# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_C157
_database_code_depnum_ccdc_archive 'CCDC 1967134'
loop_
_audit_author_name
_audit_author_address
'Jianhua Cheng'
;CIAC, CAS
China
;
_audit_update_record             
;
2019-11-21 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[(TpAd,iPr)Ca(p-CH2C6H4CH3)(THF)]'
_chemical_melting_point          ?
_chemical_formula_moiety         "'C120 H174 B2 Ca2 N12 O2"
_chemical_formula_sum            'C120 H174 B2 Ca2 N12 O2'
_chemical_formula_weight         1918.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

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

_cell_length_a                   15.552(3)
_cell_length_b                   15.578(3)
_cell_length_c                   45.215(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.580(4)
_cell_angle_gamma                90
_cell_volume                     10953(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2360
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      18.13

_exptl_crystal_description       Fragment
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_F_000             4176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.160
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53094
_diffrn_reflns_av_unetI/netI     0.2220
_diffrn_reflns_av_R_equivalents  0.1639
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         1.383
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             19243
_reflns_number_gt                7587
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2018/2)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0952P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19243
_refine_ls_number_parameters     1167
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.2307
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.2495
_refine_ls_wR_factor_gt          0.1914
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2605(4) 0.7023(4) 0.13695(12) 0.0342(16) Uani 1 1 d . . . . .
H1A H 0.309808 0.663708 0.141011 0.041 Uiso 1 1 calc R U . . .
H1B H 0.278096 0.745131 0.121989 0.041 Uiso 1 1 calc R U . . .
C2 C 0.2341(4) 0.7456(4) 0.16419(14) 0.0405(17) Uani 1 1 d . . . . .
C3 C 0.2521(4) 0.7123(4) 0.19220(14) 0.0413(17) Uani 1 1 d . . . . .
H3 H 0.286056 0.661798 0.193818 0.050 Uiso 1 1 calc R U . . .
C4 C 0.2223(4) 0.7506(4) 0.21772(15) 0.0483(19) Uani 1 1 d . . . . .
H4 H 0.235275 0.724789 0.236257 0.058 Uiso 1 1 calc R U . . .
C5 C 0.1736(5) 0.8260(5) 0.21715(14) 0.053(2) Uani 1 1 d . . . . .
C6 C 0.1416(6) 0.8676(5) 0.24493(16) 0.079(3) Uani 1 1 d . . . . .
H6A H 0.157683 0.832337 0.262047 0.119 Uiso 1 1 calc R U . . .
H6B H 0.167317 0.924770 0.246996 0.119 Uiso 1 1 calc R U . . .
H6C H 0.078837 0.872966 0.243845 0.119 Uiso 1 1 calc R U . . .
C7 C 0.1601(5) 0.8618(4) 0.18954(15) 0.053(2) Uani 1 1 d . . . . .
H7 H 0.130716 0.915105 0.188100 0.064 Uiso 1 1 calc R U . . .
C8 C 0.1880(5) 0.8223(4) 0.16380(15) 0.0493(19) Uani 1 1 d . . . . .
H8 H 0.175321 0.848507 0.145301 0.059 Uiso 1 1 calc R U . . .
C9 C 0.0224(5) 0.6703(6) 0.18124(16) 0.0777(13) Uani 1 1 d . . . . .
H9A H 0.079884 0.684066 0.189585 0.093 Uiso 1 1 calc R U . . .
H9B H 0.007092 0.611008 0.187070 0.093 Uiso 1 1 calc R U . . .
C10 C -0.0428(5) 0.7322(6) 0.19213(16) 0.0777(13) Uani 1 1 d . . . . .
H10A H -0.076192 0.706755 0.208475 0.093 Uiso 1 1 calc R U . . .
H10B H -0.014826 0.785393 0.199323 0.093 Uiso 1 1 calc R U . . .
C11 C -0.0988(5) 0.7504(6) 0.16664(16) 0.0777(13) Uani 1 1 d . . . . .
H11A H -0.151313 0.714436 0.167217 0.093 Uiso 1 1 calc R U . . .
H11B H -0.116012 0.811556 0.166384 0.093 Uiso 1 1 calc R U . . .
C12 C -0.0497(5) 0.7305(6) 0.14189(16) 0.0777(13) Uani 1 1 d . . . . .
H12A H -0.029588 0.784414 0.132666 0.093 Uiso 1 1 calc R U . . .
H12B H -0.086257 0.700015 0.127237 0.093 Uiso 1 1 calc R U . . .
C21 C -0.2033(5) 0.5369(5) 0.12022(17) 0.066(2) Uani 1 1 d . . . . .
H21A H -0.262104 0.530662 0.112533 0.099 Uiso 1 1 calc R U . . .
H21B H -0.204249 0.568809 0.138889 0.099 Uiso 1 1 calc R U . . .
H21C H -0.168468 0.568076 0.105829 0.099 Uiso 1 1 calc R U . . .
C22 C -0.2222(4) 0.3959(5) 0.14584(16) 0.063(2) Uani 1 1 d . . . . .
H22A H -0.280595 0.393670 0.137496 0.094 Uiso 1 1 calc R U . . .
H22B H -0.199281 0.337540 0.147609 0.094 Uiso 1 1 calc R U . . .
H22C H -0.223702 0.422722 0.165437 0.094 Uiso 1 1 calc R U . . .
C23 C -0.1647(4) 0.4487(4) 0.12551(15) 0.0446(17) Uani 1 1 d . . . . .
H23 H -0.162593 0.418604 0.106004 0.054 Uiso 1 1 calc R U . . .
C24 C -0.0745(4) 0.4541(4) 0.13732(13) 0.0337(15) Uani 1 1 d . . . . .
C25 C -0.0427(4) 0.4350(4) 0.16531(14) 0.0416(17) Uani 1 1 d . . . . .
H25 H -0.073962 0.414328 0.181801 0.050 Uiso 1 1 calc R U . . .
C26 C 0.0461(4) 0.4528(4) 0.16399(14) 0.0371(16) Uani 1 1 d . . . . .
C27 C 0.1154(6) 0.4354(6) 0.1865(2) 0.0878(10) Uani 1 1 d . . . . .
C28 C 0.1985(5) 0.4849(6) 0.17997(19) 0.0878(10) Uani 1 1 d . . . . .
H28A H 0.187216 0.547427 0.180920 0.105 Uiso 1 1 calc R U . . .
H28B H 0.218164 0.471007 0.159784 0.105 Uiso 1 1 calc R U . . .
C29 C 0.0870(6) 0.4589(6) 0.21758(18) 0.0878(10) Uani 1 1 d . . . . .
H29A H 0.034517 0.426206 0.222577 0.105 Uiso 1 1 calc R U . . .
H29B H 0.073046 0.520821 0.218402 0.105 Uiso 1 1 calc R U . . .
C30 C 0.1372(6) 0.3414(6) 0.18489(19) 0.0878(10) Uani 1 1 d . . . . .
H30A H 0.160165 0.327767 0.165105 0.105 Uiso 1 1 calc R U . . .
H30B H 0.084629 0.306780 0.187885 0.105 Uiso 1 1 calc R U . . .
C31 C 0.2066(6) 0.3183(6) 0.20953(19) 0.0878(10) Uani 1 1 d . . . . .
H31 H 0.218428 0.255226 0.209718 0.105 Uiso 1 1 calc R U . . .
C32 C 0.1730(6) 0.3468(6) 0.23852(19) 0.0878(10) Uani 1 1 d . . . . .
H32A H 0.117440 0.317796 0.242051 0.105 Uiso 1 1 calc R U . . .
H32B H 0.213638 0.328376 0.254270 0.105 Uiso 1 1 calc R U . . .
C33 C 0.1605(6) 0.4379(6) 0.2408(2) 0.0878(10) Uani 1 1 d . . . . .
H33 H 0.142265 0.453808 0.261240 0.105 Uiso 1 1 calc R U . . .
C34 C 0.2392(6) 0.4858(6) 0.23245(18) 0.0878(10) Uani 1 1 d . . . . .
H34A H 0.226983 0.548169 0.232701 0.105 Uiso 1 1 calc R U . . .
H34B H 0.285398 0.474261 0.247148 0.105 Uiso 1 1 calc R U . . .
C35 C 0.2689(6) 0.4607(6) 0.20270(19) 0.0878(10) Uani 1 1 d . . . . .
H35 H 0.322643 0.493059 0.198064 0.105 Uiso 1 1 calc R U . . .
C36 C 0.2868(6) 0.3683(5) 0.20140(19) 0.0878(10) Uani 1 1 d . . . . .
H36A H 0.334162 0.353830 0.215311 0.105 Uiso 1 1 calc R U . . .
H36B H 0.304888 0.352418 0.181197 0.105 Uiso 1 1 calc R U . . .
C41 C -0.2346(5) 0.5678(5) 0.03081(18) 0.076(3) Uani 1 1 d . . . . .
H41A H -0.274520 0.525234 0.022527 0.114 Uiso 1 1 calc R U . . .
H41B H -0.259552 0.593293 0.048586 0.114 Uiso 1 1 calc R U . . .
H41C H -0.224373 0.612897 0.016140 0.114 Uiso 1 1 calc R U . . .
C42 C -0.1112(5) 0.4786(5) 0.01267(17) 0.070(2) Uani 1 1 d . . . . .
H42A H -0.057013 0.451836 0.018930 0.105 Uiso 1 1 calc R U . . .
H42B H -0.150930 0.434321 0.005452 0.105 Uiso 1 1 calc R U . . .
H42C H -0.100108 0.519893 -0.003203 0.105 Uiso 1 1 calc R U . . .
C43 C -0.1509(4) 0.5249(5) 0.03873(15) 0.053(2) Uani 1 1 d . . . . .
H43 H -0.162924 0.481087 0.054315 0.063 Uiso 1 1 calc R U . . .
C44 C -0.0879(4) 0.5885(4) 0.05155(14) 0.0424(17) Uani 1 1 d . . . . .
C45 C -0.0784(4) 0.6737(4) 0.04531(14) 0.0501(19) Uani 1 1 d . . . . .
H45 H -0.113483 0.706594 0.032248 0.060 Uiso 1 1 calc R U . . .
C46 C -0.0081(4) 0.7036(4) 0.06155(14) 0.0368(16) Uani 1 1 d . . . . .
C47 C 0.0291(4) 0.7922(4) 0.06166(13) 0.0329(15) Uani 1 1 d . . . . .
C48 C 0.1095(4) 0.8005(4) 0.08125(12) 0.0351(16) Uani 1 1 d . . . . .
H48A H 0.153643 0.759284 0.074535 0.042 Uiso 1 1 calc R U . . .
H48B H 0.094827 0.786056 0.101922 0.042 Uiso 1 1 calc R U . . .
C49 C 0.0553(4) 0.8161(4) 0.02978(13) 0.0416(17) Uani 1 1 d . . . . .
H49A H 0.098931 0.774889 0.022683 0.050 Uiso 1 1 calc R U . . .
H49B H 0.004442 0.812232 0.016505 0.050 Uiso 1 1 calc R U . . .
C50 C -0.0375(4) 0.8594(4) 0.07177(15) 0.0489(19) Uani 1 1 d . . . . .
H50A H -0.089205 0.855940 0.058851 0.059 Uiso 1 1 calc R U . . .
H50B H -0.055277 0.846291 0.092252 0.059 Uiso 1 1 calc R U . . .
C51 C -0.0012(5) 0.9490(4) 0.07060(16) 0.0516(19) Uani 1 1 d . . . . .
H51 H -0.045433 0.990931 0.077432 0.062 Uiso 1 1 calc R U . . .
C52 C 0.0247(5) 0.9706(4) 0.03870(15) 0.053(2) Uani 1 1 d . . . . .
H52A H -0.026239 0.967227 0.025461 0.064 Uiso 1 1 calc R U . . .
H52B H 0.047750 1.029817 0.037830 0.064 Uiso 1 1 calc R U . . .
C53 C 0.0923(4) 0.9078(4) 0.02865(13) 0.0406(17) Uani 1 1 d . . . . .
H53 H 0.108644 0.921542 0.007841 0.049 Uiso 1 1 calc R U . . .
C54 C 0.1713(4) 0.9133(4) 0.04829(13) 0.0429(17) Uani 1 1 d . . . . .
H54A H 0.196025 0.971757 0.047340 0.051 Uiso 1 1 calc R U . . .
H54B H 0.215301 0.872041 0.041455 0.051 Uiso 1 1 calc R U . . .
C55 C 0.1462(4) 0.8924(4) 0.08006(13) 0.0390(16) Uani 1 1 d . . . . .
H55 H 0.198151 0.896376 0.093210 0.047 Uiso 1 1 calc R U . . .
C56 C 0.0786(4) 0.9551(4) 0.09052(15) 0.0482(18) Uani 1 1 d . . . . .
H56A H 0.101846 1.014246 0.089973 0.058 Uiso 1 1 calc R U . . .
H56B H 0.062962 0.941764 0.111187 0.058 Uiso 1 1 calc R U . . .
C61 C 0.0215(4) 0.2629(4) 0.08964(15) 0.055(2) Uani 1 1 d . . . . .
H61A H -0.018596 0.215368 0.086091 0.083 Uiso 1 1 calc R U . . .
H61B H 0.072310 0.241576 0.100323 0.083 Uiso 1 1 calc R U . . .
H61C H -0.006768 0.307185 0.101478 0.083 Uiso 1 1 calc R U . . .
C62 C 0.0877(5) 0.2324(4) 0.04044(16) 0.064(2) Uani 1 1 d . . . . .
H62A H 0.046271 0.185543 0.037793 0.096 Uiso 1 1 calc R U . . .
H62B H 0.101468 0.257109 0.021122 0.096 Uiso 1 1 calc R U . . .
H62C H 0.140245 0.210192 0.049781 0.096 Uiso 1 1 calc R U . . .
C63 C 0.0489(4) 0.3013(4) 0.05998(14) 0.0434(18) Uani 1 1 d . . . . .
H63 H -0.003626 0.324153 0.049760 0.052 Uiso 1 1 calc R U . . .
C64 C 0.1107(5) 0.3747(4) 0.06459(12) 0.0358(16) Uani 1 1 d . . . . .
C65 C 0.1967(4) 0.3773(4) 0.05911(12) 0.0333(15) Uani 1 1 d . . . . .
H65 H 0.230801 0.333402 0.050562 0.040 Uiso 1 1 calc R U . . .
C66 C 0.2245(4) 0.4584(4) 0.06871(12) 0.0296(15) Uani 1 1 d . . . . .
C67 C 0.3140(4) 0.4956(3) 0.06850(12) 0.0283(14) Uani 1 1 d . . . . .
C68 C 0.3499(4) 0.5050(4) 0.10019(12) 0.0385(16) Uani 1 1 d . . . . .
H68A H 0.311969 0.543290 0.111688 0.046 Uiso 1 1 calc R U . . .
H68B H 0.350786 0.448162 0.109969 0.046 Uiso 1 1 calc R U . . .
C69 C 0.3147(4) 0.5842(4) 0.05369(13) 0.0372(16) Uani 1 1 d . . . . .
H69A H 0.292032 0.579188 0.033219 0.045 Uiso 1 1 calc R U . . .
H69B H 0.276599 0.623652 0.064673 0.045 Uiso 1 1 calc R U . . .
C70 C 0.3747(4) 0.4357(4) 0.05124(13) 0.0380(16) Uani 1 1 d . . . . .
H70A H 0.375875 0.378307 0.060659 0.046 Uiso 1 1 calc R U . . .
H70B H 0.353234 0.428861 0.030685 0.046 Uiso 1 1 calc R U . . .
C71 C 0.4664(4) 0.4736(4) 0.05097(14) 0.0436(18) Uani 1 1 d . . . . .
H71 H 0.505065 0.434400 0.039716 0.052 Uiso 1 1 calc R U . . .
C72 C 0.4647(4) 0.5612(4) 0.03601(14) 0.0483(18) Uani 1 1 d . . . . .
H72A H 0.443677 0.555207 0.015366 0.058 Uiso 1 1 calc R U . . .
H72B H 0.523477 0.585459 0.035570 0.058 Uiso 1 1 calc R U . . .
C73 C 0.4054(4) 0.6213(4) 0.05306(14) 0.0445(17) Uani 1 1 d . . . . .
H73 H 0.404193 0.678817 0.043277 0.053 Uiso 1 1 calc R U . . .
C74 C 0.4398(4) 0.6305(4) 0.08471(14) 0.0438(18) Uani 1 1 d . . . . .
H74A H 0.402689 0.670340 0.095904 0.053 Uiso 1 1 calc R U . . .
H74B H 0.498637 0.654600 0.084411 0.053 Uiso 1 1 calc R U . . .
C75 C 0.4411(4) 0.5422(4) 0.09994(13) 0.0396(17) Uani 1 1 d . . . . .
H75 H 0.463027 0.548397 0.120696 0.048 Uiso 1 1 calc R U . . .
C76 C 0.5000(4) 0.4823(4) 0.08273(14) 0.0472(18) Uani 1 1 d . . . . .
H76A H 0.501636 0.425152 0.092312 0.057 Uiso 1 1 calc R U . . .
H76B H 0.559207 0.505701 0.082668 0.057 Uiso 1 1 calc R U . . .
C101 C 0.7556(4) 0.9176(4) 0.10926(12) 0.0337(15) Uani 1 1 d . . . . .
H10C H 0.804420 0.957892 0.107226 0.040 Uiso 1 1 calc R U . . .
H10D H 0.773708 0.870955 0.122825 0.040 Uiso 1 1 calc R U . . .
C102 C 0.7344(4) 0.8821(4) 0.08095(14) 0.0373(16) Uani 1 1 d . . . . .
C103 C 0.6895(5) 0.8053(4) 0.07832(16) 0.054(2) Uani 1 1 d . . . . .
H103 H 0.676645 0.773364 0.095616 0.065 Uiso 1 1 calc R U . . .
C104 C 0.6626(5) 0.7739(5) 0.0505(2) 0.064(2) Uani 1 1 d . . . . .
H104 H 0.629823 0.722483 0.049470 0.077 Uiso 1 1 calc R U . . .
C105 C 0.6828(5) 0.8162(6) 0.02465(17) 0.063(2) Uani 1 1 d . . . . .
C106 C 0.6526(6) 0.7816(6) -0.00505(19) 0.107(4) Uani 1 1 d . . . . .
H10E H 0.620455 0.728182 -0.002053 0.160 Uiso 1 1 calc R U . . .
H10F H 0.615229 0.823942 -0.014760 0.160 Uiso 1 1 calc R U . . .
H10G H 0.702451 0.770156 -0.017524 0.160 Uiso 1 1 calc R U . . .
C107 C 0.7291(5) 0.8901(5) 0.02680(16) 0.055(2) Uani 1 1 d . . . . .
H107 H 0.744672 0.919681 0.009261 0.066 Uiso 1 1 calc R U . . .
C108 C 0.7543(4) 0.9235(4) 0.05422(15) 0.0431(17) Uani 1 1 d . . . . .
H108 H 0.785903 0.975707 0.054844 0.052 Uiso 1 1 calc R U . . .
C109 C 0.5201(4) 0.9535(4) 0.06604(14) 0.0493(19) Uani 1 1 d . . . . .
H10H H 0.577288 0.942175 0.057452 0.059 Uiso 1 1 calc R U . . .
H10I H 0.503875 1.013785 0.061930 0.059 Uiso 1 1 calc R U . . .
C110 C 0.4541(5) 0.8929(5) 0.05358(17) 0.071(2) Uani 1 1 d . . . . .
H11C H 0.424962 0.918147 0.036066 0.086 Uiso 1 1 calc R U . . .
H11D H 0.480924 0.837817 0.047790 0.086 Uiso 1 1 calc R U . . .
C111 C 0.3931(5) 0.8800(5) 0.07775(15) 0.059(2) Uani 1 1 d . . . . .
H11E H 0.364570 0.823408 0.076091 0.071 Uiso 1 1 calc R U . . .
H11F H 0.348687 0.925521 0.077721 0.071 Uiso 1 1 calc R U . . .
C112 C 0.4470(5) 0.8847(5) 0.10464(16) 0.070(2) Uani 1 1 d . . . . .
H11G H 0.414384 0.910921 0.121014 0.083 Uiso 1 1 calc R U . . .
H11H H 0.465402 0.826430 0.110763 0.083 Uiso 1 1 calc R U . . .
C121 C 0.2890(5) 1.0786(6) 0.1271(2) 0.0952(19) Uani 1 1 d . . . . .
H12C H 0.273023 1.061316 0.106979 0.143 Uiso 1 1 calc R U . . .
