0.0104(16)
O1A 0.0423(15) 0.0438(15) 0.0609(18) 0.0040(13) 0.0190(14) 0.0036(12)
O1B 0.158(5) 0.071(3) 0.234(8) 0.011(4) 0.123(6) 0.013(3)
O2A 0.0394(14) 0.0487(15) 0.0328(13) 0.0081(11) 0.0059(11) 0.0040(12)
O2B 0.074(2) 0.095(3) 0.080(3) 0.013(2) 0.032(2) 0.025(2)
O3A 0.0374(14) 0.0582(17) 0.0375(14) 0.0047(12) 0.0086(11) 0.0142(12)
O3B 0.074(4) 0.117(5) 0.083(5) 0.031(4) 0.027(3) 0.004(4)
O3C 0.142(15) 0.092(10) 0.064(10) -0.010(7) -0.013(9) 0.031(10)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
C1A N2A 1.347(5) . ?
C1A C2A 1.397(6) . ?
C1A C4A 1.512(6) . ?
C1B N2B 1.320(6) . ?
C1B C2B 1.395(7) . ?
C1B C4B 1.520(7) . ?
C2A C3A 1.372(6) . ?
C2A H2A 0.95 . ?
C2B C3B 1.381(7) . ?
C2B H2B 0.95 . ?
C3A N1A 1.347(5) . ?
C3A H3A 0.95 . ?
C3B N1B 1.348(6) . ?
C3B H3B 0.95 . ?
C4A C7A 1.519(6) . ?
C4A C6A 1.530(6) . ?
C4A C5A 1.539(6) . ?
C4B C7B 1.543(10) . ?
C4B C6B 1.543(8) . ?
C4B C5B 1.545(10) . ?
C5A H5A1 0.98 . ?
C5A H5A2 0.98 . ?
C5A H5A3 0.98 . ?
C5B H5B1 0.98 . ?
C5B H5B2 0.98 . ?
C5B H5B3 0.98 . ?
C6A H6A1 0.98 . ?
C6A H6A2 0.98 . ?
C6A H6A3 0.98 . ?
C6B H6B1 0.98 . ?
C6B H6B2 0.98 . ?
C6B H6B3 0.98 . ?
C7A O1A 1.442(5) . ?
C7A H7A1 0.99 . ?
C7A H7A2 0.99 . ?
C7B O1B 1.347(9) . ?
C7B H7B1 0.99 . ?
C7B H7B2 0.99 . ?
C8A O1A 1.451(6) . ?
C8A H8A1 0.98 . ?
C8A H8A2 0.98 . ?
C8A H8A3 0.98 . ?
C8B O1B 1.413(14) . ?
C8B H8B1 0.98 . ?
C8B H8B2 0.98 . ?
C8B H8B3 0.98 . ?
C9A N4A 1.346(5) . ?
C9A C10A 1.393(6) . ?
C9A C12A 1.516(5) . ?
C9B N4B 1.326(6) . ?
C9B C10B 1.367(8) . ?
C9B C12B 1.542(8) . ?
C10A C11A 1.372(6) . ?
C10A H10A 0.95 . ?
C10B C11B 1.372(8) . ?
C10B H10B 0.95 . ?
C11A N3A 1.341(5) . ?
C11A H11A 0.95 . ?
C11B N3B 1.344(6) . ?
C11B H11B 0.95 . ?
C12A C15A 1.527(6) . ?
C12A C13A 1.530(6) . ?
C12A C14A 1.547(5) . ?
C12B C15B 1.524(8) . ?
C12B C13B 1.533(8) . ?
C12B C14B 1.537(8) . ?
C13A H13A 0.98 . ?
C13A H13B 0.98 . ?
C13A H13C 0.98 . ?
C13B H13D 0.98 . ?
C13B H13E 0.98 . ?
C13B H13F 0.98 . ?
C14A H14A 0.98 . ?
C14A H14B 0.98 . ?
C14A H14C 0.98 . ?
C14B H14D 0.98 . ?
C14B H14E 0.98 . ?
C14B H14F 0.98 . ?
C15A O2A 1.455(5) . ?
C15A H15A 0.99 . ?
C15A H15B 0.99 . ?
C15B O2B 1.386(7) . ?
C15B H15C 0.99 . ?
C15B H15D 0.99 . ?
