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

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

data_hasj160613a
_database_code_depnum_ccdc_archive 'CCDC 1520541'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT305_hasj160613a         
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??)            H Check
RESPONSE: This is a calcium hydride - distances too long to be recognized as bonding
;
# Added during the CSD deposition process: Friday 02 December 2016 04:36 PM
# end Validation Reply Form

_audit_creation_date             2016-08-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H48 Ca N3'
_chemical_formula_sum            'C32 H48 Ca N3'
_chemical_formula_weight         514.81
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca O Si'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.88056(13)
_cell_length_b                   15.1230(2)
_cell_length_c                   22.2473(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.5639(13)
_cell_angle_gamma                90
_cell_volume                     2968.24(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5758
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.5860
_cell_measurement_theta_min      4.9240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.4586
_exptl_crystal_size_mid          0.0636
_exptl_crystal_size_min          0.0489
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10589
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.695
_diffrn_reflns_theta_min         3.541
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -66.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
  2 omega -110.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000    0.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega   82.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  -60.0000 69

#__ type_ start__ end____ width___ exp.time_
  4 omega   95.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
  5 omega   41.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -180.0000 49

#__ type_ start__ end____ width___ exp.time_
  6 omega   40.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000    0.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00  128.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   90.0000 92

#__ type_ start__ end____ width___ exp.time_
  8 omega   33.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   60.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0757412000
_diffrn_orient_matrix_UB_12      0.0598427000
_diffrn_orient_matrix_UB_13      0.0507385000
_diffrn_orient_matrix_UB_21      -0.0893430000
_diffrn_orient_matrix_UB_22      0.0799659000
_diffrn_orient_matrix_UB_23      -0.0283787000
_diffrn_orient_matrix_UB_31      -0.1295763000
_diffrn_orient_matrix_UB_32      -0.0200266000
_diffrn_orient_matrix_UB_33      0.0384334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5198
_reflns_number_total             5747
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+0.8280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0925
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C32, C31, N3, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: N3(0.5) C31(0.5) H31A(0.5) H31B(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 N4(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C27(H27), C24(H24), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C35(H35A,H35B), C33(H33A,H33B), C34(H34A,H34B), C30(H30A,
 H30B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C22(H22), C20(H20), C10(H10), C9(H9), C21(H21)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.61232(3) 0.41815(2) 0.53939(2) 0.01126(8) Uani 1 1 d . . . . .
N2 N 0.59037(13) 0.26118(7) 0.53076(5) 0.0127(2) Uani 1 1 d . . . . .
N1 N 0.63441(12) 0.38870(7) 0.64572(5) 0.0123(2) Uani 1 1 d . . . . .
N3 N 0.8646(16) 0.4577(7) 0.5025(5) 0.0158(14) Uani 0.5 1 d . U P . .
C2 C 0.73187(14) 0.32349(8) 0.66069(6) 0.0115(2) Uani 1 1 d . . . . .
C4 C 0.69436(14) 0.21931(9) 0.56762(6) 0.0123(2) Uani 1 1 d . . . . .
C3 C 0.77146(15) 0.25540(9) 0.62168(6) 0.0126(2) Uani 1 1 d . . . . .
C7 C 0.67647(15) 0.50986(9) 0.72220(6) 0.0149(3) Uani 1 1 d . . . . .
C6 C 0.58652(15) 0.44120(9) 0.69405(6) 0.0131(3) Uani 1 1 d . . . . .
C23 C 0.54260(16) 0.21676(9) 0.42347(6) 0.0161(3) Uani 1 1 d . . . . .
C18 C 0.50458(15) 0.21194(9) 0.48330(6) 0.0139(3) Uani 1 1 d . . . . .
C1 C 0.80647(15) 0.31557(9) 0.72539(6) 0.0145(3) Uani 1 1 d . . . . .
H1A H 0.8678 0.3669 0.7355 0.022 Uiso 1 1 calc GR . . . .
H1B H 0.8690 0.2637 0.7292 0.022 Uiso 1 1 calc GR . . . .
H1C H 0.7297 0.3112 0.7523 0.022 Uiso 1 1 calc GR . . . .
C12 C 0.82813(16) 0.53693(9) 0.70250(6) 0.0172(3) Uani 1 1 d . . . . .
H12 H 0.8588 0.4914 0.6750 0.021 Uiso 1 1 calc R . . . .