H12D H 0.237328 1.080941 0.139355 0.143 Uiso 1 1 calc R U . . .
H12E H 0.329452 1.036762 0.135539 0.143 Uiso 1 1 calc R U . . .
C122 C 0.2772(5) 1.2303(6) 0.1114(2) 0.0952(19) Uani 1 1 d . . . . .
H12F H 0.307423 1.285474 0.111667 0.143 Uiso 1 1 calc R U . . .
H12G H 0.222162 1.236136 0.121561 0.143 Uiso 1 1 calc R U . . .
H12H H 0.266628 1.212765 0.090828 0.143 Uiso 1 1 calc R U . . .
C123 C 0.3302(5) 1.1649(6) 0.1265(2) 0.0952(19) Uani 1 1 d . . . . .
H123 H 0.335522 1.183838 0.147524 0.114 Uiso 1 1 calc R U . . .
C124 C 0.4191(4) 1.1599(4) 0.11506(14) 0.0374(16) Uani 1 1 d . . . . .
C125 C 0.4531(4) 1.1867(4) 0.08843(13) 0.0412(17) Uani 1 1 d . . . . .
H125 H 0.422789 1.212293 0.072363 0.049 Uiso 1 1 calc R U . . .
C126 C 0.5415(4) 1.1682(4) 0.08995(13) 0.0316(15) Uani 1 1 d . . . . .
C127 C 0.6129(4) 1.1924(3) 0.06982(12) 0.0306(15) Uani 1 1 d . . . . .
C128 C 0.6946(4) 1.1403(4) 0.07563(15) 0.0491(19) Uani 1 1 d . . . . .
H12I H 0.682850 1.078753 0.071877 0.059 Uiso 1 1 calc R U . . .
H12J H 0.712176 1.146629 0.096619 0.059 Uiso 1 1 calc R U . . .
C129 C 0.6351(5) 1.2870(4) 0.07572(16) 0.056(2) Uani 1 1 d . . . . .
H12K H 0.651807 1.294065 0.096761 0.067 Uiso 1 1 calc R U . . .
H12L H 0.583515 1.322778 0.071930 0.067 Uiso 1 1 calc R U . . .
C130 C 0.5860(5) 1.1849(5) 0.03693(14) 0.063(2) Uani 1 1 d . . . . .
H13A H 0.534810 1.221174 0.033010 0.076 Uiso 1 1 calc R U . . .
H13B H 0.570856 1.124707 0.032227 0.076 Uiso 1 1 calc R U . . .
C131 C 0.6625(5) 1.2151(5) 0.01697(15) 0.061(2) Uani 1 1 d . . . . .
H131 H 0.646613 1.208890 -0.004411 0.073 Uiso 1 1 calc R U . . .
C132 C 0.6803(5) 1.3090(5) 0.02430(16) 0.064(2) Uani 1 1 d . . . . .
H13C H 0.725587 1.331347 0.011140 0.077 Uiso 1 1 calc R U . . .
H13D H 0.627489 1.343255 0.020889 0.077 Uiso 1 1 calc R U . . .
C133 C 0.7089(5) 1.3180(4) 0.05603(17) 0.059(2) Uani 1 1 d . . . . .
H133 H 0.722278 1.379489 0.060470 0.071 Uiso 1 1 calc R U . . .
C134 C 0.7868(5) 1.2632(5) 0.06226(16) 0.058(2) Uani 1 1 d . . . . .
H13E H 0.835275 1.283057 0.050008 0.070 Uiso 1 1 calc R U . . .
H13F H 0.803857 1.269199 0.083313 0.070 Uiso 1 1 calc R U . . .
C135 C 0.7683(5) 1.1706(5) 0.05559(16) 0.057(2) Uani 1 1 d . . . . .
H135 H 0.820875 1.135304 0.059504 0.069 Uiso 1 1 calc R U . . .
C136 C 0.7402(5) 1.1598(5) 0.02428(16) 0.061(2) Uani 1 1 d . . . . .
H13G H 0.725734 1.098770 0.020662 0.073 Uiso 1 1 calc R U . . .
H13H H 0.788051 1.175495 0.011073 0.073 Uiso 1 1 calc R U . . .
C141 C 0.5163(5) 1.3477(4) 0.16316(15) 0.058(2) Uani 1 1 d . . . . .
H14A H 0.474270 1.393141 0.166855 0.088 Uiso 1 1 calc R U . . .
H14B H 0.568563 1.372834 0.154853 0.088 Uiso 1 1 calc R U . . .
H14C H 0.491958 1.306085 0.149137 0.088 Uiso 1 1 calc R U . . .
C142 C 0.5726(5) 1.3662(4) 0.21522(16) 0.062(2) Uani 1 1 d . . . . .
H14D H 0.530035 1.411632 0.218200 0.092 Uiso 1 1 calc R U . . .
H14E H 0.583224 1.336203 0.233965 0.092 Uiso 1 1 calc R U . . .
H14F H 0.626411 1.391496 0.208246 0.092 Uiso 1 1 calc R U . . .
C143 C 0.5386(4) 1.3023(4) 0.19219(13) 0.0382(16) Uani 1 1 d . . . . .
H143 H 0.484824 1.275832 0.200006 0.046 Uiso 1 1 calc R U . . .
C144 C 0.6041(4) 1.2310(4) 0.18724(12) 0.0306(15) Uani 1 1 d . . . . .
C145 C 0.6916(4) 1.2319(4) 0.19101(12) 0.0317(15) Uani 1 1 d . . . . .
H145 H 0.725411 1.277336 0.199001 0.038 Uiso 1 1 calc R U . . .
C146 C 0.7210(4) 1.1535(4) 0.18083(12) 0.0285(15) Uani 1 1 d . . . . .
C147 C 0.8127(4) 1.1210(4) 0.17967(12) 0.0270(14) Uani 1 1 d . . . . .
C148 C 0.8698(4) 1.1768(4) 0.19961(14) 0.0395(17) Uani 1 1 d . . . . .
H14G H 0.848685 1.173996 0.220174 0.047 Uiso 1 1 calc R U . . .
H14H H 0.866420 1.237242 0.192960 0.047 Uiso 1 1 calc R U . . .
C149 C 0.8197(4) 1.0272(4) 0.19042(13) 0.0369(16) Uani 1 1 d . . . . .
H14I H 0.797802 1.023075 0.210856 0.044 Uiso 1 1 calc R U . . .
H14J H 0.783561 0.990033 0.177611 0.044 Uiso 1 1 calc R U . . .
C150 C 0.8478(4) 1.1253(4) 0.14809(12) 0.0360(16) Uani 1 1 d . . . . .
H15A H 0.844917 1.185212 0.140793 0.043 Uiso 1 1 calc R U . . .
H15B H 0.812092 1.089141 0.134814 0.043 Uiso 1 1 calc R U . . .
C151 C 0.9414(4) 1.0939(4) 0.14763(13) 0.0408(17) Uani 1 1 d . . . . .
H151 H 0.962947 1.096937 0.126889 0.049 Uiso 1 1 calc R U . . .
C152 C 0.9968(4) 1.1508(4) 0.16712(14) 0.0488(19) Uani 1 1 d . . . . .
H15C H 0.993934 1.210846 0.159964 0.059 Uiso 1 1 calc R U . . .
H15D H 1.057427 1.131651 0.166369 0.059 Uiso 1 1 calc R U . . .
C153 C 0.9646(4) 1.1460(4) 0.19876(14) 0.0434(18) Uani 1 1 d . . . . .
H153 H 1.000965 1.183217 0.211864 0.052 Uiso 1 1 calc R U . . .
C154 C 0.9667(4) 1.0542(4) 0.20997(13) 0.0472(18) Uani 1 1 d . . . . .
H15E H 0.943842 1.052128 0.230319 0.057 Uiso 1 1 calc R U . . .
H15F H 1.026815 1.033413 0.210583 0.057 Uiso 1 1 calc R U . . .
C155 C 0.9126(4) 0.9960(4) 0.18973(13) 0.0372(16) Uani 1 1 d . . . . .
H155 H 0.915839 0.935279 0.196872 0.045 Uiso 1 1 calc R U . . .
C156 C 0.9465(4) 1.0018(4) 0.15820(13) 0.0408(16) Uani 1 1 d . . . . .
H15G H 1.006934 0.981774 0.157734 0.049 Uiso 1 1 calc R U . . .
H15H H 0.911898 0.964474 0.144954 0.049 Uiso 1 1 calc R U . . .
C161 C 0.2747(9) 1.0293(10) 0.2237(4) 0.063(2) Uani 0.492(7) 1 d D . P A 2
H16A H 0.235804 1.072877 0.231630 0.095 Uiso 0.492(7) 1 calc R U P A 2
H16B H 0.247744 1.002000 0.206382 0.095 Uiso 0.492(7) 1 calc R U P A 2
H16C H 0.286597 0.985881 0.238818 0.095 Uiso 0.492(7) 1 calc R U P A 2
C162 C 0.4051(10) 1.1200(9) 0.2405(3) 0.063(2) Uani 0.492(7) 1 d D . P A 2
H16D H 0.365020 1.161669 0.248977 0.095 Uiso 0.492(7) 1 calc R U P A 2
H16E H 0.421663 1.078033 0.255722 0.095 Uiso 0.492(7) 1 calc R U P A 2
H16F H 0.456442 1.149900 0.233559 0.095 Uiso 0.492(7) 1 calc R U P A 2
C163 C 0.3610(9) 1.0730(11) 0.2143(4) 0.063(2) Uani 0.492(7) 1 d D . P A 2
H163 H 0.347507 1.116394 0.198599 0.076 Uiso 0.492(7) 1 calc R U P A 2
C261 C 0.2894(10) 1.0754(10) 0.2080(3) 0.063(2) Uani 0.508(7) 1 d D . P A 1
H26A H 0.253431 1.113089 0.220010 0.095 Uiso 0.508(7) 1 calc R U P A 1
H26B H 0.294915 1.099709 0.188093 0.095 Uiso 0.508(7) 1 calc R U P A 1
H26C H 0.262647 1.018500 0.206601 0.095 Uiso 0.508(7) 1 calc R U P A 1
C262 C 0.3704(10) 1.0365(9) 0.2537(3) 0.063(2) Uani 0.508(7) 1 d D . P A 1
H26D H 0.428355 1.031951 0.262264 0.095 Uiso 0.508(7) 1 calc R U P A 1
H26E H 0.336597 1.077452 0.265266 0.095 Uiso 0.508(7) 1 calc R U P A 1
H26F H 0.342458 0.980092 0.254174 0.095 Uiso 0.508(7) 1 calc R U P A 1
C263 C 0.3760(11) 1.0674(12) 0.2219(3) 0.063(2) Uani 0.508(7) 1 d D . P A 1
H263 H 0.404266 1.125085 0.221808 0.076 Uiso 0.508(7) 1 calc R U P A 1
C164 C 0.4249(4) 1.0084(4) 0.20157(15) 0.0474(19) Uani 1 1 d D . . . .
C165 C 0.4388(5) 0.9236(4) 0.20701(16) 0.060(2) Uani 1 1 d . . . . .
H165 H 0.410756 0.889396 0.221399 0.072 Uiso 1 1 calc R U . . .
C166 C 0.5020(4) 0.8962(4) 0.18748(13) 0.0379(16) Uani 1 1 d . . . . .
C167 C 0.5430(4) 0.8090(4) 0.18555(12) 0.0369(16) Uani 1 1 d . . . . .
C168 C 0.4756(4) 0.7419(4) 0.17592(15) 0.0482(19) Uani 1 1 d . . . . .
H16G H 0.426569 0.743295 0.189712 0.058 Uiso 1 1 calc R U . . .
H16H H 0.453608 0.756217 0.155900 0.058 Uiso 1 1 calc R U . . .
C169 C 0.5782(5) 0.7829(4) 0.21600(14) 0.053(2) Uani 1 1 d . . . . .
H16I H 0.531347 0.785675 0.230627 0.064 Uiso 1 1 calc R U . . .
H16J H 0.623430 0.824050 0.222217 0.064 Uiso 1 1 calc R U . . .
C170 C 0.6170(4) 0.8055(4) 0.16359(14) 0.0425(17) Uani 1 1 d . . . . .
H17A H 0.661251 0.848260 0.169262 0.051 Uiso 1 1 calc R U . . .
H17B H 0.595273 0.820302 0.143572 0.051 Uiso 1 1 calc R U . . .
C171 C 0.6578(4) 0.7149(4) 0.16301(13) 0.0402(17) Uani 1 1 d . . . . .
H171 H 0.706586 0.713295 0.148761 0.048 Uiso 1 1 calc R U . . .
C172 C 0.6896(5) 0.6919(5) 0.19426(15) 0.057(2) Uani 1 1 d . . . . .
H17C H 0.716740 0.634406 0.193997 0.068 Uiso 1 1 calc R U . . .
H17D H 0.733488 0.734019 0.200790 0.068 Uiso 1 1 calc R U . . .
C173 C 0.6160(5) 0.6919(5) 0.21571(15) 0.058(2) Uani 1 1 d . . . . .
H173 H 0.637645 0.676627 0.235931 0.070 Uiso 1 1 calc R U . . .
C174 C 0.5468(5) 0.6291(4) 0.20629(15) 0.060(2) Uani 1 1 d . . . . .
H17E H 0.570348 0.570058 0.206332 0.072 Uiso 1 1 calc R U . . .
H17F H 0.498580 0.631234 0.220401 0.072 Uiso 1 1 calc R U . . .
C175 C 0.5147(5) 0.6517(4) 0.17566(15) 0.0472(18) Uani 1 1 d . . . . .
H175 H 0.469872 0.609307 0.169302 0.057 Uiso 1 1 calc R U . . .
C176 C 0.5879(4) 0.6512(4) 0.15371(15) 0.0515(19) Uani 1 1 d . . . . .
H17G H 0.565544 0.666593 0.133825 0.062 Uiso 1 1 calc R U . . .
H17H H 0.612713 0.592756 0.152591 0.062 Uiso 1 1 calc R U . . .
B1 B -0.0039(5) 0.4799(5) 0.08551(16) 0.0345(19) Uani 1 1 d . . . . .
B2 B 0.4923(5) 1.1215(5) 0.16644(16) 0.0353(18) Uani 1 1 d . . . . .
N1 N -0.0076(3) 0.4808(3) 0.12017(10) 0.0317(12) Uani 1 1 d . . . . .
N2 N 0.0670(3) 0.4812(3) 0.13689(11) 0.0347(13) Uani 1 1 d . . . . .
N3 N -0.0254(3) 0.5682(3) 0.07183(10) 0.0350(13) Uani 1 1 d . . . . .
N4 N 0.0234(3) 0.6402(3) 0.07844(10) 0.0341(13) Uani 1 1 d . . . . .
N5 N 0.0870(3) 0.4512(3) 0.07621(10) 0.0360(13) Uani 1 1 d . . . . .
N6 N 0.1584(3) 0.5033(3) 0.07941(10) 0.0314(12) Uani 1 1 d . . . . .
N7 N 0.4858(3) 1.1271(3) 0.13165(10) 0.0340(13) Uani 1 1 d . . . . .
N8 N 0.5608(3) 1.1317(3) 0.11605(10) 0.0317(12) Uani 1 1 d . . . . .
N9 N 0.5817(3) 1.1542(3) 0.17562(10) 0.0283(12) Uani 1 1 d . . . . .
N10 N 0.6545(3) 1.1051(3) 0.17135(9) 0.0290(12) Uani 1 1 d . . . . .
N11 N 0.4757(3) 1.0310(3) 0.17859(11) 0.0347(13) Uani 1 1 d . . . . .
N12 N 0.5246(3) 0.9624(3) 0.16969(10) 0.0342(13) Uani 1 1 d . . . . .
O1 O 0.0226(3) 0.6785(3) 0.14910(9) 0.0478(12) Uani 1 1 d . . . . .
O2 O 0.5209(3) 0.9368(3) 0.09758(9) 0.0440(12) Uani 1 1 d . . . . .
Ca1 Ca 0.12868(8) 0.61427(7) 0.11763(3) 0.0315(3) Uani 1 1 d . . . . .
Ca2 Ca 0.62640(8) 0.99741(8) 0.13136(2) 0.0302(3) Uani 1 1 d . . . . .
H1B2 H 0.442(3) 1.169(2) 0.1755(8) 0.002(11) Uiso 1 1 d . . . . .
H1B1 H -0.056(3) 0.435(3) 0.0795(9) 0.012(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.466(8) . ?
C1 Ca1 2.610(6) . ?
C2 C8 1.393(8) . ?
C2 C3 1.394(8) . ?
C3 C4 1.383(8) . ?
C4 C5 1.396(9) . ?
C5 C7 1.382(9) . ?
C5 C6 1.503(9) . ?
C7 C8 1.390(8) . ?
C9 O1 1.459(8) . ?
C9 C10 1.487(9) . ?
C10 C11 1.465(10) . ?
C11 C12 1.396(9) . ?
C12 O1 1.421(8) . ?
C21 C23 1.517(9) . ?
C22 C23 1.529(9) . ?
C23 C24 1.498(8) . ?
C24 N1 1.368(7) . ?
C24 C25 1.387(8) . ?
C25 C26 1.411(8) . ?
C26 N2 1.345(7) . ?
C26 C27 1.500(10) . ?
C27 C30 1.504(11) . ?
C27 C29 1.521(11) . ?
C27 C28 1.536(11) . ?
C28 C35 1.541(10) . ?
C29 C33 1.579(10) . ?
C30 C31 1.584(10) . ?
C31 C32 1.484(11) . ?
C31 C36 1.519(11) . ?
C32 C33 1.435(11) . ?
C33 C34 1.486(11) . ?
C34 C35 1.479(11) . ?
C35 C36 1.468(11) . ?
C41 C43 1.504(9) . ?
C42 C43 1.518(9) . ?
C43 C44 1.505(9) . ?
C44 C45 1.365(8) . ?
C44 N3 1.366(8) . ?
C45 C46 1.392(9) . ?
C46 N4 1.338(7) . ?
C46 C47 1.496(8) . ?
C47 C48 1.531(8) . ?
C47 C50 1.545(8) . ?
C47 C49 1.548(8) . ?
C48 C55 1.543(8) . ?
C49 C53 1.541(8) . ?
C50 C51 1.508(9) . ?
C51 C56 1.529(9) . ?
C51 C52 1.539(9) . ?
C52 C53 1.510(8) . ?
C53 C54 1.511(8) . ?
C54 C55 1.527(8) . ?
C55 C56 1.514(8) . ?
C61 C63 1.533(8) . ?
C62 C63 1.518(9) . ?
C63 C64 1.507(8) . ?
C64 N5 1.356(7) . ?
C64 C65 1.364(8) . ?
C65 C66 1.402(7) . ?
C66 N6 1.338(7) . ?
C66 C67 1.508(8) . ?
C67 C69 1.535(7) . ?
C67 C68 1.540(7) . ?
C67 C70 1.545(7) . ?
C68 C75 1.532(8) . ?
C69 C73 1.525(8) . ?
C70 C71 1.544(8) . ?
C71 C72 1.522(8) . ?
C71 C76 1.529(8) . ?
C72 C73 1.528(8) . ?
C73 C74 1.529(8) . ?
C74 C75 1.538(8) . ?
C75 C76 1.527(8) . ?
C101 C102 1.430(8) . ?
C101 Ca2 2.573(6) . ?
C102 C103 1.390(9) . ?
C102 C108 1.407(8) . ?
C103 C104 1.410(9) . ?
C104 C105 1.380(10) . ?
C105 C107 1.361(10) . ?
C105 C106 1.518(10) . ?
C107 C108 1.397(9) . ?
C109 O2 1.449(7) . ?
C109 C110 1.500(9) . ?
C110 C111 1.468(9) . ?
C111 C112 1.471(9) . ?
C112 O2 1.446(7) . ?
C121 C123 1.490(11) . ?
C122 C123 1.474(11) . ?
C123 C124 1.483(10) . ?
C124 N7 1.372(7) . ?
C124 C125 1.384(8) . ?
C125 C126 1.405(8) . ?
C126 N8 1.342(7) . ?
C126 C127 1.491(8) . ?
C127 C128 1.528(8) . ?
C127 C129 1.536(8) . ?
C127 C130 1.545(8) . ?
C128 C135 1.543(9) . ?
C129 C133 1.538(9) . ?
C130 C131 1.573(9) . ?
C131 C136 1.517(10) . ?
C131 C132 1.525(10) . ?
C132 C133 1.504(10) . ?
C133 C134 1.507(9) . ?
C134 C135 1.500(9) . ?
C135 C136 1.487(9) . ?
C141 C143 1.527(8) . ?
C142 C143 1.530(8) . ?
C143 C144 1.526(8) . ?
C144 N9 1.350(7) . ?
C144 C145 1.371(8) . ?
C145 C146 1.385(7) . ?
C146 N10 1.347(7) . ?
C146 C147 1.515(8) . ?
C147 C148 1.529(8) . ?
C147 C150 1.536(7) . ?
C147 C149 1.543(8) . ?
C148 C153 1.552(8) . ?
C149 C155 1.525(8) . ?
C150 C151 1.536(8) . ?
C151 C152 1.514(8) . ?
C151 C156 1.514(8) . ?
C152 C153 1.523(8) . ?
C153 C154 1.517(9) . ?
C154 C155 1.535(8) . ?
C155 C156 1.528(8) . ?
C161 C163 1.567(18) . ?
C162 C163 1.550(17) . ?
C163 C164 1.529(13) . ?
C261 C263 1.487(17) . ?
C262 C263 1.520(17) . ?
C263 C164 1.511(13) . ?
C164 N11 1.358(7) . ?
C164 C165 1.362(9) . ?
C165 C166 1.395(8) . ?
C166 N12 1.356(7) . ?
C166 C167 1.503(8) . ?
C167 C170 1.529(8) . ?
C167 C169 1.532(8) . ?
C167 C168 1.540(8) . ?
C168 C175 1.531(8) . ?
C169 C173 1.535(9) . ?
C170 C171 1.548(8) . ?
C171 C176 1.529(8) . ?
C171 C172 1.535(8) . ?
C172 C173 1.508(9) . ?
C173 C174 1.512(9) . ?
C174 C175 1.509(9) . ?
C175 C176 1.518(9) . ?
B1 N3 1.544(8) . ?
B1 N5 1.546(9) . ?
B1 N1 1.569(8) . ?
B1 Ca1 3.268(7) . ?
B2 N9 1.534(9) . ?
B2 N11 1.535(8) . ?
B2 N7 1.578(8) . ?
B2 Ca2 3.266(8) . ?
N1 N2 1.379(6) . ?
N1 Ca1 2.973(5) . ?
N2 Ca1 2.448(5) . ?
N3 N4 1.386(6) . ?
N4 Ca1 2.434(5) . ?
N5 N6 1.381(6) . ?
N6 Ca1 2.491(5) . ?
N7 N8 1.371(6) . ?
N7 Ca2 2.978(5) . ?
N8 Ca2 2.425(5) . ?
N9 N10 1.383(6) . ?
N10 Ca2 2.502(5) . ?
N11 N12 1.374(6) . ?
N12 Ca2 2.421(5) . ?
O1 Ca1 2.407(4) . ?
O2 Ca2 2.422(4) . ?