C16A O2A 1.436(5) . ?
C16A H16A 0.98 . ?
C16A H16B 0.98 . ?
C16A H16C 0.98 . ?
C16B O2B 1.420(8) . ?
C16B H16D 0.98 . ?
C16B H16E 0.98 . ?
C16B H16F 0.98 . ?
C17A N6A 1.337(5) . ?
C17A C18A 1.401(5) . ?
C17A C20A 1.513(5) . ?
C17B N6B 1.350(6) . ?
C17B C18B 1.417(7) . ?
C17B C20B 1.458(7) . ?
C18A C19A 1.356(6) . ?
C18A H18A 0.95 . ?
C18B C19B 1.368(7) . ?
C18B H18B 0.95 . ?
C19A N5A 1.350(5) . ?
C19A H19A 0.95 . ?
C19B N5B 1.347(6) . ?
C19B H19B 0.95 . ?
C20A C23A 1.519(5) . ?
C20A C22A 1.537(6) . ?
C20A C21A 1.540(6) . ?
C21A H21A 0.98 . ?
C21A H21B 0.98 . ?
C21A H21C 0.98 . ?
C22A H22A 0.98 . ?
C22A H22B 0.98 . ?
C22A H22C 0.98 . ?
C23A O3A 1.453(5) . ?
C23A H23A 0.99 . ?
C23A H23B 0.99 . ?
C20B C23B 1.400(9) . ?
C20B C21B 1.563(8) . ?
C20B C22B 1.593(9) . ?
C24A O3A 1.445(5) . ?
C24A H24A 0.98 . ?
C24A H24B 0.98 . ?
C24A H24C 0.98 . ?
C21B H21D 0.98 . ?
C21B H21E 0.98 . ?
C21B H21F 0.98 . ?
C22B H22D 0.98 . ?
C22B H22E 0.98 . ?
C22B H22F 0.98 . ?
C23B O3C 1.280(12) . ?
C23B O3B 1.300(10) . ?
C23B H23C 0.99 . ?
C23B H23D 0.99 . ?
C23B H23E 0.99 . ?
C23B H23F 0.99 . ?
C24B O3B 1.456(11) . ?
C24B H24D 0.98 . ?
C24B H24E 0.98 . ?
C24B H24F 0.98 . ?
C24C O3C 1.422(17) . ?
C24C H24G 0.98 . ?
C24C H24H 0.98 . ?
C24C H24I 0.98 . ?
B1A N5A 1.533(5) . ?
B1A N1A 1.543(5) . ?
B1A N3A 1.549(5) . ?
B1A H1A 1 . ?
B1B N5B 1.534(6) . ?
B1B N1B 1.550(6) . ?
B1B N3B 1.555(6) . ?
B1B H1B 1 . ?
Mg O3A 2.150(3) . ?
Mg O1A 2.157(3) . ?
Mg O2A 2.163(3) . ?
Mg N6A 2.173(3) . ?
Mg N4A 2.187(3) . ?
Mg N2A 2.219(3) . ?
N1A N2A 1.364(4) . ?
N1B N2B 1.366(5) . ?
N3A N4A 1.369(4) . ?
N3B N4B 1.363(6) . ?
N5A N6A 1.373(4) . ?
N5B N6B 1.371(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
N2A C1A C2A 110.3(3) . . ?
N2A C1A C4A 121.8(3) . . ?
C2A C1A C4A 127.8(4) . . ?
N2B C1B C2B 110.7(4) . . ?
N2B C1B C4B 120.7(4) . . ?
C2B C1B C4B 128.6(4) . . ?
C3A C2A C1A 105.3(3) . . ?
C3A C2A H2A 127.4 . . ?
C1A C2A H2A 127.4 . . ?
C3B C2B C1B 105.0(4) . . ?
C3B C2B H2B 127.5 . . ?
C1B C2B H2B 127.5 . . ?
N1A C3A C2A 108.2(4) . . ?
N1A C3A H3A 125.9 . . ?
C2A C3A H3A 125.9 . . ?
N1B C3B C2B 107.7(4) . . ?
N1B C3B H3B 126.2 . . ?
C2B C3B H3B 126.2 . . ?
C1A C4A C7A 110.2(3) . . ?
C1A C4A C6A 109.0(4) . . ?
C7A C4A C6A 113.7(4) . . ?