C5 C 0.73581(16) 0.12383(9) 0.55618(6) 0.0177(3) Uani 1 1 d . . . . .
H5A H 0.7141 0.1109 0.5138 0.026 Uiso 1 1 calc GR . . . .
H5B H 0.6776 0.0853 0.5789 0.026 Uiso 1 1 calc GR . . . .
H5C H 0.8419 0.1150 0.5686 0.026 Uiso 1 1 calc GR . . . .
C8 C 0.62314(17) 0.55766(9) 0.76939(6) 0.0178(3) Uani 1 1 d . . . . .
H8 H 0.6827 0.6026 0.7881 0.021 Uiso 1 1 calc R . . . .
C22 C 0.45384(18) 0.17070(10) 0.37806(6) 0.0206(3) Uani 1 1 d . . . . .
H22 H 0.4797 0.1726 0.3387 0.025 Uiso 1 1 calc R . . . .
C11 C 0.44291(16) 0.42373(9) 0.71303(6) 0.0152(3) Uani 1 1 d . . . . .
C19 C 0.37818(16) 0.16180(9) 0.49593(6) 0.0164(3) Uani 1 1 d . . . . .
C27 C 0.68161(16) 0.26615(10) 0.40756(6) 0.0189(3) Uani 1 1 d . . . . .
H27 H 0.7149 0.3053 0.4416 0.023 Uiso 1 1 calc R . . . .
C24 C 0.33057(17) 0.15462(10) 0.55933(7) 0.0206(3) Uani 1 1 d . . . . .
H24 H 0.4065 0.1853 0.5873 0.025 Uiso 1 1 calc R . . . .
C20 C 0.29139(17) 0.11823(10) 0.44856(7) 0.0204(3) Uani 1 1 d . . . . .
H20 H 0.2070 0.0859 0.4566 0.024 Uiso 1 1 calc R . . . .
C10 C 0.39457(16) 0.47316(10) 0.76026(6) 0.0190(3) Uani 1 1 d . . . . .
H10 H 0.3004 0.4613 0.7729 0.023 Uiso 1 1 calc R . . . .
C15 C 0.34380(15) 0.34971(10) 0.68439(6) 0.0177(3) Uani 1 1 d . . . . .
H15 H 0.3580 0.3470 0.6414 0.021 Uiso 1 1 calc R . . . .
C9 C 0.48406(17) 0.53950(10) 0.78873(7) 0.0206(3) Uani 1 1 d . . . . .
H9 H 0.4508 0.5714 0.8204 0.025 Uiso 1 1 calc R . . . .
C21 C 0.32849(18) 0.12227(10) 0.38986(7) 0.0223(3) Uani 1 1 d . . . . .
H21 H 0.2699 0.0928 0.3588 0.027 Uiso 1 1 calc R . . . .
C13 C 0.81096(19) 0.62464(10) 0.66760(7) 0.0239(3) Uani 1 1 d . . . . .
H13A H 0.7350 0.6183 0.6335 0.036 Uiso 1 1 calc GR . . . .
H13B H 0.9059 0.6401 0.6537 0.036 Uiso 1 1 calc GR . . . .
H13C H 0.7813 0.6703 0.6938 0.036 Uiso 1 1 calc GR . . . .
C28 C 0.64866(18) 0.32404(10) 0.35125(7) 0.0231(3) Uani 1 1 d . . . . .
H28A H 0.6184 0.2873 0.3168 0.035 Uiso 1 1 calc GR . . . .
H28B H 0.7383 0.3564 0.3446 0.035 Uiso 1 1 calc GR . . . .
H28C H 0.5686 0.3647 0.3570 0.035 Uiso 1 1 calc GR . . . .
C14 C 0.95350(17) 0.54525(10) 0.75564(7) 0.0218(3) Uani 1 1 d . . . . .
H14A H 0.9285 0.5919 0.7820 0.033 Uiso 1 1 calc GR . . . .
H14B H 1.0480 0.5585 0.7405 0.033 Uiso 1 1 calc GR . . . .
H14C H 0.9625 0.4906 0.7776 0.033 Uiso 1 1 calc GR . . . .
C17 C 0.39173(19) 0.26059(11) 0.71295(7) 0.0255(3) Uani 1 1 d . . . . .
H17A H 0.4924 0.2465 0.7043 0.038 Uiso 1 1 calc GR . . . .