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
C2 C1 Ca1 107.2(4) . . ?
C8 C2 C3 115.4(6) . . ?
C8 C2 C1 122.1(6) . . ?
C3 C2 C1 122.5(6) . . ?
C4 C3 C2 122.1(6) . . ?
C3 C4 C5 122.3(6) . . ?
C7 C5 C4 115.7(6) . . ?
C7 C5 C6 122.1(7) . . ?
C4 C5 C6 122.1(7) . . ?
C5 C7 C8 122.1(7) . . ?
C7 C8 C2 122.3(7) . . ?
O1 C9 C10 106.3(6) . . ?
C11 C10 C9 105.5(6) . . ?
C12 C11 C10 105.2(7) . . ?
C11 C12 O1 112.4(7) . . ?
C24 C23 C21 111.9(5) . . ?
C24 C23 C22 111.6(6) . . ?
C21 C23 C22 110.4(6) . . ?
N1 C24 C25 108.5(6) . . ?
N1 C24 C23 122.0(5) . . ?
C25 C24 C23 129.6(6) . . ?
C24 C25 C26 105.0(5) . . ?
N2 C26 C25 110.4(5) . . ?
N2 C26 C27 120.0(6) . . ?
C25 C26 C27 129.2(6) . . ?
C26 C27 C30 107.6(7) . . ?
C26 C27 C29 111.8(7) . . ?
C30 C27 C29 110.3(7) . . ?
C26 C27 C28 112.2(7) . . ?
C30 C27 C28 106.8(8) . . ?
C29 C27 C28 108.1(7) . . ?
C27 C28 C35 110.0(7) . . ?
C27 C29 C33 110.5(8) . . ?
C27 C30 C31 109.8(7) . . ?
C32 C31 C36 110.9(8) . . ?
C32 C31 C30 108.1(8) . . ?
C36 C31 C30 105.6(7) . . ?
C33 C32 C31 114.2(8) . . ?
C32 C33 C34 111.4(9) . . ?
C32 C33 C29 104.7(8) . . ?
C34 C33 C29 108.6(7) . . ?
C35 C34 C33 111.4(8) . . ?
C36 C35 C34 110.9(7) . . ?
C36 C35 C28 110.3(8) . . ?
C34 C35 C28 108.4(8) . . ?
C35 C36 C31 109.7(8) . . ?
C41 C43 C44 111.0(6) . . ?
C41 C43 C42 112.6(6) . . ?
C44 C43 C42 110.1(6) . . ?
C45 C44 N3 106.6(6) . . ?
C45 C44 C43 129.1(6) . . ?
N3 C44 C43 124.2(6) . . ?
C44 C45 C46 107.6(6) . . ?
N4 C46 C45 109.6(5) . . ?
N4 C46 C47 122.7(6) . . ?
C45 C46 C47 127.7(6) . . ?
C46 C47 C48 113.2(5) . . ?
C46 C47 C50 111.5(5) . . ?
C48 C47 C50 108.5(5) . . ?
C46 C47 C49 109.0(5) . . ?
C48 C47 C49 107.3(5) . . ?
C50 C47 C49 107.2(5) . . ?
C47 C48 C55 111.0(5) . . ?
C53 C49 C47 110.9(5) . . ?
C51 C50 C47 111.4(5) . . ?
C50 C51 C56 109.8(6) . . ?
C50 C51 C52 109.7(6) . . ?
C56 C51 C52 108.7(6) . . ?
C53 C52 C51 109.3(5) . . ?
C52 C53 C54 110.5(5) . . ?
C52 C53 C49 109.2(5) . . ?
C54 C53 C49 109.5(5) . . ?
C53 C54 C55 109.1(5) . . ?
C56 C55 C54 110.0(5) . . ?
C56 C55 C48 109.2(5) . . ?
C54 C55 C48 109.2(5) . . ?
C55 C56 C51 109.7(5) . . ?
C64 C63 C62 111.1(6) . . ?
C64 C63 C61 110.9(5) . . ?
C62 C63 C61 110.4(5) . . ?
N5 C64 C65 108.3(6) . . ?
N5 C64 C63 123.1(6) . . ?
C65 C64 C63 128.6(6) . . ?
C64 C65 C66 105.7(5) . . ?
N6 C66 C65 110.4(5) . . ?
N6 C66 C67 120.9(5) . . ?
C65 C66 C67 128.7(5) . . ?
C66 C67 C69 111.1(5) . . ?
C66 C67 C68 110.9(5) . . ?
C69 C67 C68 108.4(5) . . ?
C66 C67 C70 109.9(5) . . ?
C69 C67 C70 108.4(5) . . ?
C68 C67 C70 108.0(5) . . ?
C75 C68 C67 110.9(5) . . ?
C73 C69 C67 111.1(5) . . ?
C71 C70 C67 110.0(5) . . ?
C72 C71 C76 110.0(5) . . ?
C72 C71 C70 109.5(5) . . ?
C76 C71 C70 109.5(5) . . ?
C71 C72 C73 109.4(5) . . ?
C69 C73 C72 109.9(5) . . ?
C69 C73 C74 109.4(5) . . ?
C72 C73 C74 108.8(5) . . ?
C73 C74 C75 109.8(5) . . ?
C76 C75 C68 109.5(5) . . ?
C76 C75 C74 108.9(5) . . ?
C68 C75 C74 109.5(5) . . ?
C75 C76 C71 109.3(5) . . ?
C102 C101 Ca2 111.1(4) . . ?
C103 C102 C108 115.9(6) . . ?
C103 C102 C101 121.4(6) . . ?
C108 C102 C101 122.7(6) . . ?
C102 C103 C104 121.3(7) . . ?
C105 C104 C103 121.4(7) . . ?
C107 C105 C104 118.0(7) . . ?
C107 C105 C106 121.6(9) . . ?
C104 C105 C106 120.5(9) . . ?
C105 C107 C108 121.4(7) . . ?
C107 C108 C102 122.0(7) . . ?
O2 C109 C110 104.8(5) . . ?
C111 C110 C109 104.5(6) . . ?
C110 C111 C112 104.0(6) . . ?
O2 C112 C111 107.0(6) . . ?
C122 C123 C124 113.3(7) . . ?
C122 C123 C121 113.2(8) . . ?
C124 C123 C121 111.3(8) . . ?
N7 C124 C125 107.1(5) . . ?
N7 C124 C123 122.1(6) . . ?
C125 C124 C123 130.7(7) . . ?
C124 C125 C126 106.1(6) . . ?
N8 C126 C125 109.9(5) . . ?
N8 C126 C127 118.9(5) . . ?
C125 C126 C127 130.8(6) . . ?
C126 C127 C128 112.6(5) . . ?
C126 C127 C129 107.6(5) . . ?
C128 C127 C129 107.1(5) . . ?
C126 C127 C130 111.9(5) . . ?
C128 C127 C130 110.0(5) . . ?
C129 C127 C130 107.3(5) . . ?
C127 C128 C135 111.0(5) . . ?
C127 C129 C133 111.6(6) . . ?
C127 C130 C131 109.3(6) . . ?
C136 C131 C132 110.8(6) . . ?
C136 C131 C130 108.1(6) . . ?
C132 C131 C130 107.3(6) . . ?
C133 C132 C131 110.4(6) . . ?
C132 C133 C134 110.8(6) . . ?
C132 C133 C129 107.9(6) . . ?
C134 C133 C129 108.5(6) . . ?
C135 C134 C133 110.8(6) . . ?
C136 C135 C134 110.8(6) . . ?
C136 C135 C128 108.1(6) . . ?
C134 C135 C128 108.6(6) . . ?
C135 C136 C131 111.7(6) . . ?
C144 C143 C141 110.9(5) . . ?
C144 C143 C142 110.2(5) . . ?
C141 C143 C142 111.0(5) . . ?
N9 C144 C145 108.1(5) . . ?
N9 C144 C143 122.1(6) . . ?
C145 C144 C143 129.6(6) . . ?
C144 C145 C146 106.2(6) . . ?
N10 C146 C145 110.2(5) . . ?
N10 C146 C147 121.4(5) . . ?
C145 C146 C147 128.4(6) . . ?
C146 C147 C148 109.3(5) . . ?
C146 C147 C150 111.2(5) . . ?
C148 C147 C150 108.3(5) . . ?
C146 C147 C149 111.6(5) . . ?
C148 C147 C149 108.3(5) . . ?
C150 C147 C149 108.1(5) . . ?
C147 C148 C153 110.8(5) . . ?
C155 C149 C147 111.1(5) . . ?
C147 C150 C151 110.1(5) . . ?
C152 C151 C156 110.1(6) . . ?
C152 C151 C150 109.8(5) . . ?
C156 C151 C150 110.2(5) . . ?
C151 C152 C153 109.1(5) . . ?
C154 C153 C152 110.8(5) . . ?
C154 C153 C148 107.5(5) . . ?
C152 C153 C148 109.2(5) . . ?
C153 C154 C155 110.4(5) . . ?
C149 C155 C156 109.7(5) . . ?
C149 C155 C154 108.2(5) . . ?
C156 C155 C154 109.2(5) . . ?
C151 C156 C155 109.5(5) . . ?
C164 C163 C162 108.3(11) . . ?
C164 C163 C161 112.2(12) . . ?
C162 C163 C161 111.7(14) . . ?
C261 C263 C164 104.5(11) . . ?
C261 C263 C262 111.5(15) . . ?
C164 C263 C262 114.7(12) . . ?
N11 C164 C165 107.2(5) . . ?
N11 C164 C263 127.5(10) . . ?
C165 C164 C263 124.1(9) . . ?
N11 C164 C163 120.2(10) . . ?
C165 C164 C163 132.3(10) . . ?
C164 C165 C166 107.1(6) . . ?
N12 C166 C165 109.4(6) . . ?
N12 C166 C167 122.7(5) . . ?
C165 C166 C167 127.9(6) . . ?
C166 C167 C170 113.1(5) . . ?
C166 C167 C169 109.6(5) . . ?
C170 C167 C169 108.0(6) . . ?
C166 C167 C168 110.0(5) . . ?
C170 C167 C168 107.8(5) . . ?
C169 C167 C168 108.0(5) . . ?
C175 C168 C167 110.9(6) . . ?
C167 C169 C173 111.8(5) . . ?
C167 C170 C171 110.9(5) . . ?
C176 C171 C172 108.8(5) . . ?
C176 C171 C170 107.8(5) . . ?
C172 C171 C170 109.0(5) . . ?
C173 C172 C171 110.7(6) . . ?
C172 C173 C174 111.2(6) . . ?
C172 C173 C169 107.3(6) . . ?
C174 C173 C169 109.2(6) . . ?
C175 C174 C173 109.6(5) . . ?
C174 C175 C176 110.8(6) . . ?
C174 C175 C168 109.6(5) . . ?
C176 C175 C168 108.1(5) . . ?
C175 C176 C171 110.7(5) . . ?
N3 B1 N5 110.1(5) . . ?
N3 B1 N1 112.5(5) . . ?
N5 B1 N1 108.5(5) . . ?
N3 B1 Ca1 75.0(3) . . ?
N5 B1 Ca1 74.4(3) . . ?
N1 B1 Ca1 65.2(3) . . ?
N9 B2 N11 111.3(5) . . ?
N9 B2 N7 107.5(5) . . ?
N11 B2 N7 113.5(5) . . ?
N9 B2 Ca2 75.4(3) . . ?
N11 B2 Ca2 75.0(3) . . ?
N7 B2 Ca2 65.4(3) . . ?
C24 N1 N2 109.3(5) . . ?
C24 N1 B1 126.8(5) . . ?
N2 N1 B1 120.6(5) . . ?
C24 N1 Ca1 141.3(4) . . ?
N2 N1 Ca1 54.6(3) . . ?
B1 N1 Ca1 86.2(3) . . ?
C26 N2 N1 106.8(5) . . ?
C26 N2 Ca1 134.5(4) . . ?
N1 N2 Ca1 98.0(3) . . ?
C44 N3 N4 110.0(5) . . ?
C44 N3 B1 128.6(5) . . ?
N4 N3 B1 121.3(5) . . ?
C46 N4 N3 106.1(5) . . ?
C46 N4 Ca1 141.1(4) . . ?
N3 N4 Ca1 112.7(3) . . ?
C64 N5 N6 109.7(5) . . ?
C64 N5 B1 127.7(5) . . ?
N6 N5 B1 122.6(5) . . ?
C66 N6 N5 105.9(5) . . ?
C66 N6 Ca1 139.7(4) . . ?
N5 N6 Ca1 109.0(3) . . ?
N8 N7 C124 110.0(5) . . ?
N8 N7 B2 118.0(5) . . ?
C124 N7 B2 127.4(5) . . ?
N8 N7 Ca2 53.4(3) . . ?
C124 N7 Ca2 143.2(4) . . ?
B2 N7 Ca2 85.8(3) . . ?
C126 N8 N7 106.9(5) . . ?
C126 N8 Ca2 135.0(4) . . ?
N7 N8 Ca2 99.6(3) . . ?
C144 N9 N10 109.6(5) . . ?
C144 N9 B2 129.0(5) . . ?
N10 N9 B2 121.3(5) . . ?
C146 N10 N9 105.8(4) . . ?
C146 N10 Ca2 137.2(4) . . ?
N9 N10 Ca2 109.6(3) . . ?
C164 N11 N12 110.6(5) . . ?
C164 N11 B2 127.7(5) . . ?
N12 N11 B2 120.9(5) . . ?
C166 N12 N11 105.7(5) . . ?
C166 N12 Ca2 140.4(4) . . ?
N11 N12 Ca2 113.7(3) . . ?
C12 O1 C9 105.6(5) . . ?
C12 O1 Ca1 130.3(4) . . ?
C9 O1 Ca1 124.1(4) . . ?
C112 O2 C109 108.6(5) . . ?
C112 O2 Ca2 127.9(4) . . ?
C109 O2 Ca2 123.4(3) . . ?
O1 Ca1 N4 84.34(16) . . ?
O1 Ca1 N2 82.44(16) . . ?
N4 Ca1 N2 97.86(17) . . ?
O1 Ca1 N6 146.26(16) . . ?
N4 Ca1 N6 74.84(16) . . ?
N2 Ca1 N6 74.64(16) . . ?
O1 Ca1 C1 97.16(16) . . ?
N4 Ca1 C1 132.56(18) . . ?
N2 Ca1 C1 129.44(18) . . ?
N6 Ca1 C1 116.50(17) . . ?
O1 Ca1 N1 76.98(14) . . ?
N4 Ca1 N1 70.72(15) . . ?
N2 Ca1 N1 27.35(14) . . ?
N6 Ca1 N1 71.26(14) . . ?
C1 Ca1 N1 155.91(17) . . ?
O1 Ca1 B1 95.49(17) . . ?
N4 Ca1 B1 50.68(17) . . ?
N2 Ca1 B1 50.81(17) . . ?
N6 Ca1 B1 50.80(17) . . ?
C1 Ca1 B1 167.23(18) . . ?
N1 Ca1 B1 28.62(15) . . ?
N12 Ca2 O2 85.42(16) . . ?
N12 Ca2 N8 97.02(17) . . ?
O2 Ca2 N8 82.88(15) . . ?
N12 Ca2 N10 75.20(16) . . ?
O2 Ca2 N10 146.07(16) . . ?
N8 Ca2 N10 72.42(15) . . ?
N12 Ca2 C101 133.47(19) . . ?
O2 Ca2 C101 95.34(16) . . ?
N8 Ca2 C101 129.33(18) . . ?
N10 Ca2 C101 118.24(18) . . ?
N12 Ca2 N7 70.37(15) . . ?
O2 Ca2 N7 76.98(14) . . ?
N8 Ca2 N7 27.00(14) . . ?
N10 Ca2 N7 70.42(15) . . ?
C101 Ca2 N7 154.95(17) . . ?
N12 Ca2 B2 50.22(17) . . ?
O2 Ca2 B2 96.05(17) . . ?
N8 Ca2 B2 50.16(17) . . ?
N10 Ca2 B2 50.21(17) . . ?
C101 Ca2 B2 168.35(19) . . ?
N7 Ca2 B2 28.81(15) . . ?