C1A C4A C5A 109.2(4) . . ?
C7A C4A C5A 105.4(4) . . ?
C6A C4A C5A 109.2(4) . . ?
C1B C4B C7B 109.0(5) . . ?
C1B C4B C6B 109.5(5) . . ?
C7B C4B C6B 109.3(7) . . ?
C1B C4B C5B 106.9(6) . . ?
C7B C4B C5B 110.8(5) . . ?
C6B C4B C5B 111.2(6) . . ?
C4A C5A H5A1 109.5 . . ?
C4A C5A H5A2 109.5 . . ?
H5A1 C5A H5A2 109.5 . . ?
C4A C5A H5A3 109.5 . . ?
H5A1 C5A H5A3 109.5 . . ?
H5A2 C5A H5A3 109.5 . . ?
C4B C5B H5B1 109.5 . . ?
C4B C5B H5B2 109.5 . . ?
H5B1 C5B H5B2 109.5 . . ?
C4B C5B H5B3 109.5 . . ?
H5B1 C5B H5B3 109.5 . . ?
H5B2 C5B H5B3 109.5 . . ?
C4A C6A H6A1 109.5 . . ?
C4A C6A H6A2 109.5 . . ?
H6A1 C6A H6A2 109.5 . . ?
C4A C6A H6A3 109.5 . . ?
H6A1 C6A H6A3 109.5 . . ?
H6A2 C6A H6A3 109.5 . . ?
C4B C6B H6B1 109.5 . . ?
C4B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C4B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
O1A C7A C4A 114.7(4) . . ?
O1A C7A H7A1 108.6 . . ?
C4A C7A H7A1 108.6 . . ?
O1A C7A H7A2 108.6 . . ?
C4A C7A H7A2 108.6 . . ?
H7A1 C7A H7A2 107.6 . . ?
O1B C7B C4B 106.7(6) . . ?
O1B C7B H7B1 110.4 . . ?
C4B C7B H7B1 110.4 . . ?
O1B C7B H7B2 110.4 . . ?
C4B C7B H7B2 110.4 . . ?
H7B1 C7B H7B2 108.6 . . ?
O1A C8A H8A1 109.5 . . ?
O1A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
O1A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
O1B C8B H8B1 109.5 . . ?
O1B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
O1B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
N4A C9A C10A 110.0(3) . . ?
N4A C9A C12A 121.1(3) . . ?
C10A C9A C12A 128.9(3) . . ?
N4B C9B C10B 111.5(5) . . ?
N4B C9B C12B 118.1(5) . . ?
C10B C9B C12B 130.4(5) . . ?
C11A C10A C9A 105.4(3) . . ?
C11A C10A H10A 127.3 . . ?
C9A C10A H10A 127.3 . . ?
C9B C10B C11B 105.2(4) . . ?
C9B C10B H10B 127.4 . . ?
C11B C10B H10B 127.4 . . ?
N3A C11A C10A 108.5(3) . . ?
N3A C11A H11A 125.7 . . ?
C10A C11A H11A 125.7 . . ?
N3B C11B C10B 107.8(5) . . ?
N3B C11B H11B 126.1 . . ?
C10B C11B H11B 126.1 . . ?
C9A C12A C15A 109.7(3) . . ?
C9A C12A C13A 108.8(3) . . ?
C15A C12A C13A 112.6(3) . . ?
C9A C12A C14A 110.4(3) . . ?
C15A C12A C14A 105.4(3) . . ?
C13A C12A C14A 110.0(3) . . ?
C15B C12B C13B 107.4(6) . . ?
C15B C12B C14B 110.1(5) . . ?
C13B C12B C14B 110.3(6) . . ?
C15B C12B C9B 110.6(4) . . ?
C13B C12B C9B 109.6(5) . . ?
C14B C12B C9B 108.9(5) . . ?
C12A C13A H13A 109.5 . . ?
C12A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C12A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12B C13B H13D 109.5 . . ?
C12B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C12B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C12A C14A H14A 109.5 . . ?
C12A C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C12A C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C12B C14B H14D 109.5 . . ?
C12B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C12B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
O2A C15A C12A 113.5(3) . . ?
O2A C15A H15A 108.9 . . ?
C12A C15A H15A 108.9 . . ?
O2A C15A H15B 108.9 . . ?