H17B H 0.3229 0.2155 0.6965 0.038 Uiso 1 1 calc GR . . . .
H17C H 0.3900 0.2638 0.7560 0.038 Uiso 1 1 calc GR . . . .
C25 C 0.17842(19) 0.20042(13) 0.56192(8) 0.0313(4) Uani 1 1 d . . . . .
H25A H 0.1874 0.2618 0.5520 0.047 Uiso 1 1 calc GR . . . .
H25B H 0.1491 0.1952 0.6020 0.047 Uiso 1 1 calc GR . . . .
H25C H 0.1031 0.1731 0.5335 0.047 Uiso 1 1 calc GR . . . .
C26 C 0.3226(2) 0.05833(12) 0.58018(7) 0.0291(3) Uani 1 1 d . . . . .
H26A H 0.2391 0.0292 0.5570 0.044 Uiso 1 1 calc GR . . . .
H26B H 0.3084 0.0569 0.6223 0.044 Uiso 1 1 calc GR . . . .
H26C H 0.4153 0.0286 0.5743 0.044 Uiso 1 1 calc GR . . . .
C29 C 0.81213(19) 0.20257(13) 0.40006(8) 0.0315(4) Uani 1 1 d . . . . .
H29A H 0.8382 0.1707 0.4371 0.047 Uiso 1 1 calc GR . . . .
H29B H 0.8985 0.2355 0.3904 0.047 Uiso 1 1 calc GR . . . .
H29C H 0.7816 0.1616 0.3680 0.047 Uiso 1 1 calc GR . . . .
C16 C 0.17572(18) 0.36478(14) 0.68894(10) 0.0404(5) Uani 1 1 d . . . . .
H16A H 0.1571 0.3611 0.7305 0.061 Uiso 1 1 calc GR . . . .
H16B H 0.1173 0.3205 0.6658 0.061 Uiso 1 1 calc GR . . . .
H16C H 0.1470 0.4223 0.6733 0.061 Uiso 1 1 calc GR . . . .
C31 C 0.8495(3) 0.5129(2) 0.44894(13) 0.0183(5) Uani 0.5 1 d . U P A -1
H31A H 0.7896 0.5648 0.4558 0.022 Uiso 0.5 1 calc R . P A -1
H31B H 0.7977 0.4803 0.4151 0.022 Uiso 0.5 1 calc R . P A -1
C35 C 1.0663(3) 0.5656(2) 0.53987(14) 0.0239(7) Uani 0.5 1 d . . P A -1
H35A H 1.0397 0.6272 0.5325 0.029 Uiso 0.5 1 calc R . P A -1
H35B H 1.1449 0.5629 0.5739 0.029 Uiso 0.5 1 calc R . P A -1
N4 N 1.1235(15) 0.5272(7) 0.4853(4) 0.0152(16) Uani 0.5 1 d . . P A -1
C33 C 1.1389(3) 0.4295(2) 0.49731(14) 0.0205(6) Uani 0.5 1 d . . P A -1
H33A H 1.1963 0.4196 0.5365 0.025 Uiso 0.5 1 calc R . P A -1
H33B H 1.1930 0.4020 0.4667 0.025 Uiso 0.5 1 calc R . P A -1
C34 C 1.0082(3) 0.5415(2) 0.43385(13) 0.0207(6) Uani 0.5 1 d . . P A -1
H34A H 1.0344 0.5080 0.3994 0.025 Uiso 0.5 1 calc R . P A -1
H34B H 1.0059 0.6037 0.4230 0.025 Uiso 0.5 1 calc R . P A -1
C30 C 0.9793(3) 0.3874(2) 0.49614(17) 0.0263(7) Uani 0.5 1 d . U P A -1
H30A H 0.9538 0.3561 0.4583 0.032 Uiso 0.5 1 calc R . P A -1
H30B H 0.9792 0.3452 0.5290 0.032 Uiso 0.5 1 calc R . P A -1
C32 C 0.9250(4) 0.5134(3) 0.55489(14) 0.0257(7) Uani 0.5 1 d . U P A -1
H32A H 0.9523 0.4761 0.5899 0.031 Uiso 0.5 1 calc R . P A -1
H32B H 0.8474 0.5544 0.5646 0.031 Uiso 0.5 1 calc R . P A -1
H3 H 0.850(2) 0.2188(13) 0.6394(8) 0.019(4) Uiso 1 1 d . . . . .