_refine_diff_density_max         0.878
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.065

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_G094
_database_code_depnum_ccdc_archive 'CCDC 1967137'
loop_
_audit_author_name
_audit_author_address
'Jianhua Cheng'
;CIAC, CAS
China
;
_audit_update_record             
;
2019-11-21 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[(TpAd,iPr)Ca(PhCH2CHPh)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H83 B Ca N6'
_chemical_formula_sum            'C62 H83 B Ca N6'
_chemical_formula_weight         963.23

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

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

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

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

_cell_length_a                   11.9771(8)
_cell_length_b                   14.8686(10)
_cell_length_c                   16.6034(11)
_cell_angle_alpha                99.7570(10)
_cell_angle_beta                 99.7770(10)
_cell_angle_gamma                104.4060(10)
_cell_volume                     2751.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2660
_cell_measurement_theta_min      1.450
_cell_measurement_theta_max      26.393

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_F_000             1044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14196
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.800
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             9486
_reflns_number_gt                6719
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+0.2485P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9486
_refine_ls_number_parameters     639
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0295(2) 0.4776(2) 0.74930(18) 0.0415(7) Uani 1 1 d . . . . .
H1A H -0.042424 0.431676 0.755548 0.050 Uiso 1 1 calc R U . . .
H1B H 0.023948 0.473296 0.688528 0.050 Uiso 1 1 calc R U . . .
C2 C 0.1351(2) 0.44616(19) 0.78338(17) 0.0332(6) Uani 1 1 d . . . . .
C3 C 0.1547(2) 0.42913(17) 0.86658(16) 0.0290(6) Uani 1 1 d . . . . .
C4 C 0.2621(2) 0.41242(18) 0.90306(16) 0.0317(6) Uani 1 1 d . . . . .
H4 H 0.326228 0.423712 0.875812 0.038 Uiso 1 1 calc R U . . .
C5 C 0.2767(3) 0.38052(19) 0.97633(17) 0.0404(7) Uani 1 1 d . . . . .
H5 H 0.348982 0.368300 0.997450 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1870(3) 0.3662(2) 1.01921(18) 0.0467(8) Uani 1 1 d . . . . .
H6 H 0.195553 0.342037 1.068614 0.056 Uiso 1 1 calc R U . . .
C7 C 0.0840(3) 0.3879(2) 0.98869(19) 0.0440(8) Uani 1 1 d . . . . .
H7 H 0.023582 0.381975 1.019512 0.053 Uiso 1 1 calc R U . . .
C8 C 0.0676(2) 0.41765(19) 0.91505(18) 0.0380(7) Uani 1 1 d . . . . .
H8 H -0.004608 0.431048 0.895806 0.046 Uiso 1 1 calc R U . . .
C9 C 0.0279(2) 0.57789(19) 0.78910(16) 0.0322(6) Uani 1 1 d . . . . .
C10 C -0.0748(2) 0.6050(2) 0.76977(18) 0.0397(7) Uani 1 1 d . . . . .
H10 H -0.143524 0.560433 0.733661 0.048 Uiso 1 1 calc R U . . .
C11 C -0.0782(3) 0.6962(2) 0.80250(19) 0.0431(7) Uani 1 1 d . . . . .
H11 H -0.148863 0.713587 0.788143 0.052 Uiso 1 1 calc R U . . .
C12 C 0.0197(3) 0.7616(2) 0.85554(19) 0.0441(7) Uani 1 1 d . . . . .
H12 H 0.016932 0.823971 0.878051 0.053 Uiso 1 1 calc R U . . .
C13 C 0.1219(2) 0.7358(2) 0.87565(18) 0.0391(7) Uani 1 1 d . . . . .
H13 H 0.189973 0.780178 0.912589 0.047 Uiso 1 1 calc R U . . .
C14 C 0.1252(2) 0.6445(2) 0.84184(17) 0.0375(7) Uani 1 1 d . . . . .
H14 H 0.196559 0.627789 0.855518 0.045 Uiso 1 1 calc R U . . .
C21 C 0.5443(3) 0.2682(2) 0.9606(2) 0.0570(9) Uani 1 1 d . . . . .
H21A H 0.589097 0.237165 0.996284 0.086 Uiso 1 1 calc R U . . .
H21B H 0.537753 0.326598 0.994547 0.086 Uiso 1 1 calc R U . . .
H21C H 0.465068 0.224999 0.935176 0.086 Uiso 1 1 calc R U . . .
C22 C 0.7346(2) 0.3550(2) 0.92938(19) 0.0471(8) Uani 1 1 d . . . . .
H22A H 0.775583 0.322725 0.966171 0.071 Uiso 1 1 calc R U . . .
H22B H 0.775989 0.366108 0.884315 0.071 Uiso 1 1 calc R U . . .
H22C H 0.733383 0.416160 0.961903 0.071 Uiso 1 1 calc R U . . .
C23 C 0.6082(2) 0.29302(19) 0.89167(17) 0.0347(7) Uani 1 1 d . . . . .
H23 H 0.611770 0.232268 0.857048 0.042 Uiso 1 1 calc R U . . .
C24 C 0.5430(2) 0.34110(17) 0.83474(15) 0.0266(6) Uani 1 1 d . . . . .
C25 C 0.5724(2) 0.43427(17) 0.82842(16) 0.0307(6) Uani 1 1 d . . . . .
H25 H 0.639214 0.484095 0.860812 0.037 Uiso 1 1 calc R U . . .
C26 C 0.4845(2) 0.44147(17) 0.76481(15) 0.0257(6) Uani 1 1 d . . . . .
C27 C 0.4782(2) 0.52661(17) 0.72798(16) 0.0285(6) Uani 1 1 d . . . . .
C28 C 0.5968(2) 0.56507(19) 0.70338(19) 0.0405(7) Uani 1 1 d . . . . .
H28A H 0.662373 0.582529 0.753515 0.049 Uiso 1 1 calc R U . . .
H28B H 0.609884 0.514773 0.661799 0.049 Uiso 1 1 calc R U . . .
C29 C 0.4624(2) 0.60704(18) 0.79216(17) 0.0343(6) Uani 1 1 d . . . . .
H29A H 0.387632 0.584320 0.810183 0.041 Uiso 1 1 calc R U . . .
H29B H 0.528322 0.625550 0.842144 0.041 Uiso 1 1 calc R U . . .
C30 C 0.3794(2) 0.50040(18) 0.64910(16) 0.0357(7) Uani 1 1 d . . . . .
H30A H 0.302199 0.475548 0.663312 0.043 Uiso 1 1 calc R U . . .
H30B H 0.391159 0.449690 0.607246 0.043 Uiso 1 1 calc R U . . .
C31 C 0.3785(3) 0.5880(2) 0.61142(18) 0.0436(7) Uani 1 1 d . . . . .
H31 H 0.313124 0.570057 0.560215 0.052 Uiso 1 1 calc R U . . .
C32 C 0.3594(3) 0.6650(2) 0.67652(19) 0.0463(8) Uani 1 1 d . . . . .
H32A H 0.282913 0.640832 0.691862 0.056 Uiso 1 1 calc R U . . .
H32B H 0.356984 0.721382 0.652793 0.056 Uiso 1 1 calc R U . . .
C33 C 0.4598(2) 0.69317(19) 0.75443(19) 0.0430(7) Uani 1 1 d . . . . .
H33 H 0.447710 0.744386 0.796628 0.052 Uiso 1 1 calc R U . . .
C34 C 0.5772(3) 0.7297(2) 0.7299(2) 0.0530(9) Uani 1 1 d . . . . .
H34A H 0.576702 0.786100 0.705763 0.064 Uiso 1 1 calc R U . . .
H34B H 0.642572 0.749165 0.780342 0.064 Uiso 1 1 calc R U . . .
C35 C 0.5966(3) 0.6522(2) 0.6662(2) 0.0515(8) Uani 1 1 d . . . . .
H35 H 0.674023 0.676366 0.650886 0.062 Uiso 1 1 calc R U . . .
C36 C 0.4970(3) 0.6246(2) 0.5883(2) 0.0558(9) Uani 1 1 d . . . . .
H36A H 0.509277 0.574472 0.546139 0.067 Uiso 1 1 calc R U . . .
H36B H 0.497062 0.680661 0.563474 0.067 Uiso 1 1 calc R U . . .
C41 C 0.5913(2) 0.2387(2) 0.60801(19) 0.0453(8) Uani 1 1 d . . . . .
H41A H 0.666993 0.225757 0.605146 0.068 Uiso 1 1 calc R U . . .
H41B H 0.581951 0.287844 0.576960 0.068 Uiso 1 1 calc R U . . .
H41C H 0.589563 0.260997 0.666695 0.068 Uiso 1 1 calc R U . . .
C42 C 0.4950(2) 0.1082(2) 0.47910(17) 0.0416(7) Uani 1 1 d . . . . .
H42A H 0.572485 0.097871 0.478149 0.062 Uiso 1 1 calc R U . . .
H42B H 0.433009 0.047729 0.456427 0.062 Uiso 1 1 calc R U . . .
H42C H 0.482637 0.154009 0.444889 0.062 Uiso 1 1 calc R U . . .
C43 C 0.4902(2) 0.14738(19) 0.56928(16) 0.0323(6) Uani 1 1 d . . . . .
H43 H 0.500326 0.098772 0.602617 0.039 Uiso 1 1 calc R U . . .
C44 C 0.3723(2) 0.16381(17) 0.57227(16) 0.0276(6) Uani 1 1 d . . . . .
C45 C 0.2896(2) 0.1758(2) 0.50990(16) 0.0343(6) Uani 1 1 d . . . . .
H45 H 0.293018 0.171725 0.452704 0.041 Uiso 1 1 calc R U . . .
C46 C 0.1998(2) 0.19493(18) 0.54696(15) 0.0270(6) Uani 1 1 d . . . . .
C47 C 0.0875(2) 0.21537(19) 0.50839(15) 0.0294(6) Uani 1 1 d . . . . .
C48 C 0.1142(2) 0.2884(2) 0.45391(19) 0.0475(8) Uani 1 1 d . . . . .
H48A H 0.151277 0.263763 0.409344 0.057 Uiso 1 1 calc R U . . .
H48B H 0.170491 0.348481 0.488818 0.057 Uiso 1 1 calc R U . . .
C49 C -0.0002(2) 0.1239(2) 0.45330(18) 0.0455(8) Uani 1 1 d . . . . .
H49A H -0.019174 0.076420 0.487770 0.055 Uiso 1 1 calc R U . . .
H49B H 0.036146 0.097215 0.409140 0.055 Uiso 1 1 calc R U . . .
C50 C 0.0295(2) 0.2566(2) 0.57544(17) 0.0402(7) Uani 1 1 d . . . . .
H50A H 0.084888 0.316902 0.610654 0.048 Uiso 1 1 calc R U . . .
H50B H 0.011499 0.211362 0.612064 0.048 Uiso 1 1 calc R U . . .
C51 C -0.0854(2) 0.2755(2) 0.53459(18) 0.0460(8) Uani 1 1 d . . . . .
H51 H -0.122602 0.301608 0.579272 0.055 Uiso 1 1 calc R U . . .
C52 C -0.1695(2) 0.1833(2) 0.4814(2) 0.0529(9) Uani 1 1 d . . . . .
H52A H -0.244251 0.194576 0.455803 0.063 Uiso 1 1 calc R U . . .
H52B H -0.187965 0.136789 0.516863 0.063 Uiso 1 1 calc R U . . .
C53 C -0.1138(2) 0.1431(2) 0.41258(19) 0.0498(8) Uani 1 1 d . . . . .
H53 H -0.170131 0.082468 0.376916 0.060 Uiso 1 1 calc R U . . .
C54 C -0.0847(3) 0.2149(2) 0.35917(18) 0.0522(9) Uani 1 1 d . . . . .
H54A H -0.158160 0.226507 0.331593 0.063 Uiso 1 1 calc R U . . .
H54B H -0.047399 0.189582 0.314978 0.063 Uiso 1 1 calc R U . . .
C55 C -0.0004(3) 0.3081(2) 0.4140(2) 0.0511(8) Uani 1 1 d . . . . .
H55 H 0.018225 0.355505 0.378522 0.061 Uiso 1 1 calc R U . . .
C56 C -0.0560(3) 0.3470(2) 0.4815(2) 0.0552(9) Uani 1 1 d . . . . .
H56A H -0.128898 0.360777 0.455700 0.066 Uiso 1 1 calc R U . . .
H56B H -0.000681 0.407137 0.516919 0.066 Uiso 1 1 calc R U . . .
C61 C 0.4160(2) -0.0521(2) 0.73100(18) 0.0428(7) Uani 1 1 d . . . . .
H61A H 0.484450 -0.077342 0.736962 0.064 Uiso 1 1 calc R U . . .
H61B H 0.343193 -0.105079 0.711934 0.064 Uiso 1 1 calc R U . . .
H61C H 0.420776 -0.011973 0.689886 0.064 Uiso 1 1 calc R U . . .
C62 C 0.4166(3) -0.0533(2) 0.8806(2) 0.0575(9) Uani 1 1 d . . . . .
H62A H 0.483979 -0.079637 0.882293 0.086 Uiso 1 1 calc R U . . .
H62B H 0.423521 -0.013233 0.935648 0.086 Uiso 1 1 calc R U . . .
H62C H 0.342974 -0.105371 0.866405 0.086 Uiso 1 1 calc R U . . .
C63 C 0.4153(2) 0.00652(18) 0.81474(17) 0.0319(6) Uani 1 1 d . . . . .
H63 H 0.489583 0.060638 0.832094 0.038 Uiso 1 1 calc R U . . .
C64 C 0.3123(2) 0.04801(17) 0.81090(15) 0.0275(6) Uani 1 1 d . . . . .
C65 C 0.2072(2) 0.01744(18) 0.83407(17) 0.0325(6) Uani 1 1 d . . . . .
H65 H 0.182148 -0.037411 0.855924 0.039 Uiso 1 1 calc R U . . .
C66 C 0.1442(2) 0.08264(17) 0.81929(15) 0.0262(6) Uani 1 1 d . . . . .
C67 C 0.0190(2) 0.07887(17) 0.82594(15) 0.0263(6) Uani 1 1 d . . . . .
C68 C -0.0007(2) 0.0671(2) 0.91313(16) 0.0339(6) Uani 1 1 d . . . . .
H68A H 0.019329 0.009348 0.925258 0.041 Uiso 1 1 calc R U . . .
H68B H 0.051878 0.122752 0.956238 0.041 Uiso 1 1 calc R U . . .
C69 C -0.0659(2) -0.00799(19) 0.75975(18) 0.0381(7) Uani 1 1 d . . . . .
H69A H -0.054699 -0.001451 0.703094 0.046 Uiso 1 1 calc R U . . .
H69B H -0.047629 -0.066953 0.770101 0.046 Uiso 1 1 calc R U . . .
C70 C -0.0133(2) 0.16775(18) 0.80809(17) 0.0310(6) Uani 1 1 d . . . . .
H70A H -0.002231 0.175342 0.751613 0.037 Uiso 1 1 calc R U . . .
H70B H 0.039978 0.224605 0.849518 0.037 Uiso 1 1 calc R U . . .
C71 C -0.1421(2) 0.1606(2) 0.81269(18) 0.0374(7) Uani 1 1 d . . . . .
H71 H -0.161255 0.219702 0.801573 0.045 Uiso 1 1 calc R U . . .
C72 C -0.1586(2) 0.1487(2) 0.89988(18) 0.0385(7) Uani 1 1 d . . . . .
H72A H -0.105794 0.204604 0.942628 0.046 Uiso 1 1 calc R U . . .
H72B H -0.241257 0.144825 0.903584 0.046 Uiso 1 1 calc R U . . .
C73 C -0.1301(2) 0.0586(2) 0.91666(18) 0.0369(7) Uani 1 1 d . . . . .
H73 H -0.141723 0.050846 0.973603 0.044 Uiso 1 1 calc R U . . .
C74 C -0.2108(2) -0.0276(2) 0.8512(2) 0.0465(8) Uani 1 1 d . . . . .
H74A H -0.294154 -0.034180 0.854419 0.056 Uiso 1 1 calc R U . . .
H74B H -0.191478 -0.086007 0.862015 0.056 Uiso 1 1 calc R U . . .
C75 C -0.1945(2) -0.0151(2) 0.76396(19) 0.0450(8) Uani 1 1 d . . . . .
H75 H -0.248236 -0.071395 0.720852 0.054 Uiso 1 1 calc R U . . .
C76 C -0.2234(2) 0.0744(2) 0.74726(18) 0.0456(8) Uani 1 1 d . . . . .
H76A H -0.306807 0.069461 0.749406 0.055 Uiso 1 1 calc R U . . .
H76B H -0.213254 0.082008 0.690615 0.055 Uiso 1 1 calc R U . . .
B1 B 0.3959(2) 0.1845(2) 0.73551(18) 0.0243(6) Uani 1 1 d . . . . .
N1 N 0.44055(16) 0.29378(13) 0.77736(12) 0.0220(4) Uani 1 1 d . . . . .
N2 N 0.40360(16) 0.35707(14) 0.73398(12) 0.0246(5) Uani 1 1 d . . . . .
N3 N 0.33094(16) 0.17353(13) 0.64401(12) 0.0233(5) Uani 1 1 d . . . . .
N4 N 0.22432(16) 0.19369(14) 0.62786(12) 0.0243(5) Uani 1 1 d . . . . .
N5 N 0.31224(16) 0.12895(13) 0.78319(12) 0.0228(5) Uani 1 1 d . . . . .
N6 N 0.20820(16) 0.15099(14) 0.78954(12) 0.0250(5) Uani 1 1 d . . . . .
Ca1 Ca 0.19903(4) 0.29615(3) 0.74739(3) 0.02364(14) Uani 1 1 d . . . . .
H1B1 H 0.4731(18) 0.1572(15) 0.7363(13) 0.017(6) Uiso 1 1 d . . . . .
H2 H 0.212(2) 0.4795(19) 0.7688(16) 0.045(8) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.510(3) . ?
C1 C9 1.532(4) . ?
C2 C3 1.437(4) . ?
C2 Ca1 2.544(3) . ?
C3 C8 1.417(3) . ?
C3 C4 1.424(3) . ?
C3 Ca1 2.768(3) . ?
C4 C5 1.378(4) . ?
C4 Ca1 2.723(3) . ?
C5 C6 1.380(4) . ?
C6 C7 1.386(4) . ?
C7 C8 1.369(4) . ?
C9 C14 1.375(4) . ?
C9 C10 1.391(3) . ?
C10 C11 1.385(4) . ?
C11 C12 1.374(4) . ?
C12 C13 1.377(4) . ?
C13 C14 1.391(4) . ?
C21 C23 1.527(4) . ?
C22 C23 1.524(4) . ?
C23 C24 1.507(3) . ?
C24 N1 1.362(3) . ?
C24 C25 1.369(3) . ?
C25 C26 1.397(3) . ?
C26 N2 1.336(3) . ?
C26 C27 1.509(3) . ?
C27 C30 1.530(3) . ?
C27 C29 1.533(4) . ?
C27 C28 1.544(3) . ?
C28 C35 1.527(4) . ?
C29 C33 1.523(4) . ?
C30 C31 1.540(3) . ?
C31 C32 1.524(4) . ?
C31 C36 1.526(4) . ?
C32 C33 1.527(4) . ?
C33 C34 1.525(4) . ?
C34 C35 1.518(4) . ?
C35 C36 1.522(4) . ?
C41 C43 1.531(4) . ?
C42 C43 1.528(4) . ?
C43 C44 1.499(3) . ?
C44 N3 1.365(3) . ?
C44 C45 1.373(3) . ?
C45 C46 1.390(3) . ?
C46 N4 1.330(3) . ?
C46 C47 1.512(3) . ?
C47 C49 1.526(4) . ?
C47 C50 1.531(4) . ?
C47 C48 1.536(4) . ?
C48 C55 1.537(4) . ?
C49 C53 1.528(4) . ?
C50 C51 1.540(3) . ?
C50 Ca1 3.080(3) . ?
C51 C56 1.506(4) . ?
C51 C52 1.508(4) . ?
C52 C53 1.528(4) . ?
C53 C54 1.512(4) . ?
C54 C55 1.527(4) . ?
C55 C56 1.503(4) . ?
C61 C63 1.513(4) . ?
C62 C63 1.522(4) . ?
C63 C64 1.507(3) . ?
C64 N5 1.359(3) . ?
C64 C65 1.370(3) . ?
C65 C66 1.397(3) . ?
C66 N6 1.332(3) . ?
C66 C67 1.510(3) . ?
C67 C70 1.527(3) . ?
C67 C68 1.537(3) . ?
C67 C69 1.548(3) . ?
C68 C73 1.535(3) . ?
C69 C75 1.531(4) . ?
C70 C71 1.536(3) . ?
C70 Ca1 3.199(2) . ?
C71 C76 1.523(4) . ?
C71 C72 1.527(4) . ?
C72 C73 1.521(4) . ?
C73 C74 1.520(4) . ?
C74 C75 1.530(4) . ?
C75 C76 1.513(4) . ?
B1 N3 1.547(3) . ?
B1 N5 1.547(3) . ?
B1 N1 1.571(3) . ?
B1 Ca1 3.217(3) . ?
N1 N2 1.389(2) . ?
N1 Ca1 2.8608(19) . ?
N2 Ca1 2.4540(19) . ?
N3 N4 1.376(2) . ?
N4 Ca1 2.400(2) . ?
N5 N6 1.381(3) . ?
N6 Ca1 2.4009(19) . ?