C12A C15A H15B 108.9 . . ?
H15A C15A H15B 107.7 . . ?
O2B C15B C12B 113.5(4) . . ?
O2B C15B H15C 108.9 . . ?
C12B C15B H15C 108.9 . . ?
O2B C15B H15D 108.9 . . ?
C12B C15B H15D 108.9 . . ?
H15C C15B H15D 107.7 . . ?
O2A C16A H16A 109.5 . . ?
O2A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
O2A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
O2B C16B H16D 109.5 . . ?
O2B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
O2B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
N6A C17A C18A 109.8(3) . . ?
N6A C17A C20A 120.7(3) . . ?
C18A C17A C20A 129.3(3) . . ?
N6B C17B C18B 108.6(4) . . ?
N6B C17B C20B 123.3(4) . . ?
C18B C17B C20B 128.1(4) . . ?
C19A C18A C17A 105.4(3) . . ?
C19A C18A H18A 127.3 . . ?
C17A C18A H18A 127.3 . . ?
C19B C18B C17B 105.9(4) . . ?
C19B C18B H18B 127 . . ?
C17B C18B H18B 127 . . ?
N5A C19A C18A 109.1(3) . . ?
N5A C19A H19A 125.4 . . ?
C18A C19A H19A 125.4 . . ?
N5B C19B C18B 108.6(4) . . ?
N5B C19B H19B 125.7 . . ?
C18B C19B H19B 125.7 . . ?
C17A C20A C23A 109.6(3) . . ?
C17A C20A C22A 110.8(3) . . ?
C23A C20A C22A 111.4(4) . . ?
C17A C20A C21A 109.2(3) . . ?
C23A C20A C21A 105.4(3) . . ?
C22A C20A C21A 110.3(4) . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C20A C22A H22A 109.5 . . ?
C20A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C20A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
O3A C23A C20A 112.4(3) . . ?
O3A C23A H23A 109.1 . . ?
C20A C23A H23A 109.1 . . ?
O3A C23A H23B 109.1 . . ?
C20A C23A H23B 109.1 . . ?
H23A C23A H23B 107.9 . . ?
C23B C20B C17B 114.5(6) . . ?
C23B C20B C21B 115.1(6) . . ?
C17B C20B C21B 110.6(4) . . ?
C23B C20B C22B 103.2(6) . . ?
C17B C20B C22B 108.8(5) . . ?
C21B C20B C22B 103.5(6) . . ?
O3A C24A H24A 109.5 . . ?
O3A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
O3A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
C20B C22B H22D 109.5 . . ?
C20B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C20B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O3C C23B C20B 125.8(10) . . ?
O3B C23B C20B 115.2(8) . . ?
O3B C23B H23C 108.5 . . ?
C20B C23B H23C 108.5 . . ?
O3B C23B H23D 108.5 . . ?
C20B C23B H23D 108.5 . . ?
H23C C23B H23D 107.5 . . ?
O3C C23B H23E 105.9 . . ?
C20B C23B H23E 105.9 . . ?
O3C C23B H23F 105.8 . . ?
C20B C23B H23F 105.9 . . ?
H23E C23B H23F 106.2 . . ?
O3B C24B H24D 109.5 . . ?
O3B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
O3B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
O3C C24C H24G 109.5 . . ?
O3C C24C H24H 109.5 . . ?
H24G C24C H24H 109.5 . . ?
O3C C24C H24I 109.5 . . ?
H24G C24C H24I 109.5 . . ?
H24H C24C H24I 109.5 . . ?
N5A B1A N1A 109.4(3) . . ?
N5A B1A N3A 108.7(3) . . ?
N1A B1A N3A 108.3(3) . . ?
N5A B1A H1A 110.1 . . ?
N1A B1A H1A 110.1 . . ?
N3A B1A H1A 110.1 . . ?
N5B B1B N1B 109.2(4) . . ?
N5B B1B N3B 110.9(3) . . ?
N1B B1B N3B 105.4(4) . . ?
N5B B1B H1B 110.4 . . ?
N1B B1B H1B 110.4 . . ?
N3B B1B H1B 110.4 . . ?
O3A Mg O1A 87.45(11) . . ?
O3A Mg O2A 82.52(11) . . ?
O1A Mg O2A 86.95(11) . . ?
O3A Mg N6A 79.90(11) . . ?
O1A Mg N6A 121.79(12) . . ?
O2A Mg N6A 145.19(12) . . ?
O3A Mg N4A 120.18(12) . . ?
O1A Mg N4A 146.74(13) . . ?
O2A Mg N4A 79.49(11) . . ?
N6A Mg N4A 83.76(12) . . ?
O3A Mg N2A 150.53(12) . . ?
O1A Mg N2A 76.88(11) . . ?
O2A Mg N2A 120.71(12) . . ?
N6A Mg N2A 87.30(11) . . ?
N4A Mg N2A 84.19(11) . . ?
C3A N1A N2A 110.4(3) . . ?
C3A N1A B1A 128.8(3) . . ?
N2A N1A B1A 120.7(3) . . ?
C3B N1B N2B 109.9(4) . . ?
C3B N1B B1B 128.9(4) . . ?
N2B N1B B1B 121.2(3) . . ?
C1A N2A N1A 105.8(3) . . ?
C1A N2A Mg 136.8(3) . . ?
N1A N2A Mg 117.4(2) . . ?
C1B N2B N1B 106.6(4) . . ?
C11A N3A N4A 109.9(3) . . ?
C11A N3A B1A 129.0(3) . . ?
N4A N3A B1A 121.0(3) . . ?
C11B N3B N4B 109.8(4) . . ?
C11B N3B B1B 128.7(5) . . ?
N4B N3B B1B 118.3(3) . . ?
C9A N4A N3A 106.1(3) . . ?
C9A N4A Mg 136.3(2) . . ?
N3A N4A Mg 117.5(2) . . ?
C9B N4B N3B 105.7(4) . . ?
C19A N5A N6A 109.0(3) . . ?
C19A N5A B1A 129.1(3) . . ?
N6A N5A B1A 121.4(3) . . ?
C19B N5B N6B 109.7(4) . . ?
C19B N5B B1B 128.1(4) . . ?
N6B N5B B1B 122.1(3) . . ?
C17A N6A N5A 106.6(3) . . ?
C17A N6A Mg 136.4(2) . . ?
N5A N6A Mg 116.9(2) . . ?
C17B N6B N5B 107.1(3) . . ?
C7A O1A C8A 112.1(4) . . ?
C7A O1A Mg 114.5(2) . . ?
C8A O1A Mg 133.4(3) . . ?
C7B O1B C8B 109.1(7) . . ?
C16A O2A C15A 113.2(3) . . ?
C16A O2A Mg 134.3(3) . . ?
C15A O2A Mg 111.9(2) . . ?
C15B O2B C16B 112.7(5) . . ?
C24A O3A C23A 112.0(3) . . ?
C24A O3A Mg 125.1(3) . . ?
C23A O3A Mg 121.2(2) . . ?
C23B O3B C24B 112.7(8) . . ?
C23B O3C C24C 119.4(15) . . ?

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
N2A C1A C2A C3A -0.1(4) . . . . ?
C4A C1A C2A C3A -178.5(4) . . . . ?
N2B C1B C2B C3B -0.5(6) . . . . ?
C4B C1B C2B C3B -178.7(6) . . . . ?
C1A C2A C3A N1A 0.1(4) . . . . ?
C1B C2B C3B N1B -1.1(6) . . . . ?
N2A C1A C4A C7A 17.3(5) . . . . ?
C2A C1A C4A C7A -164.5(4) . . . . ?
N2A C1A C4A C6A -108.1(4) . . . . ?
C2A C1A C4A C6A 70.1(5) . . . . ?
N2A C1A C4A C5A 132.7(4) . . . . ?
C2A C1A C4A C5A -49.1(5) . . . . ?
N2B C1B C4B C7B 51.3(7) . . . . ?
C2B C1B C4B C7B -130.7(6) . . . . ?
N2B C1B C4B C6B 170.8(7) . . . . ?
C2B C1B C4B C6B -11.2(10) . . . . ?
N2B C1B C4B C5B -68.6(7) . . . . ?
C2B C1B C4B C5B 109.5(6) . . . . ?
C1A C4A C7A O1A -60.3(5) . . . . ?
C6A C4A C7A O1A 62.4(5) . . . . ?
C5A C4A C7A O1A -178.1(3) . . . . ?
C1B C4B C7B O1B 64.0(6) . . . . ?