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
C2 C1 C9 117.0(2) . . ?
C3 C2 C1 121.0(2) . . ?
C3 C2 Ca1 83.12(15) . . ?
C1 C2 Ca1 134.35(18) . . ?
C8 C3 C4 114.6(2) . . ?
C8 C3 C2 124.1(2) . . ?
C4 C3 C2 121.0(2) . . ?
C8 C3 Ca1 129.80(17) . . ?
C4 C3 Ca1 73.22(14) . . ?
C2 C3 Ca1 65.85(14) . . ?
C5 C4 C3 122.6(2) . . ?
C5 C4 Ca1 123.82(18) . . ?
C3 C4 Ca1 76.73(14) . . ?
C4 C5 C6 120.4(3) . . ?
C5 C6 C7 118.6(3) . . ?
C8 C7 C6 121.4(3) . . ?
C7 C8 C3 122.2(3) . . ?
C14 C9 C10 117.7(3) . . ?
C14 C9 C1 123.0(2) . . ?
C10 C9 C1 119.3(2) . . ?
C11 C10 C9 120.9(3) . . ?
C12 C11 C10 120.7(3) . . ?
C11 C12 C13 119.2(3) . . ?
C12 C13 C14 119.9(3) . . ?
C9 C14 C13 121.7(3) . . ?
C24 C23 C22 110.6(2) . . ?
C24 C23 C21 111.7(2) . . ?
C22 C23 C21 110.6(2) . . ?
N1 C24 C25 108.0(2) . . ?
N1 C24 C23 123.0(2) . . ?
C25 C24 C23 129.0(2) . . ?
C24 C25 C26 106.3(2) . . ?
N2 C26 C25 110.1(2) . . ?
N2 C26 C27 121.4(2) . . ?
C25 C26 C27 128.4(2) . . ?
C26 C27 C30 111.9(2) . . ?
C26 C27 C29 111.5(2) . . ?
C30 C27 C29 109.8(2) . . ?
C26 C27 C28 108.0(2) . . ?
C30 C27 C28 108.0(2) . . ?
C29 C27 C28 107.4(2) . . ?
C35 C28 C27 110.6(2) . . ?
C33 C29 C27 110.6(2) . . ?
C27 C30 C31 110.5(2) . . ?
C32 C31 C36 109.9(2) . . ?
C32 C31 C30 108.7(2) . . ?
C36 C31 C30 109.1(2) . . ?
C31 C32 C33 109.8(2) . . ?
C29 C33 C34 109.0(2) . . ?
C29 C33 C32 109.9(2) . . ?
C34 C33 C32 109.2(3) . . ?
C35 C34 C33 109.9(2) . . ?
C34 C35 C36 109.1(3) . . ?
C34 C35 C28 109.7(3) . . ?
C36 C35 C28 109.3(2) . . ?
C35 C36 C31 109.8(2) . . ?
C44 C43 C42 110.4(2) . . ?
C44 C43 C41 111.4(2) . . ?
C42 C43 C41 110.5(2) . . ?
N3 C44 C45 107.3(2) . . ?
N3 C44 C43 123.0(2) . . ?
C45 C44 C43 129.7(2) . . ?
C44 C45 C46 106.5(2) . . ?
N4 C46 C45 110.0(2) . . ?
N4 C46 C47 120.5(2) . . ?
C45 C46 C47 129.5(2) . . ?
C46 C47 C49 109.9(2) . . ?
C46 C47 C50 111.6(2) . . ?
C49 C47 C50 108.8(2) . . ?
C46 C47 C48 110.5(2) . . ?
C49 C47 C48 108.5(2) . . ?
C50 C47 C48 107.4(2) . . ?
C47 C48 C55 110.3(2) . . ?
C47 C49 C53 110.9(2) . . ?
C47 C50 C51 110.6(2) . . ?
C47 C50 Ca1 108.09(15) . . ?
C51 C50 Ca1 140.75(18) . . ?
C56 C51 C52 110.4(3) . . ?
C56 C51 C50 108.8(2) . . ?
C52 C51 C50 109.2(3) . . ?
C51 C52 C53 109.9(2) . . ?
C54 C53 C52 109.4(3) . . ?
C54 C53 C49 109.4(2) . . ?
C52 C53 C49 108.9(2) . . ?
C53 C54 C55 109.7(2) . . ?
C56 C55 C54 110.2(3) . . ?
C56 C55 C48 109.8(2) . . ?
C54 C55 C48 108.6(3) . . ?
C55 C56 C51 109.8(3) . . ?
C64 C63 C61 112.8(2) . . ?
C64 C63 C62 110.6(2) . . ?
C61 C63 C62 110.0(2) . . ?
N5 C64 C65 107.5(2) . . ?
N5 C64 C63 122.7(2) . . ?
C65 C64 C63 129.8(2) . . ?
C64 C65 C66 106.6(2) . . ?
N6 C66 C65 109.7(2) . . ?
N6 C66 C67 120.9(2) . . ?
C65 C66 C67 129.2(2) . . ?
C66 C67 C70 112.04(19) . . ?
C66 C67 C68 111.3(2) . . ?
C70 C67 C68 108.8(2) . . ?
C66 C67 C69 108.3(2) . . ?
C70 C67 C69 107.7(2) . . ?
C68 C67 C69 108.5(2) . . ?
C73 C68 C67 110.2(2) . . ?
C75 C69 C67 110.4(2) . . ?
C67 C70 C71 110.9(2) . . ?
C67 C70 Ca1 108.73(14) . . ?
C71 C70 Ca1 139.63(16) . . ?
C76 C71 C72 109.5(2) . . ?
C76 C71 C70 109.1(2) . . ?
C72 C71 C70 109.2(2) . . ?
C73 C72 C71 109.7(2) . . ?
C74 C73 C72 110.0(2) . . ?
C74 C73 C68 109.7(2) . . ?
C72 C73 C68 109.0(2) . . ?
C73 C74 C75 109.4(2) . . ?
C76 C75 C74 110.0(2) . . ?
C76 C75 C69 109.8(2) . . ?
C74 C75 C69 108.8(2) . . ?
C75 C76 C71 109.8(2) . . ?
N3 B1 N5 110.38(19) . . ?
N3 B1 N1 107.55(19) . . ?
N5 B1 N1 111.4(2) . . ?
N3 B1 Ca1 74.35(12) . . ?
N5 B1 Ca1 75.65(12) . . ?
N1 B1 Ca1 62.70(11) . . ?
C24 N1 N2 109.18(18) . . ?
C24 N1 B1 127.24(19) . . ?
N2 N1 B1 118.80(18) . . ?
C24 N1 Ca1 137.62(15) . . ?
N2 N1 Ca1 59.02(10) . . ?
B1 N1 Ca1 88.09(12) . . ?
C26 N2 N1 106.40(18) . . ?
C26 N2 Ca1 132.27(16) . . ?
N1 N2 Ca1 91.96(12) . . ?
C44 N3 N4 109.30(18) . . ?
C44 N3 B1 129.41(19) . . ?
N4 N3 B1 119.99(19) . . ?
C46 N4 N3 106.93(18) . . ?
C46 N4 Ca1 130.34(16) . . ?
N3 N4 Ca1 111.36(13) . . ?
C64 N5 N6 109.50(18) . . ?
C64 N5 B1 130.3(2) . . ?
N6 N5 B1 119.25(18) . . ?
C66 N6 N5 106.74(18) . . ?
C66 N6 Ca1 140.12(16) . . ?
N5 N6 Ca1 113.13(13) . . ?
N4 Ca1 N6 73.96(7) . . ?
N4 Ca1 N2 72.73(7) . . ?
N6 Ca1 N2 100.04(6) . . ?
N4 Ca1 C2 139.73(8) . . ?
N6 Ca1 C2 143.63(8) . . ?
N2 Ca1 C2 103.53(8) . . ?
N4 Ca1 C4 156.85(7) . . ?
N6 Ca1 C4 97.72(7) . . ?
N2 Ca1 C4 87.95(7) . . ?
C2 Ca1 C4 56.33(8) . . ?
N4 Ca1 C3 170.70(7) . . ?
N6 Ca1 C3 114.58(7) . . ?
N2 Ca1 C3 108.09(7) . . ?
C2 Ca1 C3 31.03(8) . . ?
C4 Ca1 C3 30.06(7) . . ?
N4 Ca1 N1 72.13(6) . . ?
N6 Ca1 N1 71.94(6) . . ?
N2 Ca1 N1 29.02(6) . . ?
C2 Ca1 N1 123.54(7) . . ?
C4 Ca1 N1 84.78(7) . . ?
C3 Ca1 N1 113.29(7) . . ?
N4 Ca1 C50 59.54(7) . . ?
N6 Ca1 C50 111.47(8) . . ?
N2 Ca1 C50 109.55(7) . . ?
C2 Ca1 C50 86.15(8) . . ?
C4 Ca1 C50 141.83(8) . . ?
C3 Ca1 C50 112.28(7) . . ?
N1 Ca1 C50 126.67(6) . . ?
N4 Ca1 C70 104.89(7) . . ?
N6 Ca1 C70 57.63(6) . . ?
N2 Ca1 C70 156.31(6) . . ?
C2 Ca1 C70 93.24(8) . . ?
C4 Ca1 C70 87.60(7) . . ?
C3 Ca1 C70 78.16(7) . . ?
N1 Ca1 C70 127.32(6) . . ?
C50 Ca1 C70 87.88(7) . . ?
N4 Ca1 B1 51.10(7) . . ?
N6 Ca1 B1 50.97(7) . . ?
N2 Ca1 B1 51.29(7) . . ?
C2 Ca1 B1 152.71(8) . . ?
C4 Ca1 B1 106.76(8) . . ?
C3 Ca1 B1 136.80(7) . . ?
N1 Ca1 B1 29.21(6) . . ?
C50 Ca1 B1 110.63(7) . . ?
C70 Ca1 B1 108.26(7) . . ?

_refine_diff_density_max         0.251
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.048

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_D004
_database_code_depnum_ccdc_archive 'CCDC 1967136'
loop_
_audit_author_name
_audit_author_address
'Jianhua Cheng'
;CIAC, CAS
China
;
_audit_update_record             
;
2019-11-21 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[(TpAd,iPr)Ca(Ph2CCH3)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H83 B Ca N6'
_chemical_formula_sum            'C62 H83 B Ca N6'
_chemical_formula_weight         963.23

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

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

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

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

_cell_length_a                   11.7488(13)
_cell_length_b                   15.0579(15)
_cell_length_c                   15.7679(17)
_cell_angle_alpha                96.695(2)
_cell_angle_beta                 94.947(2)
_cell_angle_gamma                101.734(3)
_cell_volume                     2695.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    1334
_cell_measurement_theta_min      1.309
_cell_measurement_theta_max      26.390