C6B C4B C7B O1B -55.6(7) . . . . ?
C5B C4B C7B O1B -178.6(5) . . . . ?
N4A C9A C10A C11A 0.4(5) . . . . ?
C12A C9A C10A C11A -177.5(4) . . . . ?
N4B C9B C10B C11B -1.4(6) . . . . ?
C12B C9B C10B C11B 175.5(5) . . . . ?
C9A C10A C11A N3A -0.5(5) . . . . ?
C9B C10B C11B N3B 1.3(6) . . . . ?
N4A C9A C12A C15A 23.7(5) . . . . ?
C10A C9A C12A C15A -158.6(4) . . . . ?
N4A C9A C12A C13A -99.8(4) . . . . ?
C10A C9A C12A C13A 77.9(5) . . . . ?
N4A C9A C12A C14A 139.3(4) . . . . ?
C10A C9A C12A C14A -42.9(5) . . . . ?
N4B C9B C12B C15B -30.3(6) . . . . ?
C10B C9B C12B C15B 153.0(5) . . . . ?
N4B C9B C12B C13B 87.9(7) . . . . ?
C10B C9B C12B C13B -88.8(7) . . . . ?
N4B C9B C12B C14B -151.4(5) . . . . ?
C10B C9B C12B C14B 31.9(7) . . . . ?
C9A C12A C15A O2A -67.4(4) . . . . ?
C13A C12A C15A O2A 53.9(4) . . . . ?
C14A C12A C15A O2A 173.9(3) . . . . ?
C13B C12B C15B O2B 61.7(7) . . . . ?
C14B C12B C15B O2B -58.4(7) . . . . ?
C9B C12B C15B O2B -178.8(5) . . . . ?
N6A C17A C18A C19A 1.6(4) . . . . ?
C20A C17A C18A C19A -174.0(4) . . . . ?
N6B C17B C18B C19B -2.1(6) . . . . ?
C20B C17B C18B C19B -179.7(5) . . . . ?
C17A C18A C19A N5A -0.4(5) . . . . ?
C17B C18B C19B N5B 0.8(6) . . . . ?
N6A C17A C20A C23A -28.3(5) . . . . ?
C18A C17A C20A C23A 146.8(4) . . . . ?
N6A C17A C20A C22A 95.0(4) . . . . ?
C18A C17A C20A C22A -89.9(5) . . . . ?
N6A C17A C20A C21A -143.3(4) . . . . ?
C18A C17A C20A C21A 31.8(6) . . . . ?
C17A C20A C23A O3A 69.4(4) . . . . ?
C22A C20A C23A O3A -53.6(4) . . . . ?
C21A C20A C23A O3A -173.2(4) . . . . ?
N6B C17B C20B C23B 110.3(7) . . . . ?
C18B C17B C20B C23B -72.5(8) . . . . ?
N6B C17B C20B C21B -21.7(7) . . . . ?
C18B C17B C20B C21B 155.5(5) . . . . ?
N6B C17B C20B C22B -134.8(6) . . . . ?
C18B C17B C20B C22B 42.4(8) . . . . ?
C17B C20B C23B O3C -149.2(15) . . . . ?
C21B C20B C23B O3C -19.3(18) . . . . ?
C22B C20B C23B O3C 92.7(16) . . . . ?
C17B C20B C23B O3B -67.6(9) . . . . ?
C21B C20B C23B O3B 62.2(10) . . . . ?
C22B C20B C23B O3B 174.2(7) . . . . ?
C2A C3A N1A N2A -0.1(4) . . . . ?
C2A C3A N1A B1A 175.8(3) . . . . ?
N5A B1A N1A C3A -120.0(4) . . . . ?
N3A B1A N1A C3A 121.6(4) . . . . ?
N5A B1A N1A N2A 55.5(4) . . . . ?
N3A B1A N1A N2A -62.9(4) . . . . ?
C2B C3B N1B N2B 2.3(6) . . . . ?
C2B C3B N1B B1B -177.9(4) . . . . ?
N5B B1B N1B C3B 114.1(5) . . . . ?
N3B B1B N1B C3B -5.1(6) . . . . ?
N5B B1B N1B N2B -66.1(5) . . . . ?
N3B B1B N1B N2B 174.8(4) . . . . ?
C2A C1A N2A N1A 0.1(4) . . . . ?
C4A C1A N2A N1A 178.6(3) . . . . ?
C2A C1A N2A Mg 178.9(3) . . . . ?
C4A C1A N2A Mg -2.6(6) . . . . ?
C3A N1A N2A C1A 0.0(4) . . . . ?
B1A N1A N2A C1A -176.3(3) . . . . ?
C3A N1A N2A Mg -179.1(2) . . . . ?
B1A N1A N2A Mg 4.7(4) . . . . ?
O3A Mg N2A C1A 74.8(4) . . . . ?
O1A Mg N2A C1A 15.2(4) . . . . ?
O2A Mg N2A C1A -63.2(4) . . . . ?
N6A Mg N2A C1A 138.7(4) . . . . ?
N4A Mg N2A C1A -137.3(4) . . . . ?
O3A Mg N2A N1A -106.5(3) . . . . ?
O1A Mg N2A N1A -166.2(3) . . . . ?
O2A Mg N2A N1A 115.5(2) . . . . ?
N6A Mg N2A N1A -42.6(2) . . . . ?
N4A Mg N2A N1A 41.4(2) . . . . ?
C2B C1B N2B N1B 1.8(6) . . . . ?
C4B C1B N2B N1B -179.8(5) . . . . ?
C3B N1B N2B C1B -2.5(5) . . . . ?
B1B N1B N2B C1B 177.6(4) . . . . ?
C10A C11A N3A N4A 0.3(4) . . . . ?
C10A C11A N3A B1A 176.1(4) . . . . ?
N5A B1A N3A C11A 122.5(4) . . . . ?
N1A B1A N3A C11A -118.7(4) . . . . ?
N5A B1A N3A N4A -62.2(4) . . . . ?
N1A B1A N3A N4A 56.6(4) . . . . ?
C10B C11B N3B N4B -0.8(5) . . . . ?
C10B C11B N3B B1B -159.7(4) . . . . ?
N5B B1B N3B C11B -35.7(6) . . . . ?
N1B B1B N3B C11B 82.4(6) . . . . ?
N5B B1B N3B N4B 166.9(4) . . . . ?
N1B B1B N3B N4B -75.0(5) . . . . ?
C10A C9A N4A N3A -0.2(4) . . . . ?
C12A C9A N4A N3A 177.9(3) . . . . ?
C10A C9A N4A Mg 176.8(3) . . . . ?
C12A C9A N4A Mg -5.0(5) . . . . ?
C11A N3A N4A C9A -0.1(4) . . . . ?
B1A N3A N4A C9A -176.2(3) . . . . ?
C11A N3A N4A Mg -177.8(2) . . . . ?
B1A N3A N4A Mg 6.1(4) . . . . ?
O3A Mg N4A C9A -61.2(4) . . . . ?
O1A Mg N4A C9A 81.3(4) . . . . ?
O2A Mg N4A C9A 13.7(3) . . . . ?
N6A Mg N4A C9A -135.6(4) . . . . ?
N2A Mg N4A C9A 136.4(4) . . . . ?
O3A Mg N4A N3A 115.7(2) . . . . ?
O1A Mg N4A N3A -101.9(3) . . . . ?
O2A Mg N4A N3A -169.5(2) . . . . ?
N6A Mg N4A N3A 41.2(2) . . . . ?
N2A Mg N4A N3A -46.7(2) . . . . ?
C10B C9B N4B N3B 0.9(5) . . . . ?
C12B C9B N4B N3B -176.4(4) . . . . ?
C11B N3B N4B C9B 0.0(5) . . . . ?
B1B N3B N4B C9B 161.4(4) . . . . ?
C18A C19A N5A N6A -0.8(4) . . . . ?
C18A C19A N5A B1A 170.7(4) . . . . ?
N1A B1A N5A C19A 121.4(4) . . . . ?
N3A B1A N5A C19A -120.5(4) . . . . ?
N1A B1A N5A N6A -68.0(4) . . . . ?
N3A B1A N5A N6A 50.1(4) . . . . ?
C18B C19B N5B N6B 0.8(6) . . . . ?
C18B C19B N5B B1B 177.6(4) . . . . ?
N1B B1B N5B C19B -22.9(6) . . . . ?
N3B B1B N5B C19B 92.8(5) . . . . ?