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_F_000             1044
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.162
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13974
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.776
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             9305
_reflns_number_gt                5336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2018/2)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0490P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9305
_refine_ls_number_parameters     636
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0675
_refine_ls_wR_factor_ref         0.1489
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7465(3) 0.4205(3) 0.4326(2) 0.0408(10) Uani 1 1 d . . . . .
H1A H 0.789285 0.406683 0.383752 0.061 Uiso 1 1 calc R U . . .
H1B H 0.776584 0.395408 0.482384 0.061 Uiso 1 1 calc R U . . .
H1C H 0.757110 0.487035 0.446641 0.061 Uiso 1 1 calc R U . . .
C2 C 0.6163(3) 0.3775(2) 0.4091(2) 0.0306(9) Uani 1 1 d . . . . .
C3 C 0.5549(3) 0.4078(2) 0.3407(2) 0.0298(9) Uani 1 1 d . . . . .
C4 C 0.6153(4) 0.4614(2) 0.2818(2) 0.0374(10) Uani 1 1 d . . . . .
H4 H 0.698328 0.478726 0.290181 0.045 Uiso 1 1 calc R U . . .
C5 C 0.5553(4) 0.4885(3) 0.2129(3) 0.0475(12) Uani 1 1 d . . . . .
H5 H 0.598501 0.525441 0.176670 0.057 Uiso 1 1 calc R U . . .
C6 C 0.4366(4) 0.4640(3) 0.1954(3) 0.0531(12) Uani 1 1 d . . . . .
H6 H 0.396956 0.484309 0.148796 0.064 Uiso 1 1 calc R U . . .
C7 C 0.3753(4) 0.4082(3) 0.2484(3) 0.0467(11) Uani 1 1 d . . . . .
H7 H 0.292720 0.388749 0.236581 0.056 Uiso 1 1 calc R U . . .
C8 C 0.4322(4) 0.3806(2) 0.3174(2) 0.0378(10) Uani 1 1 d . . . . .
H8 H 0.387204 0.341445 0.351040 0.045 Uiso 1 1 calc R U . . .
C9 C 0.5582(3) 0.3412(2) 0.4822(2) 0.0294(9) Uani 1 1 d . . . . .
C10 C 0.6019(3) 0.2773(3) 0.5260(2) 0.0395(10) Uani 1 1 d . . . . .
H10 H 0.665864 0.254275 0.506255 0.047 Uiso 1 1 calc R U . . .
C11 C 0.5541(4) 0.2468(3) 0.5974(3) 0.0482(11) Uani 1 1 d . . . . .
H11 H 0.585633 0.203543 0.626013 0.058 Uiso 1 1 calc R U . . .
C12 C 0.4610(4) 0.2789(3) 0.6270(2) 0.0493(12) Uani 1 1 d . . . . .
H12 H 0.428005 0.257926 0.675880 0.059 Uiso 1 1 calc R U . . .
C13 C 0.4164(4) 0.3415(3) 0.5851(3) 0.0456(11) Uani 1 1 d . . . . .
H13 H 0.351769 0.363417 0.604918 0.055 Uiso 1 1 calc R U . . .
C14 C 0.4646(3) 0.3729(2) 0.5142(2) 0.0360(10) Uani 1 1 d . . . . .
H14 H 0.433226 0.416993 0.486818 0.043 Uiso 1 1 calc R U . . .
C20 C 0.9146(4) 0.2230(3) 0.4820(2) 0.0452(11) Uani 1 1 d . . . . .
H20A H 0.938319 0.184294 0.523123 0.068 Uiso 1 1 calc R U . . .
H20B H 0.899252 0.278720 0.513282 0.068 Uiso 1 1 calc R U . . .
H20C H 0.843528 0.189426 0.445646 0.068 Uiso 1 1 calc R U . . .
C21 C 1.1276(3) 0.2936(3) 0.4806(2) 0.0405(10) Uani 1 1 d . . . . .
H21A H 1.145691 0.253340 0.522026 0.061 Uiso 1 1 calc R U . . .
H21B H 1.190355 0.303991 0.443468 0.061 Uiso 1 1 calc R U . . .
H21C H 1.120705 0.352294 0.511504 0.061 Uiso 1 1 calc R U . . .
C22 C 1.0125(3) 0.2488(2) 0.4259(2) 0.0311(9) Uani 1 1 d . . . . .
H22 H 1.023667 0.190794 0.393163 0.037 Uiso 1 1 calc R U . . .
C23 C 0.9814(3) 0.3082(2) 0.3615(2) 0.0259(8) Uani 1 1 d . . . . .
C24 C 1.0275(3) 0.3976(2) 0.3549(2) 0.0303(9) Uani 1 1 d . . . . .
H24 H 1.089949 0.437663 0.391672 0.036 Uiso 1 1 calc R U . . .
C25 C 0.9643(3) 0.4188(2) 0.2828(2) 0.0279(9) Uani 1 1 d . . . . .
C26 C 0.9856(3) 0.5066(2) 0.2433(2) 0.0319(9) Uani 1 1 d . . . . .
C27 C 0.9707(4) 0.5873(2) 0.3072(2) 0.0418(11) Uani 1 1 d . . . . .
H27A H 1.025222 0.593283 0.360048 0.050 Uiso 1 1 calc R U . . .
H27B H 0.889889 0.575888 0.323142 0.050 Uiso 1 1 calc R U . . .
C28 C 0.9028(4) 0.4995(2) 0.1613(2) 0.0379(10) Uani 1 1 d . . . . .
H28A H 0.820801 0.487781 0.174893 0.045 Uiso 1 1 calc R U . . .
H28B H 0.911811 0.447627 0.119555 0.045 Uiso 1 1 calc R U . . .
C29 C 1.1122(4) 0.5264(2) 0.2206(3) 0.0456(11) Uani 1 1 d . . . . .
H29A H 1.166903 0.531440 0.273228 0.055 Uiso 1 1 calc R U . . .
H29B H 1.123798 0.474990 0.179453 0.055 Uiso 1 1 calc R U . . .
C30 C 1.1388(4) 0.6145(3) 0.1814(3) 0.0611(14) Uani 1 1 d . . . . .
H30 H 1.221475 0.626359 0.167266 0.073 Uiso 1 1 calc R U . . .
C31 C 1.1218(5) 0.6939(3) 0.2454(3) 0.0730(16) Uani 1 1 d . . . . .
H31A H 1.175823 0.699972 0.298573 0.088 Uiso 1 1 calc R U . . .
H31B H 1.139998 0.751766 0.220422 0.088 Uiso 1 1 calc R U . . .
C32 C 0.9957(5) 0.6764(3) 0.2669(3) 0.0579(14) Uani 1 1 d . . . . .
H32 H 0.985002 0.728429 0.308722 0.069 Uiso 1 1 calc R U . . .
C33 C 0.9125(5) 0.6671(3) 0.1861(3) 0.0626(14) Uani 1 1 d . . . . .
H33A H 0.926879 0.725048 0.160886 0.075 Uiso 1 1 calc R U . . .
H33B H 0.830775 0.654580 0.200219 0.075 Uiso 1 1 calc R U . . .
C34 C 0.9302(4) 0.5892(3) 0.1213(3) 0.0496(12) Uani 1 1 d . . . . .
H34 H 0.875758 0.583826 0.067746 0.060 Uiso 1 1 calc R U . . .
C35 C 1.0556(4) 0.6063(3) 0.0996(3) 0.0618(14) Uani 1 1 d . . . . .
H35A H 1.073364 0.663436 0.073315 0.074 Uiso 1 1 calc R U . . .
H35B H 1.065987 0.555121 0.057632 0.074 Uiso 1 1 calc R U . . .
C40 C 0.8674(4) -0.0815(3) 0.3830(3) 0.0621(14) Uani 1 1 d . . . . .
H40A H 0.936500 -0.108684 0.383760 0.093 Uiso 1 1 calc R U . . .
H40B H 0.865336 -0.048187 0.439869 0.093 Uiso 1 1 calc R U . . .
H40C H 0.796632 -0.130050 0.368208 0.093 Uiso 1 1 calc R U . . .
C41 C 0.8854(3) -0.0652(3) 0.2284(2) 0.0430(11) Uani 1 1 d . . . . .
H41A H 0.954408 -0.092293 0.232487 0.065 Uiso 1 1 calc R U . . .
H41B H 0.815343 -0.113629 0.209535 0.065 Uiso 1 1 calc R U . . .
H41C H 0.893981 -0.021459 0.186739 0.065 Uiso 1 1 calc R U . . .
C42 C 0.8735(3) -0.0156(2) 0.3164(2) 0.0278(9) Uani 1 1 d . . . . .
H42 H 0.944901 0.034350 0.333734 0.033 Uiso 1 1 calc R U . . .
C43 C 0.7681(3) 0.0276(2) 0.3136(2) 0.0238(8) Uani 1 1 d . . . . .
C44 C 0.6560(3) -0.0059(2) 0.3318(2) 0.0268(9) Uani 1 1 d . . . . .
H44 H 0.626985 -0.063874 0.349047 0.032 Uiso 1 1 calc R U . . .
C45 C 0.5933(3) 0.0624(2) 0.3196(2) 0.0235(8) Uani 1 1 d . . . . .
C46 C 0.4643(3) 0.0568(2) 0.3224(2) 0.0231(8) Uani 1 1 d . . . . .
C47 C 0.3954(3) -0.0192(2) 0.2523(2) 0.0317(9) Uani 1 1 d . . . . .
H47A H 0.416704 -0.004747 0.195257 0.038 Uiso 1 1 calc R U . . .
H47B H 0.416531 -0.078058 0.261200 0.038 Uiso 1 1 calc R U . . .
C48 C 0.4280(3) 0.1469(2) 0.3075(2) 0.0303(9) Uani 1 1 d . . . . .
H48A H 0.470627 0.196818 0.352419 0.036 Uiso 1 1 calc R U . . .
H48B H 0.449060 0.163179 0.250939 0.036 Uiso 1 1 calc R U . . .
C49 C 0.4283(3) 0.0323(2) 0.4097(2) 0.0302(9) Uani 1 1 d . . . . .
H49A H 0.450789 -0.025691 0.420319 0.036 Uiso 1 1 calc R U . . .
H49B H 0.470223 0.081000 0.455997 0.036 Uiso 1 1 calc R U . . .
C50 C 0.2961(3) 0.0217(3) 0.4116(2) 0.0375(10) Uani 1 1 d . . . . .
H50 H 0.274542 0.005647 0.468796 0.045 Uiso 1 1 calc R U . . .
C51 C 0.2310(3) -0.0538(3) 0.3409(2) 0.0409(10) Uani 1 1 d . . . . .
H51A H 0.145541 -0.061115 0.342386 0.049 Uiso 1 1 calc R U . . .
H51B H 0.252129 -0.112591 0.350071 0.049 Uiso 1 1 calc R U . . .
C52 C 0.2636(3) -0.0287(3) 0.2539(2) 0.0366(10) Uani 1 1 d . . . . .
H52 H 0.221066 -0.078266 0.207517 0.044 Uiso 1 1 calc R U . . .
C53 C 0.2295(3) 0.0611(2) 0.2392(2) 0.0387(10) Uani 1 1 d . . . . .
H53A H 0.144150 0.054767 0.240254 0.046 Uiso 1 1 calc R U . . .
H53B H 0.249525 0.076952 0.182362 0.046 Uiso 1 1 calc R U . . .
C54 C 0.2954(3) 0.1367(3) 0.3100(3) 0.0391(10) Uani 1 1 d . . . . .
H54 H 0.273308 0.195791 0.300618 0.047 Uiso 1 1 calc R U . . .
C55 C 0.2641(3) 0.1128(3) 0.3973(2) 0.0405(10) Uani 1 1 d . . . . .
H55A H 0.179299 0.108086 0.400160 0.049 Uiso 1 1 calc R U . . .
H55B H 0.307236 0.161785 0.443015 0.049 Uiso 1 1 calc R U . . .
C60 C 1.0785(3) 0.2319(3) 0.1124(3) 0.0476(11) Uani 1 1 d . . . . .
H60A H 1.156225 0.218281 0.109226 0.071 Uiso 1 1 calc R U . . .
H60B H 1.070583 0.281476 0.078777 0.071 Uiso 1 1 calc R U . . .
H60C H 1.068603 0.250673 0.172502 0.071 Uiso 1 1 calc R U . . .
C61 C 1.0023(4) 0.1124(3) -0.0160(2) 0.0453(11) Uani 1 1 d . . . . .
H61A H 1.081347 0.100936 -0.017443 0.068 Uiso 1 1 calc R U . . .
H61B H 0.944637 0.055473 -0.036793 0.068 Uiso 1 1 calc R U . . .
H61C H 0.991951 0.158846 -0.052903 0.068 Uiso 1 1 calc R U . . .
C62 C 0.9851(3) 0.1465(3) 0.0763(2) 0.0341(9) Uani 1 1 d . . . . .
H62 H 0.993366 0.097302 0.112415 0.041 Uiso 1 1 calc R U . . .
C63 C 0.8648(3) 0.1644(2) 0.0801(2) 0.0260(8) Uani 1 1 d . . . . .
C64 C 0.7879(3) 0.1783(2) 0.0148(2) 0.0307(9) Uani 1 1 d . . . . .
H64 H 0.797276 0.173258 -0.044677 0.037 Uiso 1 1 calc R U . . .
C65 C 0.6932(3) 0.2013(2) 0.0532(2) 0.0253(8) Uani 1 1 d . . . . .
C66 C 0.5829(3) 0.2205(2) 0.0105(2) 0.0252(8) Uani 1 1 d . . . . .
C67 C 0.6120(3) 0.2873(3) -0.0550(2) 0.0374(10) Uani 1 1 d . . . . .
H67A H 0.660092 0.346132 -0.024944 0.045 Uiso 1 1 calc R U . . .
H67B H 0.658373 0.261776 -0.097419 0.045 Uiso 1 1 calc R U . . .
C68 C 0.5074(3) 0.1306(2) -0.0386(2) 0.0359(10) Uani 1 1 d . . . . .
H68A H 0.552788 0.103868 -0.081031 0.043 Uiso 1 1 calc R U . . .
H68B H 0.486841 0.086286 0.002213 0.043 Uiso 1 1 calc R U . . .
C69 C 0.5100(3) 0.2607(3) 0.0744(2) 0.0362(10) Uani 1 1 d . . . . .
H69A H 0.557011 0.318780 0.106570 0.043 Uiso 1 1 calc R U . . .
H69B H 0.488664 0.217572 0.116145 0.043 Uiso 1 1 calc R U . . .
C70 C 0.3984(3) 0.2786(3) 0.0281(2) 0.0389(10) Uani 1 1 d . . . . .
H70 H 0.351993 0.305097 0.070847 0.047 Uiso 1 1 calc R U . . .
C71 C 0.4317(4) 0.3452(3) -0.0359(3) 0.0468(11) Uani 1 1 d . . . . .
H71A H 0.360112 0.358119 -0.065182 0.056 Uiso 1 1 calc R U . . .
H71B H 0.479815 0.403591 -0.005102 0.056 Uiso 1 1 calc R U . . .
C72 C 0.5002(4) 0.3044(3) -0.1019(2) 0.0424(11) Uani 1 1 d . . . . .
H72 H 0.520986 0.347887 -0.144231 0.051 Uiso 1 1 calc R U . . .
C73 C 0.4285(4) 0.2135(3) -0.1485(2) 0.0437(11) Uani 1 1 d . . . . .
H73A H 0.356544 0.223521 -0.179856 0.052 Uiso 1 1 calc R U . . .
H73B H 0.474407 0.187397 -0.190894 0.052 Uiso 1 1 calc R U . . .
C74 C 0.3959(4) 0.1468(3) -0.0849(2) 0.0409(10) Uani 1 1 d . . . . .
H74 H 0.347898 0.087527 -0.115997 0.049 Uiso 1 1 calc R U . . .
C75 C 0.3265(3) 0.1880(3) -0.0198(2) 0.0448(11) Uani 1 1 d . . . . .
H75A H 0.304667 0.144796 0.021844 0.054 Uiso 1 1 calc R U . . .
H75B H 0.253607 0.198264 -0.049614 0.054 Uiso 1 1 calc R U . . .
B1 B 0.8638(4) 0.1738(3) 0.2476(2) 0.0223(9) Uani 1 1 d . . . . .
N1 N 0.8930(2) 0.27531(18) 0.29545(17) 0.0241(7) Uani 1 1 d . . . . .
N2 N 0.8826(3) 0.34578(19) 0.24640(17) 0.0282(7) Uani 1 1 d . . . . .
N3 N 0.7720(2) 0.11310(18) 0.29217(16) 0.0234(7) Uani 1 1 d . . . . .
N4 N 0.6635(2) 0.13514(18) 0.29698(17) 0.0251(7) Uani 1 1 d . . . . .
N5 N 0.8150(2) 0.17572(18) 0.15392(17) 0.0249(7) Uani 1 1 d . . . . .
N6 N 0.7088(2) 0.20019(18) 0.13757(17) 0.0246(7) Uani 1 1 d . . . . .
Ca1 Ca 0.66879(7) 0.28920(5) 0.26533(4) 0.0263(2) Uani 1 1 d . . . . .
H1B1 H 0.944(2) 0.1463(17) 0.2486(16) 0.012(7) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.530(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.415(5) . ?
C2 C9 1.491(5) . ?
C2 Ca1 2.675(3) . ?
C3 C8 1.419(5) . ?
C3 C4 1.441(5) . ?
C3 Ca1 2.672(3) . ?
C4 C5 1.390(5) . ?
C4 Ca1 2.779(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.363(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.378(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.395(5) . ?
C9 C10 1.401(5) . ?
C10 C11 1.385(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C20 C22 1.526(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.523(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.498(4) . ?
C22 H22 1.0000 . ?
C23 C24 1.366(5) . ?
C23 N1 1.376(4) . ?
C24 C25 1.407(5) . ?
C24 H24 0.9500 . ?
C25 N2 1.337(4) . ?
C25 C26 1.512(5) . ?
C26 C28 1.530(5) . ?
C26 C27 1.534(5) . ?
C26 C29 1.538(5) . ?
C27 C32 1.536(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C34 1.543(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.516(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C35 1.526(6) . ?
C30 C31 1.529(6) . ?
C30 H30 1.0000 . ?
C31 C32 1.525(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.512(6) . ?
C32 H32 1.0000 . ?
C33 C34 1.523(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.518(6) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C40 C42 1.523(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.529(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.511(4) . ?
C42 H42 1.0000 . ?
C43 N3 1.362(4) . ?
C43 C44 1.377(4) . ?
C44 C45 1.404(4) . ?
C44 H44 0.9500 . ?
C45 N4 1.335(4) . ?
C45 C46 1.505(5) . ?
C46 C49 1.537(4) . ?
C46 C47 1.537(4) . ?
C46 C48 1.540(4) . ?
C47 C52 1.528(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C54 1.539(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.532(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.524(5) . ?
C50 C55 1.531(5) . ?
C50 H50 1.0000 . ?
C51 C52 1.524(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.523(5) . ?
C52 H52 1.0000 . ?
C53 C54 1.528(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.520(5) . ?
C54 H54 1.0000 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C60 C62 1.526(5) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.531(5) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.496(5) . ?
C62 H62 1.0000 . ?
C63 N5 1.356(4) . ?
C63 C64 1.373(5) . ?
C64 C65 1.396(5) . ?
C64 H64 0.9500 . ?
C65 N6 1.330(4) . ?
C65 C66 1.504(5) . ?
C66 C69 1.527(5) . ?
C66 C67 1.536(4) . ?
C66 C68 1.539(5) . ?
C67 C72 1.535(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C74 1.521(5) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.533(5) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.522(5) . ?
C70 C75 1.525(5) . ?
C70 H70 1.0000 . ?
C71 C72 1.517(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.520(5) . ?
C72 H72 1.0000 . ?
C73 C74 1.518(5) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.519(5) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
B1 N3 1.540(5) . ?
B1 N5 1.544(4) . ?
B1 N1 1.580(5) . ?
B1 Ca1 3.157(4) . ?
B1 H1B1 1.10(3) . ?
N1 N2 1.403(3) . ?
N1 Ca1 2.691(3) . ?
N2 Ca1 2.538(3) . ?
N3 N4 1.387(3) . ?
N4 Ca1 2.419(3) . ?
N5 N6 1.383(3) . ?
N5 Ca1 3.158(3) . ?
N6 Ca1 2.422(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C9 122.6(3) . . ?
C3 C2 C1 118.3(3) . . ?
C9 C2 C1 113.3(3) . . ?
C3 C2 Ca1 74.53(19) . . ?
C9 C2 Ca1 130.4(2) . . ?
C1 C2 Ca1 88.8(2) . . ?
C2 C3 C8 124.3(3) . . ?
C2 C3 C4 121.7(4) . . ?
C8 C3 C4 113.6(3) . . ?
C2 C3 Ca1 74.78(19) . . ?
C8 C3 Ca1 111.8(2) . . ?
C4 C3 Ca1 78.80(19) . . ?
C5 C4 C3 121.7(4) . . ?
C5 C4 Ca1 119.8(2) . . ?
C3 C4 Ca1 70.63(18) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
Ca1 C4 H4 80.3 . . ?
C6 C5 C4 122.4(4) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 117.8(4) . . ?
C5 C6 H6 121.1 . . ?
C7 C6 H6 121.1 . . ?
C8 C7 C6 121.3(4) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C3 123.1(4) . . ?
C7 C8 H8 118.4 . . ?
C3 C8 H8 118.4 . . ?
C14 C9 C10 116.7(3) . . ?
C14 C9 C2 122.7(3) . . ?
C10 C9 C2 120.5(3) . . ?
C11 C10 C9 121.6(4) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C9 121.4(4) . . ?
C13 C14 H14 119.3 . . ?
C9 C14 H14 119.3 . . ?
C22 C20 H20A 109.5 . . ?
C22 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C22 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C21 111.3(3) . . ?
C23 C22 C20 112.0(3) . . ?
C21 C22 C20 111.1(3) . . ?
C23 C22 H22 107.4 . . ?
C21 C22 H22 107.4 . . ?
C20 C22 H22 107.4 . . ?
C24 C23 N1 108.1(3) . . ?
C24 C23 C22 130.5(3) . . ?
N1 C23 C22 121.4(3) . . ?
C23 C24 C25 106.4(3) . . ?
C23 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
N2 C25 C24 110.5(3) . . ?
N2 C25 C26 121.4(3) . . ?
C24 C25 C26 128.0(3) . . ?
C25 C26 C28 111.7(3) . . ?
C25 C26 C27 110.8(3) . . ?
C28 C26 C27 109.0(3) . . ?
C25 C26 C29 108.5(3) . . ?
C28 C26 C29 108.6(3) . . ?
C27 C26 C29 108.1(3) . . ?
C26 C27 C32 110.1(3) . . ?
C26 C27 H27A 109.6 . . ?
C32 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C32 C27 H27B 109.6 . . ?
H27A C27 H27B 108.2 . . ?
C26 C28 C34 110.0(3) . . ?
C26 C28 H28A 109.7 . . ?
C34 C28 H28A 109.7 . . ?
C26 C28 H28B 109.7 . . ?
C34 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C30 C29 C26 110.8(3) . . ?
C30 C29 H29A 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
C29 C30 C35 109.5(4) . . ?
C29 C30 C31 109.3(4) . . ?
C35 C30 C31 109.1(4) . . ?
C29 C30 H30 109.6 . . ?
C35 C30 H30 109.6 . . ?
C31 C30 H30 109.6 . . ?
C32 C31 C30 109.8(4) . . ?
C32 C31 H31A 109.7 . . ?
C30 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C30 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C33 C32 C31 110.1(4) . . ?
C33 C32 C27 109.6(4) . . ?
C31 C32 C27 108.6(4) . . ?
C33 C32 H32 109.5 . . ?
C31 C32 H32 109.5 . . ?
C27 C32 H32 109.5 . . ?
C32 C33 C34 109.8(4) . . ?
C32 C33 H33A 109.7 . . ?
C34 C33 H33A 109.7 . . ?
C32 C33 H33B 109.7 . . ?
C34 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
C35 C34 C33 110.6(4) . . ?
C35 C34 C28 109.5(3) . . ?
C33 C34 C28 108.4(3) . . ?
C35 C34 H34 109.5 . . ?
C33 C34 H34 109.5 . . ?
C28 C34 H34 109.5 . . ?
C34 C35 C30 109.5(4) . . ?
C34 C35 H35A 109.8 . . ?
C30 C35 H35A 109.8 . . ?
C34 C35 H35B 109.8 . . ?
C30 C35 H35B 109.8 . . ?
H35A C35 H35B 108.2 . . ?
C42 C40 H40A 109.5 . . ?
C42 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C42 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C40 110.8(3) . . ?
C43 C42 C41 111.6(3) . . ?
C40 C42 C41 110.0(3) . . ?
C43 C42 H42 108.1 . . ?
C40 C42 H42 108.1 . . ?
C41 C42 H42 108.1 . . ?
N3 C43 C44 107.4(3) . . ?
N3 C43 C42 122.6(3) . . ?
C44 C43 C42 130.0(3) . . ?
C43 C44 C45 106.5(3) . . ?
C43 C44 H44 126.8 . . ?
C45 C44 H44 126.8 . . ?
N4 C45 C44 109.9(3) . . ?
N4 C45 C46 122.1(3) . . ?
C44 C45 C46 127.9(3) . . ?
C45 C46 C49 110.5(3) . . ?
C45 C46 C47 109.3(3) . . ?
C49 C46 C47 107.9(3) . . ?
C45 C46 C48 112.7(3) . . ?
C49 C46 C48 108.4(3) . . ?
C47 C46 C48 108.1(3) . . ?
C52 C47 C46 111.1(3) . . ?
C52 C47 H47A 109.4 . . ?
C46 C47 H47A 109.4 . . ?
C52 C47 H47B 109.4 . . ?
C46 C47 H47B 109.4 . . ?
H47A C47 H47B 108.0 . . ?
C54 C48 C46 110.3(3) . . ?
C54 C48 H48A 109.6 . . ?
C46 C48 H48A 109.6 . . ?
C54 C48 H48B 109.6 . . ?
C46 C48 H48B 109.6 . . ?
H48A C48 H48B 108.1 . . ?
C50 C49 C46 110.9(3) . . ?
C50 C49 H49A 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 108.0 . . ?
C51 C50 C55 110.0(3) . . ?
C51 C50 C49 109.7(3) . . ?
C55 C50 C49 108.4(3) . . ?
C51 C50 H50 109.6 . . ?
C55 C50 H50 109.6 . . ?
C49 C50 H50 109.6 . . ?
C50 C51 C52 109.3(3) . . ?
C50 C51 H51A 109.8 . . ?
C52 C51 H51A 109.8 . . ?
C50 C51 H51B 109.8 . . ?
C52 C51 H51B 109.8 . . ?
H51A C51 H51B 108.3 . . ?
C53 C52 C51 109.8(3) . . ?
C53 C52 C47 110.0(3) . . ?
C51 C52 C47 109.1(3) . . ?
C53 C52 H52 109.3 . . ?
C51 C52 H52 109.3 . . ?
C47 C52 H52 109.3 . . ?
C52 C53 C54 109.1(3) . . ?
C52 C53 H53A 109.9 . . ?
C54 C53 H53A 109.9 . . ?
C52 C53 H53B 109.9 . . ?
C54 C53 H53B 109.9 . . ?
H53A C53 H53B 108.3 . . ?
C55 C54 C53 110.0(3) . . ?
C55 C54 C48 109.2(3) . . ?
C53 C54 C48 109.6(3) . . ?
C55 C54 H54 109.3 . . ?
C53 C54 H54 109.3 . . ?
C48 C54 H54 109.3 . . ?
C54 C55 C50 109.7(3) . . ?
C54 C55 H55A 109.7 . . ?
C50 C55 H55A 109.7 . . ?
C54 C55 H55B 109.7 . . ?
C50 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C62 C60 H60A 109.5 . . ?
C62 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C62 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C60 111.1(3) . . ?
C63 C62 C61 110.4(3) . . ?
C60 C62 C61 110.7(3) . . ?
C63 C62 H62 108.2 . . ?
C60 C62 H62 108.2 . . ?
C61 C62 H62 108.2 . . ?
N5 C63 C64 107.1(3) . . ?
N5 C63 C62 123.8(3) . . ?
C64 C63 C62 129.0(3) . . ?
C63 C64 C65 106.4(3) . . ?
C63 C64 H64 126.8 . . ?
C65 C64 H64 126.8 . . ?
N6 C65 C64 110.3(3) . . ?
N6 C65 C66 121.3(3) . . ?
C64 C65 C66 128.3(3) . . ?
C65 C66 C69 112.9(3) . . ?
C65 C66 C67 110.4(3) . . ?
C69 C66 C67 108.4(3) . . ?
C65 C66 C68 109.1(3) . . ?
C69 C66 C68 108.1(3) . . ?
C67 C66 C68 107.7(3) . . ?
C72 C67 C66 111.0(3) . . ?
C72 C67 H67A 109.4 . . ?
C66 C67 H67A 109.4 . . ?
C72 C67 H67B 109.4 . . ?
C66 C67 H67B 109.4 . . ?
H67A C67 H67B 108.0 . . ?
C74 C68 C66 111.2(3) . . ?
C74 C68 H68A 109.4 . . ?
C66 C68 H68A 109.4 . . ?
C74 C68 H68B 109.4 . . ?
C66 C68 H68B 109.4 . . ?
H68A C68 H68B 108.0 . . ?
C66 C69 C70 111.0(3) . . ?
C66 C69 H69A 109.4 . . ?
C70 C69 H69A 109.4 . . ?
C66 C69 H69B 109.4 . . ?
C70 C69 H69B 109.4 . . ?
H69A C69 H69B 108.0 . . ?
C71 C70 C75 109.5(3) . . ?
C71 C70 C69 109.2(3) . . ?
C75 C70 C69 108.5(3) . . ?
C71 C70 H70 109.9 . . ?
C75 C70 H70 109.9 . . ?
C69 C70 H70 109.9 . . ?
C72 C71 C70 110.0(3) . . ?
C72 C71 H71A 109.7 . . ?
C70 C71 H71A 109.7 . . ?
C72 C71 H71B 109.7 . . ?
C70 C71 H71B 109.7 . . ?
H71A C71 H71B 108.2 . . ?
C71 C72 C73 110.4(3) . . ?
C71 C72 C67 108.5(3) . . ?
C73 C72 C67 108.6(3) . . ?
C71 C72 H72 109.8 . . ?
C73 C72 H72 109.8 . . ?
C67 C72 H72 109.8 . . ?
C74 C73 C72 110.4(3) . . ?
C74 C73 H73A 109.6 . . ?
C72 C73 H73A 109.6 . . ?
C74 C73 H73B 109.6 . . ?
C72 C73 H73B 109.6 . . ?
H73A C73 H73B 108.1 . . ?
C73 C74 C68 108.9(3) . . ?
C73 C74 C75 109.0(3) . . ?
C68 C74 C75 109.3(3) . . ?
C73 C74 H74 109.9 . . ?
C68 C74 H74 109.9 . . ?
C75 C74 H74 109.9 . . ?
C74 C75 C70 110.5(3) . . ?
C74 C75 H75A 109.5 . . ?
C70 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
C70 C75 H75B 109.5 . . ?
H75A C75 H75B 108.1 . . ?
N3 B1 N5 109.9(3) . . ?
N3 B1 N1 110.0(3) . . ?
N5 B1 N1 107.9(3) . . ?
N3 B1 Ca1 77.07(19) . . ?
N5 B1 Ca1 75.89(18) . . ?
N1 B1 Ca1 58.44(16) . . ?
N3 B1 H1B1 109.4(14) . . ?
N5 B1 H1B1 109.9(13) . . ?
N1 B1 H1B1 109.8(14) . . ?
Ca1 B1 H1B1 168.2(14) . . ?
C23 N1 N2 108.9(3) . . ?
C23 N1 B1 123.9(3) . . ?
N2 N1 B1 117.9(2) . . ?
C23 N1 Ca1 135.1(2) . . ?
N2 N1 Ca1 68.50(16) . . ?
B1 N1 Ca1 91.55(19) . . ?
C25 N2 N1 106.2(3) . . ?
C25 N2 Ca1 133.4(2) . . ?
N1 N2 Ca1 80.55(17) . . ?
C43 N3 N4 109.7(3) . . ?
C43 N3 B1 130.0(3) . . ?
N4 N3 B1 118.7(3) . . ?
C45 N4 N3 106.6(3) . . ?
C45 N4 Ca1 142.6(2) . . ?
N3 N4 Ca1 110.84(19) . . ?
C63 N5 N6 110.2(3) . . ?
C63 N5 B1 130.1(3) . . ?
N6 N5 B1 119.5(3) . . ?
C63 N5 Ca1 147.2(2) . . ?
N6 N5 Ca1 46.44(14) . . ?
B1 N5 Ca1 75.81(18) . . ?
C65 N6 N5 106.0(3) . . ?
C65 N6 Ca1 136.5(2) . . ?
N5 N6 Ca1 109.11(18) . . ?
N4 Ca1 N6 72.29(9) . . ?
N4 Ca1 N2 102.47(9) . . ?
N6 Ca1 N2 72.53(9) . . ?
N4 Ca1 C3 125.92(10) . . ?
N6 Ca1 C3 150.40(10) . . ?
N2 Ca1 C3 118.36(11) . . ?
N4 Ca1 C2 104.46(10) . . ?
N6 Ca1 C2 176.28(10) . . ?
N2 Ca1 C2 110.26(11) . . ?
C3 Ca1 C2 30.69(10) . . ?
N4 Ca1 N1 73.68(9) . . ?
N6 Ca1 N1 74.30(9) . . ?
N2 Ca1 N1 30.94(8) . . ?
C3 Ca1 N1 130.10(11) . . ?
C2 Ca1 N1 106.74(10) . . ?
N4 Ca1 C4 156.50(10) . . ?
N6 Ca1 C4 128.42(10) . . ?
N2 Ca1 C4 95.44(11) . . ?
C3 Ca1 C4 30.58(10) . . ?
C2 Ca1 C4 54.38(10) . . ?
N1 Ca1 C4 119.31(11) . . ?
N4 Ca1 B1 51.69(10) . . ?
N6 Ca1 B1 51.91(9) . . ?
N2 Ca1 B1 51.97(9) . . ?
C3 Ca1 B1 157.13(11) . . ?
C2 Ca1 B1 127.62(11) . . ?
N1 Ca1 B1 30.01(9) . . ?
C4 Ca1 B1 147.25(12) . . ?
N4 Ca1 N5 64.32(8) . . ?
N6 Ca1 N5 24.45(8) . . ?
N2 Ca1 N5 55.86(8) . . ?
C3 Ca1 N5 169.68(9) . . ?
C2 Ca1 N5 155.67(10) . . ?
N1 Ca1 N5 50.38(8) . . ?
C4 Ca1 N5 139.18(9) . . ?
B1 Ca1 N5 28.30(8) . . ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.055