N1B B1B N5B N6B 153.5(4) . . . . ?
N3B B1B N5B N6B -90.7(5) . . . . ?
C18A C17A N6A N5A -2.1(4) . . . . ?
C20A C17A N6A N5A 173.9(3) . . . . ?
C18A C17A N6A Mg 172.7(3) . . . . ?
C20A C17A N6A Mg -11.3(5) . . . . ?
C19A N5A N6A C17A 1.8(4) . . . . ?
B1A N5A N6A C17A -170.5(3) . . . . ?
C19A N5A N6A Mg -174.2(2) . . . . ?
B1A N5A N6A Mg 13.5(4) . . . . ?
O3A Mg N6A C17A 12.0(3) . . . . ?
O1A Mg N6A C17A -68.6(4) . . . . ?
O2A Mg N6A C17A 72.8(4) . . . . ?
N4A Mg N6A C17A 134.2(4) . . . . ?
N2A Mg N6A C17A -141.3(4) . . . . ?
O3A Mg N6A N5A -173.6(2) . . . . ?
O1A Mg N6A N5A 105.8(2) . . . . ?
O2A Mg N6A N5A -112.8(3) . . . . ?
N4A Mg N6A N5A -51.4(2) . . . . ?
N2A Mg N6A N5A 33.0(2) . . . . ?
C18B C17B N6B N5B 2.6(5) . . . . ?
C20B C17B N6B N5B -179.7(4) . . . . ?
C19B N5B N6B C17B -2.1(5) . . . . ?
B1B N5B N6B C17B -179.1(4) . . . . ?
C4A C7A O1A C8A -96.0(5) . . . . ?
C4A C7A O1A Mg 86.1(4) . . . . ?
O3A Mg O1A C7A 155.7(3) . . . . ?
O2A Mg O1A C7A 73.0(3) . . . . ?
N6A Mg O1A C7A -127.9(3) . . . . ?
N4A Mg O1A C7A 7.5(4) . . . . ?
N2A Mg O1A C7A -49.5(3) . . . . ?
O3A Mg O1A C8A -21.6(5) . . . . ?
O2A Mg O1A C8A -104.2(5) . . . . ?
N6A Mg O1A C8A 54.9(6) . . . . ?
N4A Mg O1A C8A -169.8(5) . . . . ?
N2A Mg O1A C8A 133.3(6) . . . . ?
C4B C7B O1B C8B -159.7(8) . . . . ?
C12A C15A O2A C16A -101.3(4) . . . . ?
C12A C15A O2A Mg 85.9(3) . . . . ?
O3A Mg O2A C16A -94.6(4) . . . . ?
O1A Mg O2A C16A -6.8(4) . . . . ?
N6A Mg O2A C16A -154.7(4) . . . . ?
N4A Mg O2A C16A 142.7(5) . . . . ?
N2A Mg O2A C16A 66.0(5) . . . . ?
O3A Mg O2A C15A 76.1(2) . . . . ?
O1A Mg O2A C15A 163.9(2) . . . . ?
N6A Mg O2A C15A 16.0(3) . . . . ?
N4A Mg O2A C15A -46.6(2) . . . . ?
N2A Mg O2A C15A -123.3(2) . . . . ?
C12B C15B O2B C16B -173.8(5) . . . . ?
C20A C23A O3A C24A 121.6(4) . . . . ?
C20A C23A O3A Mg -72.4(4) . . . . ?
O1A Mg O3A C24A -44.5(3) . . . . ?
O2A Mg O3A C24A 42.7(3) . . . . ?
N6A Mg O3A C24A -167.5(3) . . . . ?
N4A Mg O3A C24A 115.9(3) . . . . ?
N2A Mg O3A C24A -101.8(4) . . . . ?
O1A Mg O3A C23A 151.3(3) . . . . ?
O2A Mg O3A C23A -121.4(3) . . . . ?
N6A Mg O3A C23A 28.4(3) . . . . ?
N4A Mg O3A C23A -48.2(3) . . . . ?
N2A Mg O3A C23A 94.0(3) . . . . ?
O3C C23B O3B C24B -64.2(12) . . . . ?
C20B C23B O3B C24B 174.9(9) . . . . ?
O3B C23B O3C C24C 68(2) . . . . ?
C20B C23B O3C C24C 175.1(16) . . . . ?

#END OF CIF