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MA001
_database_code_depnum_ccdc_archive 'CCDC 1967138'
loop_
_audit_author_name
_audit_author_address
'Jianhua Cheng'
;CIAC, CAS
China
;
_audit_update_record             
;
2019-11-21 deposited with the CCDC.	2020-03-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        '[(TpAd,iPr)Ca(CH2CH2CH2CH2C6H5)(THP)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H93 B Ca N6 O'
_chemical_formula_sum            'C63 H93 B Ca N6 O'
_chemical_formula_weight         1001.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.5913(16)
_cell_length_b                   14.6823(16)
_cell_length_c                   15.1498(16)
_cell_angle_alpha                61.123(2)
_cell_angle_beta                 82.567(2)
_cell_angle_gamma                88.425(2)
_cell_volume                     2815.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    3881
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.28

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.158
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   
'Sheldrick, G. M. SADABS, Version 2.10; Bruker AXS, Inc.: Madison, WI 2003.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13854
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.585
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             9656
_reflns_number_gt                7115
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis,2007)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2018)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0624P)²+0.3376P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   iterative
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9656
_refine_ls_number_parameters     633
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.23910(16) 0.06995(18) 0.41456(17) 0.0217(5) Uani 1 1 d . . . . .
H1A H 0.186893 0.018094 0.450242 0.026 Uiso 1 1 calc R U . . .
H1B H 0.296140 0.033046 0.438309 0.026 Uiso 1 1 calc R U . . .
C2 C 0.22689(16) 0.15036(18) 0.45124(17) 0.0221(5) Uani 1 1 d . . . . .
H2A H 0.168965 0.186410 0.429864 0.026 Uiso 1 1 calc R U . . .
H2B H 0.278510 0.203048 0.415812 0.026 Uiso 1 1 calc R U . . .
C3 C 0.22329(17) 0.10968(18) 0.56558(17) 0.0263(6) Uani 1 1 d . . . . .
H3A H 0.279629 0.070558 0.588204 0.032 Uiso 1 1 calc R U . . .
H3B H 0.169375 0.060265 0.601312 0.032 Uiso 1 1 calc R U . . .
C4 C 0.21619(18) 0.1948(2) 0.59773(19) 0.0306(6) Uani 1 1 d . . . . .
H4A H 0.165496 0.240617 0.566379 0.037 Uiso 1 1 calc R U . . .
H4B H 0.199556 0.161209 0.672457 0.037 Uiso 1 1 calc R U . . .
C5 C 0.30351(17) 0.26073(18) 0.56835(18) 0.0254(5) Uani 1 1 d . . . . .
C6 C 0.38004(19) 0.2190(2) 0.61906(19) 0.0325(6) Uani 1 1 d . . . . .
H6 H 0.375459 0.149961 0.674269 0.039 Uiso 1 1 calc R U . . .
C7 C 0.46216(19) 0.2760(2) 0.5907(2) 0.0377(7) Uani 1 1 d . . . . .
H7 H 0.513420 0.245901 0.626326 0.045 Uiso 1 1 calc R U . . .
C8 C 0.47062(19) 0.3768(2) 0.5106(2) 0.0364(7) Uani 1 1 d . . . . .
H8 H 0.527445 0.415917 0.490734 0.044 Uiso 1 1 calc R U . . .
C9 C 0.39524(19) 0.4197(2) 0.4601(2) 0.0330(6) Uani 1 1 d . . . . .
H9 H 0.400045 0.488845 0.405082 0.040 Uiso 1 1 calc R U . . .
C10 C 0.31280(18) 0.36227(19) 0.48946(18) 0.0274(6) Uani 1 1 d . . . . .
H10 H 0.261264 0.393220 0.454641 0.033 Uiso 1 1 calc R U . . .
C11 C 0.04227(16) 0.12093(18) 0.15533(17) 0.0223(5) Uani 1 1 d . . . . .
H11A H 0.009194 0.052983 0.181552 0.027 Uiso 1 1 calc R U . . .
H11B H 0.091997 0.128478 0.100896 0.027 Uiso 1 1 calc R U . . .
C12 C -0.02392(16) 0.20667(19) 0.11185(19) 0.0278(6) Uani 1 1 d . . . . .
H12A H -0.051378 0.202751 0.057284 0.033 Uiso 1 1 calc R U . . .
H12B H 0.009569 0.274966 0.081836 0.033 Uiso 1 1 calc R U . . .
C13 C -0.10018(17) 0.1968(2) 0.1950(2) 0.0333(6) Uani 1 1 d . . . . .
H13A H -0.139476 0.257948 0.167970 0.040 Uiso 1 1 calc R U . . .
H13B H -0.139639 0.133624 0.217689 0.040 Uiso 1 1 calc R U . . .
C14 C -0.05818(17) 0.1899(2) 0.2847(2) 0.0338(6) Uani 1 1 d . . . . .
H14A H -0.028763 0.258193 0.265123 0.041 Uiso 1 1 calc R U . . .
H14B H -0.107828 0.173549 0.341976 0.041 Uiso 1 1 calc R U . . .
C15 C 0.01291(16) 0.1076(2) 0.31889(18) 0.0264(6) Uani 1 1 d . . . . .
H15A H 0.042548 0.109446 0.373229 0.032 Uiso 1 1 calc R U . . .
H15B H -0.018155 0.038125 0.347606 0.032 Uiso 1 1 calc R U . . .
C20 C 0.2415(2) -0.0429(2) -0.11811(19) 0.0364(7) Uani 1 1 d . . . . .
H20A H 0.236466 -0.018421 -0.189948 0.055 Uiso 1 1 calc R U . . .
H20B H 0.306756 -0.051282 -0.107672 0.055 Uiso 1 1 calc R U . . .
H20C H 0.207488 -0.109979 -0.076191 0.055 Uiso 1 1 calc R U . . .
C21 C 0.10062(19) 0.0572(2) -0.1075(2) 0.0409(7) Uani 1 1 d . . . . .
H21A H 0.096545 0.080195 -0.179223 0.061 Uiso 1 1 calc R U . . .
H21B H 0.062340 -0.006741 -0.064684 0.061 Uiso 1 1 calc R U . . .
H21C H 0.078512 0.111595 -0.091100 0.061 Uiso 1 1 calc R U . . .
C22 C 0.20081(17) 0.03616(18) -0.08785(17) 0.0236(5) Uani 1 1 d . . . . .
H22 H 0.237929 0.103080 -0.129884 0.028 Uiso 1 1 calc R U . . .
C23 C 0.20750(15) 0.00074(17) 0.02234(17) 0.0201(5) Uani 1 1 d . . . . .
C24 C 0.17262(16) -0.09079(17) 0.10524(17) 0.0226(5) Uani 1 1 d . . . . .
H24 H 0.140553 -0.145869 0.104601 0.027 Uiso 1 1 calc R U . . .
C25 C 0.19361(15) -0.08686(16) 0.19047(17) 0.0178(5) Uani 1 1 d . . . . .
C26 C 0.17450(15) -0.17077(17) 0.30077(16) 0.0202(5) Uani 1 1 d D . . . .
C27 C 0.2609(2) -0.1839(2) 0.3549(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H27A H 0.314563 -0.199021 0.317588 0.036 Uiso 0.872(2) 1 calc R U P A 2
H27B H 0.275361 -0.118117 0.354346 0.036 Uiso 0.872(2) 1 calc R U P A 2
C28 C 0.0931(2) -0.1475(2) 0.3601(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H28A H 0.036921 -0.139158 0.326984 0.036 Uiso 0.872(2) 1 calc R U P A 2
H28B H 0.106434 -0.081327 0.359333 0.036 Uiso 0.872(2) 1 calc R U P A 2
C29 C 0.1525(2) -0.2755(2) 0.3055(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H29A H 0.097188 -0.269045 0.271681 0.036 Uiso 0.872(2) 1 calc R U P A 2
H29B H 0.205070 -0.292526 0.268413 0.036 Uiso 0.872(2) 1 calc R U P A 2
C30 C 0.1348(2) -0.3642(2) 0.4163(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H30 H 0.120810 -0.431084 0.417420 0.036 Uiso 0.872(2) 1 calc R U P A 2
C31 C 0.0534(2) -0.3377(3) 0.4720(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H31A H 0.040657 -0.394577 0.543087 0.036 Uiso 0.872(2) 1 calc R U P A 2
H31B H -0.002412 -0.330448 0.438603 0.036 Uiso 0.872(2) 1 calc R U P A 2
C32 C 0.0754(2) -0.2359(2) 0.4709(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H32 H 0.022080 -0.219173 0.508496 0.036 Uiso 0.872(2) 1 calc R U P A 2
C33 C 0.1625(2) -0.2471(2) 0.5217(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H33A H 0.176515 -0.181341 0.521385 0.036 Uiso 0.872(2) 1 calc R U P A 2
H33B H 0.151597 -0.303186 0.593288 0.036 Uiso 0.872(2) 1 calc R U P A 2
C34 C 0.2444(2) -0.2726(2) 0.4652(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H34 H 0.300791 -0.280117 0.498843 0.036 Uiso 0.872(2) 1 calc R U P A 2
C35 C 0.2226(2) -0.3733(2) 0.4653(2) 0.0301(3) Uani 0.872(2) 1 d D . P A 2
H35A H 0.213761 -0.431241 0.536139 0.036 Uiso 0.872(2) 1 calc R U P A 2
H35B H 0.275214 -0.389054 0.427281 0.036 Uiso 0.872(2) 1 calc R U P A 2
C27' C 0.2270(13) -0.2668(11) 0.3218(13) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H27C H 0.293981 -0.251029 0.314442 0.036 Uiso 0.128(2) 1 calc R U P A 1
H27D H 0.217053 -0.289237 0.271678 0.036 Uiso 0.128(2) 1 calc R U P A 1
C28' C 0.1923(14) -0.1287(13) 0.3721(11) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H28C H 0.151297 -0.070280 0.361004 0.036 Uiso 0.128(2) 1 calc R U P A 1
H28D H 0.257063 -0.101419 0.355507 0.036 Uiso 0.128(2) 1 calc R U P A 1
C29' C 0.0690(9) -0.2026(14) 0.3247(13) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H29C H 0.054610 -0.234108 0.282987 0.036 Uiso 0.128(2) 1 calc R U P A 1
H29D H 0.032490 -0.139473 0.305746 0.036 Uiso 0.128(2) 1 calc R U P A 1
C30' C 0.0924(13) -0.3764(15) 0.4536(17) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H30A H 0.075703 -0.433230 0.524112 0.036 Uiso 0.128(2) 1 calc R U P A 1
H30B H 0.073101 -0.399843 0.407199 0.036 Uiso 0.128(2) 1 calc R U P A 1
C31' C 0.0399(14) -0.2820(14) 0.4401(13) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H31' H -0.028393 -0.297113 0.456764 0.036 Uiso 0.128(2) 1 calc R U P A 1
C32' C 0.0759(12) -0.2450(18) 0.5061(15) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H32A H 0.039642 -0.184921 0.500559 0.036 Uiso 0.128(2) 1 calc R U P A 1
H32B H 0.062955 -0.301234 0.577466 0.036 Uiso 0.128(2) 1 calc R U P A 1
C33' C 0.1748(12) -0.2137(13) 0.4858(14) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H33' H 0.193370 -0.190018 0.532891 0.036 Uiso 0.128(2) 1 calc R U P A 1
C34' C 0.2213(15) -0.3110(14) 0.4969(16) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H34A H 0.209124 -0.364865 0.569271 0.036 Uiso 0.128(2) 1 calc R U P A 1
H34B H 0.288889 -0.295452 0.480477 0.036 Uiso 0.128(2) 1 calc R U P A 1
C35' C 0.1942(13) -0.3579(15) 0.4331(13) 0.0301(3) Uani 0.128(2) 1 d D . P A 1
H35' H 0.227340 -0.423169 0.447551 0.036 Uiso 0.128(2) 1 calc R U P A 1
C40 C 0.30891(18) 0.4211(2) -0.27577(19) 0.0354(6) Uani 1 1 d . . . . .
H40A H 0.314210 0.424881 -0.342595 0.053 Uiso 1 1 calc R U . . .
H40B H 0.297022 0.490364 -0.283196 0.053 Uiso 1 1 calc R U . . .
H40C H 0.366677 0.396796 -0.246638 0.053 Uiso 1 1 calc R U . . .
C41 C 0.13954(19) 0.3774(2) -0.2520(2) 0.0386(7) Uani 1 1 d . . . . .
H41A H 0.147675 0.380999 -0.318901 0.058 Uiso 1 1 calc R U . . .
H41B H 0.089951 0.325936 -0.207557 0.058 Uiso 1 1 calc R U . . .
H41C H 0.123235 0.445771 -0.259633 0.058 Uiso 1 1 calc R U . . .
C42 C 0.22919(18) 0.34547(18) -0.20548(17) 0.0276(6) Uani 1 1 d . . . . .
H42 H 0.243768 0.274943 -0.196969 0.033 Uiso 1 1 calc R U . . .
C43 C 0.22007(16) 0.33880(17) -0.10209(17) 0.0219(5) Uani 1 1 d . . . . .
C44 C 0.18890(17) 0.41320(18) -0.07607(17) 0.0257(6) Uani 1 1 d . . . . .
H44 H 0.165168 0.478579 -0.119173 0.031 Uiso 1 1 calc R U . . .
C45 C 0.19916(15) 0.37324(16) 0.02641(17) 0.0186(5) Uani 1 1 d . . . . .
C46 C 0.18675(15) 0.42936(16) 0.08797(16) 0.0190(5) Uani 1 1 d . . . . .
C47 C 0.09800(16) 0.49140(18) 0.06866(18) 0.0230(5) Uani 1 1 d . . . . .
H47A H 0.099305 0.538840 -0.005201 0.028 Uiso 1 1 calc R U . . .
H47B H 0.043521 0.442827 0.092113 0.028 Uiso 1 1 calc R U . . .
C48 C 0.18364(16) 0.35650(17) 0.20306(16) 0.0198(5) Uani 1 1 d . . . . .
H48A H 0.131043 0.305325 0.227524 0.024 Uiso 1 1 calc R U . . .
H48B H 0.241329 0.317738 0.216656 0.024 Uiso 1 1 calc R U . . .
C49 C 0.26972(17) 0.50663(18) 0.05332(18) 0.0246(5) Uani 1 1 d . . . . .
H49A H 0.327568 0.468071 0.065551 0.030 Uiso 1 1 calc R U . . .
H49B H 0.273121 0.555014 -0.020583 0.030 Uiso 1 1 calc R U . . .
C50 C 0.26105(18) 0.56895(18) 0.11079(18) 0.0279(6) Uani 1 1 d . . . . .
H50 H 0.315764 0.618420 0.087181 0.033 Uiso 1 1 calc R U . . .
C51 C 0.25651(17) 0.49464(18) 0.22502(18) 0.0264(6) Uani 1 1 d . . . . .
H51A H 0.313910 0.455391 0.239247 0.032 Uiso 1 1 calc R U . . .
H51B H 0.251050 0.534805 0.262275 0.032 Uiso 1 1 calc R U . . .
C52 C 0.17289(17) 0.41894(17) 0.26081(17) 0.0230(5) Uani 1 1 d . . . . .
H52 H 0.169855 0.370254 0.335461 0.028 Uiso 1 1 calc R U . . .
C53 C 0.08426(17) 0.47995(19) 0.23938(18) 0.0279(6) Uani 1 1 d . . . . .
H53A H 0.077111 0.519711 0.277038 0.033 Uiso 1 1 calc R U . . .
H53B H 0.029969 0.431167 0.262593 0.033 Uiso 1 1 calc R U . . .
C54 C 0.08936(17) 0.55481(18) 0.12496(18) 0.0275(6) Uani 1 1 d . . . . .
H54 H 0.031674 0.595023 0.110943 0.033 Uiso 1 1 calc R U . . .
C55 C 0.17273(19) 0.62986(18) 0.08952(19) 0.0326(6) Uani 1 1 d . . . . .
H55A H 0.166630 0.671033 0.125773 0.039 Uiso 1 1 calc R U . . .
H55B H 0.175741 0.678637 0.015741 0.039 Uiso 1 1 calc R U . . .
C60 C 0.5250(2) 0.1023(2) -0.1321(2) 0.0393(7) Uani 1 1 d . . . . .
H60A H 0.538005 0.114355 -0.202130 0.059 Uiso 1 1 calc R U . . .
H60B H 0.579477 0.074381 -0.097316 0.059 Uiso 1 1 calc R U . . .
H60C H 0.472394 0.052392 -0.096161 0.059 Uiso 1 1 calc R U . . .
C61 C 0.57978(19) 0.2868(2) -0.19359(19) 0.0378(7) Uani 1 1 d . . . . .
H61A H 0.592818 0.295949 -0.262549 0.057 Uiso 1 1 calc R U . . .
H61B H 0.561217 0.353021 -0.197095 0.057 Uiso 1 1 calc R U . . .
H61C H 0.635435 0.264220 -0.159796 0.057 Uiso 1 1 calc R U . . .
C62 C 0.50180(16) 0.20479(17) -0.13343(17) 0.0213(5) Uani 1 1 d . . . . .
H62 H 0.445140 0.230822 -0.167612 0.026 Uiso 1 1 calc R U . . .
C63 C 0.48112(15) 0.19010(17) -0.02673(17) 0.0186(5) Uani 1 1 d . . . . .
C64 C 0.54111(15) 0.20167(17) 0.03022(17) 0.0198(5) Uani 1 1 d . . . . .
H64 H 0.605569 0.218503 0.011359 0.024 Uiso 1 1 calc R U . . .
C65 C 0.48861(15) 0.18378(16) 0.12134(16) 0.0176(5) Uani 1 1 d . . . . .
C66 C 0.51979(15) 0.19651(18) 0.20631(17) 0.0200(5) Uani 1 1 d . . . . .
C67 C 0.53422(17) 0.09111(18) 0.29908(18) 0.0253(5) Uani 1 1 d . . . . .
H67A H 0.475282 0.049235 0.326463 0.030 Uiso 1 1 calc R U . . .
H67B H 0.580403 0.052091 0.278253 0.030 Uiso 1 1 calc R U . . .
C68 C 0.44844(16) 0.25491(19) 0.24181(18) 0.0249(5) Uani 1 1 d . . . . .
H68A H 0.437560 0.322724 0.183106 0.030 Uiso 1 1 calc R U . . .
H68B H 0.389050 0.213904 0.269397 0.030 Uiso 1 1 calc R U . . .
C69 C 0.61188(16) 0.26027(19) 0.16718(18) 0.0261(6) Uani 1 1 d . . . . .
H69A H 0.603763 0.328387 0.107459 0.031 Uiso 1 1 calc R U . . .
H69B H 0.659056 0.223088 0.145095 0.031 Uiso 1 1 calc R U . . .
C70 C 0.64593(16) 0.27807(19) 0.24980(19) 0.0273(6) Uani 1 1 d . . . . .
H70 H 0.706047 0.319266 0.222406 0.033 Uiso 1 1 calc R U . . .
C71 C 0.65945(17) 0.1724(2) 0.33995(19) 0.0314(6) Uani 1 1 d . . . . .
H71A H 0.682120 0.181996 0.393843 0.038 Uiso 1 1 calc R U . . .
H71B H 0.706303 0.134566 0.318278 0.038 Uiso 1 1 calc R U . . .
C72 C 0.56801(17) 0.1090(2) 0.38161(18) 0.0288(6) Uani 1 1 d . . . . .
H72 H 0.577071 0.040273 0.441660 0.035 Uiso 1 1 calc R U . . .
C73 C 0.49629(17) 0.1681(2) 0.41414(19) 0.0319(6) Uani 1 1 d . . . . .
H73A H 0.436848 0.127234 0.441602 0.038 Uiso 1 1 calc R U . . .
H73B H 0.517242 0.178291 0.468503 0.038 Uiso 1 1 calc R U . . .
C74 C 0.48257(17) 0.2731(2) 0.32400(19) 0.0291(6) Uani 1 1 d . . . . .
H74 H 0.435157 0.311069 0.346005 0.035 Uiso 1 1 calc R U . . .
C75 C 0.57379(17) 0.3377(2) 0.2816(2) 0.0322(6) Uani 1 1 d . . . . .
H75A H 0.564714 0.405711 0.222257 0.039 Uiso 1 1 calc R U . . .
H75B H 0.595176 0.350593 0.334149 0.039 Uiso 1 1 calc R U . . .
B1 B 0.30372(17) 0.1628(2) -0.00900(19) 0.0180(5) Uani 1 1 d . . . . .
N1 N 0.24799(12) 0.05719(14) 0.05689(13) 0.0166(4) Uani 1 1 d . . . . .
N2 N 0.23902(12) 0.00322(14) 0.16201(13) 0.0172(4) Uani 1 1 d . . . . .
N3 N 0.24691(12) 0.25741(14) -0.01758(13) 0.0184(4) Uani 1 1 d . . . . .
N4 N 0.23326(12) 0.27855(13) 0.06244(13) 0.0176(4) Uani 1 1 d . . . . .
N5 N 0.39625(12) 0.16403(14) 0.02950(13) 0.0172(4) Uani 1 1 d . . . . .
N6 N 0.40077(12) 0.15996(14) 0.12185(13) 0.0181(4) Uani 1 1 d . . . . .
Ca1 Ca 0.24900(3) 0.12534(3) 0.22839(3) 0.01618(13) Uani 1 1 d . . . . .
O1 O 0.08266(10) 0.12267(12) 0.23635(11) 0.0214(4) Uani 1 1 d . . . . .
H1B1 H 0.3214(13) 0.1716(14) -0.0867(15) 0.005(5) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.527(3) . ?
C1 Ca1 2.515(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.529(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.542(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.505(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.385(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.377(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.381(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 O1 1.440(3) . ?
C11 C12 1.499(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.522(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.521(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.507(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O1 1.437(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C20 C22 1.522(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.523(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.506(3) . ?
C22 H22 1.0000 . ?
C23 N1 1.355(3) . ?
C23 C24 1.373(3) . ?
C24 C25 1.393(3) . ?
C24 H24 0.9500 . ?
C25 N2 1.341(3) . ?
C25 C26 1.516(3) . ?
C26 C27' 1.498(12) . ?
C26 C28 1.528(3) . ?
C26 C28' 1.530(12) . ?
C26 C29 1.545(3) . ?
C26 C27 1.549(4) . ?
C26 C29' 1.565(13) . ?
C27 C34 1.536(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C32 1.540(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.540(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.519(4) . ?
C30 C35 1.534(4) . ?
C30 H30 1.0000 . ?
C31 C32 1.529(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.535(4) . ?
C32 H32 1.0000 . ?
C33 C34 1.523(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.519(4) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C27' C35' 1.584(19) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' C33' 1.554(19) . ?
C28' H28C 0.9900 . ?
C28' H28D 0.9900 . ?
C29' C31' 1.569(19) . ?
C29' H29C 0.9900 . ?
C29' H29D 0.9900 . ?
C30' C35' 1.484(16) . ?
C30' C31' 1.502(15) . ?
C30' H30A 0.9900 . ?
C30' H30B 0.9900 . ?
C31' C32' 1.498(15) . ?
C31' H31' 1.0000 . ?
C32' C33' 1.474(16) . ?
C32' H32A 0.9900 . ?
C32' H32B 0.9900 . ?
C33' C34' 1.508(16) . ?
C33' H33' 1.0000 . ?
C34' C35' 1.523(16) . ?
C34' H34A 0.9900 . ?
C34' H34B 0.9900 . ?
C35' H35' 1.0000 . ?
C40 C42 1.526(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.521(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.510(3) . ?
C42 H42 1.0000 . ?
C43 N3 1.359(3) . ?
C43 C44 1.378(3) . ?
C44 C45 1.397(3) . ?
C44 H44 0.9500 . ?
C45 N4 1.333(3) . ?
C45 C46 1.507(3) . ?
C46 C49 1.538(3) . ?
C46 C48 1.539(3) . ?
C46 C47 1.539(3) . ?
C47 C54 1.531(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C52 1.537(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.532(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C55 1.526(4) . ?
C50 C51 1.530(3) . ?
C50 H50 1.0000 . ?
C51 C52 1.529(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.531(3) . ?
C52 H52 1.0000 . ?
C53 C54 1.533(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.522(4) . ?
C54 H54 1.0000 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C60 C62 1.524(3) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.524(3) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.514(3) . ?
C62 H62 1.0000 . ?
C63 N5 1.358(3) . ?
C63 C64 1.373(3) . ?
C64 C65 1.396(3) . ?
C64 H64 0.9500 . ?
C65 N6 1.336(3) . ?
C65 C66 1.512(3) . ?
C66 C68 1.536(3) . ?
C66 C69 1.536(3) . ?
C66 C67 1.540(3) . ?
C67 C72 1.536(3) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 C74 1.535(3) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.538(3) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.523(3) . ?
C70 C75 1.527(3) . ?
C70 H70 1.0000 . ?
C71 C72 1.526(3) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 C73 1.524(3) . ?
C72 H72 1.0000 . ?
C73 C74 1.517(4) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C74 C75 1.531(3) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
B1 N5 1.542(3) . ?
B1 N3 1.556(3) . ?
B1 N1 1.558(3) . ?
B1 H1B1 1.116(19) . ?
N1 N2 1.384(2) . ?
N2 Ca1 2.4578(18) . ?
N3 N4 1.380(2) . ?
N4 Ca1 2.4683(18) . ?
N5 N6 1.381(2) . ?
N6 Ca1 2.4723(18) . ?
Ca1 O1 2.4148(15) . ?

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
C2 C1 Ca1 120.47(15) . . ?
C2 C1 H1A 107.2 . . ?
Ca1 C1 H1A 107.2 . . ?
C2 C1 H1B 107.2 . . ?
Ca1 C1 H1B 107.2 . . ?
H1A C1 H1B 106.8 . . ?
C1 C2 C3 116.77(19) . . ?
C1 C2 H2A 108.1 . . ?
C3 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
C3 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
C2 C3 C4 114.6(2) . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C3 114.1(2) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C10 C5 C6 117.4(2) . . ?
C10 C5 C4 122.5(2) . . ?
C6 C5 C4 120.0(2) . . ?
C7 C6 C5 121.3(2) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 120.2(2) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C5 121.6(2) . . ?
C9 C10 H10 119.2 . . ?
C5 C10 H10 119.2 . . ?
O1 C11 C12 111.51(18) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 109.9(2) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C12 110.1(2) . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.2 . . ?
C15 C14 C13 111.6(2) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
O1 C15 C14 111.7(2) . . ?
O1 C15 H15A 109.3 . . ?
C14 C15 H15A 109.3 . . ?
O1 C15 H15B 109.3 . . ?
C14 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C22 C20 H20A 109.5 . . ?
C22 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C22 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C20 110.80(19) . . ?
C23 C22 C21 109.7(2) . . ?
C20 C22 C21 112.2(2) . . ?
C23 C22 H22 108.0 . . ?
C20 C22 H22 108.0 . . ?
C21 C22 H22 108.0 . . ?
N1 C23 C24 107.71(19) . . ?
N1 C23 C22 124.83(19) . . ?
C24 C23 C22 127.4(2) . . ?
C23 C24 C25 106.3(2) . . ?
C23 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
N2 C25 C24 110.08(19) . . ?
N2 C25 C26 122.25(19) . . ?
C24 C25 C26 127.6(2) . . ?
C27' C26 C25 112.5(7) . . ?
C25 C26 C28 112.91(19) . . ?
C27' C26 C28' 111.7(11) . . ?
C25 C26 C28' 111.0(6) . . ?
C25 C26 C29 109.23(18) . . ?
C28 C26 C29 108.2(2) . . ?
C25 C26 C27 110.29(19) . . ?
C28 C26 C27 108.1(2) . . ?
C29 C26 C27 108.0(2) . . ?
C27' C26 C29' 107.4(11) . . ?
C25 C26 C29' 107.9(6) . . ?
C28' C26 C29' 106.1(10) . . ?
C34 C27 C26 110.9(2) . . ?
C34 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C34 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.0 . . ?
C26 C28 C32 110.8(2) . . ?
C26 C28 H28A 109.5 . . ?
C32 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C32 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C26 111.3(2) . . ?
C30 C29 H29A 109.4 . . ?
C26 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C26 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C31 C30 C35 110.5(2) . . ?
C31 C30 C29 108.8(2) . . ?
C35 C30 C29 107.8(3) . . ?
C31 C30 H30 109.9 . . ?
C35 C30 H30 109.9 . . ?
C29 C30 H30 109.9 . . ?
C30 C31 C32 109.8(3) . . ?
C30 C31 H31A 109.7 . . ?
C32 C31 H31A 109.7 . . ?
C30 C31 H31B 109.7 . . ?
C32 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C31 C32 C33 109.6(3) . . ?
C31 C32 C28 109.4(2) . . ?
C33 C32 C28 108.9(3) . . ?
C31 C32 H32 109.6 . . ?
C33 C32 H32 109.6 . . ?
C28 C32 H32 109.6 . . ?
C34 C33 C32 110.2(3) . . ?
C34 C33 H33A 109.6 . . ?
C32 C33 H33A 109.6 . . ?
C34 C33 H33B 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
C35 C34 C33 109.5(3) . . ?
C35 C34 C27 109.1(2) . . ?
C33 C34 C27 108.7(2) . . ?
C35 C34 H34 109.8 . . ?
C33 C34 H34 109.8 . . ?
C27 C34 H34 109.8 . . ?
C34 C35 C30 110.6(3) . . ?
C34 C35 H35A 109.5 . . ?
C30 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 108.1 . . ?
C26 C27' C35' 110.7(13) . . ?
C26 C27' H27C 109.5 . . ?
C35' C27' H27C 109.5 . . ?
C26 C27' H27D 109.5 . . ?
C35' C27' H27D 109.5 . . ?
H27C C27' H27D 108.1 . . ?
C26 C28' C33' 112.1(13) . . ?
C26 C28' H28C 109.2 . . ?
C33' C28' H28C 109.2 . . ?
C26 C28' H28D 109.2 . . ?
C33' C28' H28D 109.2 . . ?
H28C C28' H28D 107.9 . . ?
C26 C29' C31' 112.0(12) . . ?
C26 C29' H29C 109.2 . . ?
C31' C29' H29C 109.2 . . ?
C26 C29' H29D 109.2 . . ?
C31' C29' H29D 109.2 . . ?
H29C C29' H29D 107.9 . . ?
C35' C30' C31' 113.5(16) . . ?
C35' C30' H30A 108.9 . . ?
C31' C30' H30A 108.9 . . ?
C35' C30' H30B 108.9 . . ?
C31' C30' H30B 108.9 . . ?
H30A C30' H30B 107.7 . . ?
C32' C31' C30' 107.0(17) . . ?
C32' C31' C29' 110.6(16) . . ?
C30' C31' C29' 102.7(15) . . ?
C32' C31' H31' 112.0 . . ?
C30' C31' H31' 112.0 . . ?
C29' C31' H31' 112.0 . . ?
C33' C32' C31' 117.9(17) . . ?
C33' C32' H32A 107.8 . . ?
C31' C32' H32A 107.8 . . ?
C33' C32' H32B 107.8 . . ?
C31' C32' H32B 107.8 . . ?
H32A C32' H32B 107.2 . . ?
C32' C33' C34' 102.4(16) . . ?
C32' C33' C28' 105.8(16) . . ?
C34' C33' C28' 108.5(16) . . ?
C32' C33' H33' 113.1 . . ?
C34' C33' H33' 113.1 . . ?
C28' C33' H33' 113.1 . . ?
C33' C34' C35' 117.8(17) . . ?
C33' C34' H34A 107.9 . . ?
C35' C34' H34A 107.9 . . ?
C33' C34' H34B 107.9 . . ?
C35' C34' H34B 107.9 . . ?
H34A C34' H34B 107.2 . . ?
C30' C35' C34' 108.1(16) . . ?
C30' C35' C27' 112.3(17) . . ?
C34' C35' C27' 101.0(15) . . ?
C30' C35' H35' 111.7 . . ?
C34' C35' H35' 111.7 . . ?
C27' C35' H35' 111.7 . . ?
C42 C40 H40A 109.5 . . ?
C42 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C42 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C41 111.4(2) . . ?
C43 C42 C40 110.1(2) . . ?
C41 C42 C40 110.7(2) . . ?
C43 C42 H42 108.1 . . ?
C41 C42 H42 108.1 . . ?
C40 C42 H42 108.1 . . ?
N3 C43 C44 107.39(19) . . ?
N3 C43 C42 124.6(2) . . ?
C44 C43 C42 127.9(2) . . ?
C43 C44 C45 106.2(2) . . ?
C43 C44 H44 126.9 . . ?
C45 C44 H44 126.9 . . ?
N4 C45 C44 110.01(19) . . ?
N4 C45 C46 122.17(19) . . ?
C44 C45 C46 127.4(2) . . ?
C45 C46 C49 107.80(18) . . ?
C45 C46 C48 113.45(18) . . ?
C49 C46 C48 107.67(18) . . ?
C45 C46 C47 110.78(18) . . ?
C49 C46 C47 108.22(18) . . ?
C48 C46 C47 108.75(18) . . ?
C54 C47 C46 110.66(19) . . ?
C54 C47 H47A 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C54 C47 H47B 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C52 C48 C46 110.67(18) . . ?
C52 C48 H48A 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C52 C48 H48B 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 108.1 . . ?
C50 C49 C46 111.01(19) . . ?
C50 C49 H49A 109.4 . . ?
C46 C49 H49A 109.4 . . ?
C50 C49 H49B 109.4 . . ?
C46 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
C55 C50 C51 109.5(2) . . ?
C55 C50 C49 108.9(2) . . ?
C51 C50 C49 109.68(19) . . ?
C55 C50 H50 109.6 . . ?
C51 C50 H50 109.6 . . ?
C49 C50 H50 109.6 . . ?
C52 C51 C50 109.42(19) . . ?
C52 C51 H51A 109.8 . . ?
C50 C51 H51A 109.8 . . ?
C52 C51 H51B 109.8 . . ?
C50 C51 H51B 109.8 . . ?
H51A C51 H51B 108.2 . . ?
C51 C52 C53 109.59(19) . . ?
C51 C52 C48 108.81(19) . . ?
C53 C52 C48 109.84(19) . . ?
C51 C52 H52 109.5 . . ?
C53 C52 H52 109.5 . . ?
C48 C52 H52 109.5 . . ?
C52 C53 C54 109.37(19) . . ?
C52 C53 H53A 109.8 . . ?
C54 C53 H53A 109.8 . . ?
C52 C53 H53B 109.8 . . ?
C54 C53 H53B 109.8 . . ?
H53A C53 H53B 108.2 . . ?
C55 C54 C47 110.0(2) . . ?
C55 C54 C53 109.7(2) . . ?
C47 C54 C53 108.81(19) . . ?
C55 C54 H54 109.4 . . ?
C47 C54 H54 109.4 . . ?
C53 C54 H54 109.4 . . ?
C54 C55 C50 109.70(19) . . ?
C54 C55 H55A 109.7 . . ?
C50 C55 H55A 109.7 . . ?
C54 C55 H55B 109.7 . . ?
C50 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C62 C60 H60A 109.5 . . ?
C62 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C62 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C62 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C61 109.88(19) . . ?
C63 C62 C60 111.41(19) . . ?
C61 C62 C60 111.3(2) . . ?
C63 C62 H62 108.0 . . ?
C61 C62 H62 108.0 . . ?
C60 C62 H62 108.0 . . ?
N5 C63 C64 107.50(19) . . ?
N5 C63 C62 124.5(2) . . ?
C64 C63 C62 128.0(2) . . ?
C63 C64 C65 106.39(19) . . ?
C63 C64 H64 126.8 . . ?
C65 C64 H64 126.8 . . ?
N6 C65 C64 109.97(19) . . ?
N6 C65 C66 122.29(19) . . ?
C64 C65 C66 127.57(19) . . ?
C65 C66 C68 110.78(18) . . ?
C65 C66 C69 109.07(18) . . ?
C68 C66 C69 108.24(18) . . ?
C65 C66 C67 112.20(18) . . ?
C68 C66 C67 108.12(18) . . ?
C69 C66 C67 108.32(19) . . ?
C72 C67 C66 109.85(19) . . ?
C72 C67 H67A 109.7 . . ?
C66 C67 H67A 109.7 . . ?
C72 C67 H67B 109.7 . . ?
C66 C67 H67B 109.7 . . ?
H67A C67 H67B 108.2 . . ?
C74 C68 C66 110.75(19) . . ?
C74 C68 H68A 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C74 C68 H68B 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 108.1 . . ?
C66 C69 C70 111.43(19) . . ?
C66 C69 H69A 109.3 . . ?
C70 C69 H69A 109.3 . . ?
C66 C69 H69B 109.3 . . ?
C70 C69 H69B 109.3 . . ?
H69A C69 H69B 108.0 . . ?
C71 C70 C75 110.5(2) . . ?
C71 C70 C69 108.3(2) . . ?
C75 C70 C69 109.0(2) . . ?
C71 C70 H70 109.7 . . ?
C75 C70 H70 109.7 . . ?
C69 C70 H70 109.7 . . ?
C70 C71 C72 109.8(2) . . ?
C70 C71 H71A 109.7 . . ?
C72 C71 H71A 109.7 . . ?
C70 C71 H71B 109.7 . . ?
C72 C71 H71B 109.7 . . ?
H71A C71 H71B 108.2 . . ?
C73 C72 C71 109.2(2) . . ?
C73 C72 C67 109.51(19) . . ?
C71 C72 C67 109.8(2) . . ?
C73 C72 H72 109.4 . . ?
C71 C72 H72 109.4 . . ?
C67 C72 H72 109.4 . . ?
C74 C73 C72 110.0(2) . . ?
C74 C73 H73A 109.7 . . ?
C72 C73 H73A 109.7 . . ?
C74 C73 H73B 109.7 . . ?
C72 C73 H73B 109.7 . . ?
H73A C73 H73B 108.2 . . ?
C73 C74 C75 110.2(2) . . ?
C73 C74 C68 108.5(2) . . ?
C75 C74 C68 109.9(2) . . ?
C73 C74 H74 109.4 . . ?
C75 C74 H74 109.4 . . ?
C68 C74 H74 109.4 . . ?
C70 C75 C74 108.87(19) . . ?
C70 C75 H75A 109.9 . . ?
C74 C75 H75A 109.9 . . ?
C70 C75 H75B 109.9 . . ?
C74 C75 H75B 109.9 . . ?
H75A C75 H75B 108.3 . . ?
N5 B1 N3 109.84(18) . . ?
N5 B1 N1 112.42(19) . . ?
N3 B1 N1 112.60(18) . . ?
N5 B1 H1B1 106.5(10) . . ?
N3 B1 H1B1 108.5(10) . . ?
N1 B1 H1B1 106.6(10) . . ?
C23 N1 N2 109.76(17) . . ?
C23 N1 B1 126.59(18) . . ?
N2 N1 B1 123.48(17) . . ?
C25 N2 N1 106.10(17) . . ?
C25 N2 Ca1 137.23(14) . . ?
N1 N2 Ca1 109.94(12) . . ?
C43 N3 N4 109.76(17) . . ?
C43 N3 B1 128.56(18) . . ?
N4 N3 B1 120.53(17) . . ?
C45 N4 N3 106.59(17) . . ?
C45 N4 Ca1 138.68(14) . . ?
N3 N4 Ca1 113.34(12) . . ?
C63 N5 N6 109.76(17) . . ?
C63 N5 B1 126.37(18) . . ?
N6 N5 B1 122.55(17) . . ?
C65 N6 N5 106.36(17) . . ?
C65 N6 Ca1 139.82(14) . . ?
N5 N6 Ca1 113.62(12) . . ?
O1 Ca1 N2 83.71(6) . . ?
O1 Ca1 N4 80.53(6) . . ?
N2 Ca1 N4 92.91(6) . . ?
O1 Ca1 N6 147.30(6) . . ?
N2 Ca1 N6 78.89(6) . . ?
N4 Ca1 N6 73.01(6) . . ?
O1 Ca1 C1 92.00(6) . . ?
N2 Ca1 C1 123.69(7) . . ?
N4 Ca1 C1 141.78(7) . . ?
N6 Ca1 C1 120.69(7) . . ?
C15 O1 C11 111.05(16) . . ?
C15 O1 Ca1 129.36(13) . . ?
C11 O1 Ca1 118.96(12) . . ?

_refine_diff_density_max         0.389
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.053