H H 0.522(3) 0.5479(19) 0.5473(12) 0.058(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
Ca1 N2 2.3879(11) . ?
Ca1 N1 2.3931(11) . ?
Ca1 N3 2.543(14) . ?
Ca1 H 2.13(3) . ?
N2 C4 1.3240(17) . ?
N2 C18 1.4373(17) . ?
N1 C2 1.3292(17) . ?
N1 C6 1.4395(17) . ?
N3 C31 1.449(13) . ?
N3 C30 1.491(13) . ?
N3 C32 1.486(8) . ?
C2 C3 1.4166(18) . ?
C2 C1 1.5189(17) . ?
C4 C3 1.4229(18) . ?
C4 C5 1.5188(18) . ?
C3 H3 0.94(2) . ?
C7 C6 1.4121(19) . ?
C7 C12 1.5193(19) . ?
C7 C8 1.4008(19) . ?
C6 C11 1.413(2) . ?
C23 C18 1.4120(19) . ?
C23 C22 1.3947(19) . ?
C23 C27 1.5189(19) . ?
C18 C19 1.409(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C12 H12 0.9800 . ?
C12 C13 1.536(2) . ?
C12 C14 1.534(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C8 H8 0.9300 . ?
C8 C9 1.381(2) . ?
C22 H22 0.9300 . ?
C22 C21 1.382(2) . ?
C11 C10 1.397(2) . ?
C11 C15 1.5184(19) . ?
C19 C24 1.5218(19) . ?
C19 C20 1.398(2) . ?
C27 H27 0.9800 . ?
C27 C28 1.529(2) . ?
C27 C29 1.530(2) . ?
C24 H24 0.9800 . ?
C24 C25 1.525(2) . ?
C24 C26 1.532(2) . ?
C20 H20 0.9300 . ?
C20 C21 1.384(2) . ?
C10 H10 0.9300 . ?
C10 C9 1.387(2) . ?
C15 H15 0.9800 . ?
C15 C17 1.530(2) . ?
C15 C16 1.525(2) . ?
C9 H9 0.9300 . ?
C21 H21 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C34 1.547(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 N4 1.487(10) . ?
C35 C32 1.551(4) . ?
N4 C33 1.504(12) . ?
N4 C34 1.463(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C30 1.551(4) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ca1 N1 83.75(4) . . ?
N2 Ca1 N3 106.0(2) . . ?
N2 Ca1 H 153.2(8) . . ?
N1 Ca1 N3 112.7(2) . . ?
N1 Ca1 H 94.5(7) . . ?
N3 Ca1 H 99.4(8) . . ?
C4 N2 Ca1 112.39(8) . . ?
C4 N2 C18 118.74(11) . . ?
C18 N2 Ca1 127.27(8) . . ?
C2 N1 Ca1 111.30(8) . . ?
C2 N1 C6 117.49(10) . . ?
C6 N1 Ca1 129.64(8) . . ?
C31 N3 Ca1 113.5(7) . . ?
C31 N3 C30 109.4(8) . . ?
C31 N3 C32 108.1(7) . . ?
C30 N3 Ca1 120.0(7) . . ?
C32 N3 Ca1 97.6(6) . . ?
C32 N3 C30 106.8(8) . . ?
N1 C2 C3 125.86(12) . . ?
N1 C2 C1 119.79(11) . . ?
C3 C2 C1 114.29(11) . . ?
N2 C4 C3 125.04(12) . . ?
N2 C4 C5 121.07(12) . . ?
C3 C4 C5 113.82(11) . . ?
C2 C3 C4 131.87(12) . . ?
C2 C3 H3 113.2(11) . . ?
C4 C3 H3 113.1(11) . . ?
C6 C7 C12 123.04(12) . . ?
C8 C7 C6 119.29(13) . . ?
C8 C7 C12 117.64(12) . . ?
C7 C6 N1 122.44(12) . . ?
C7 C6 C11 119.27(12) . . ?
C11 C6 N1 118.28(12) . . ?
C18 C23 C27 122.23(12) . . ?
C22 C23 C18 118.73(13) . . ?
C22 C23 C27 118.94(12) . . ?
C23 C18 N2 120.13(12) . . ?
C19 C18 N2 119.97(12) . . ?
C19 C18 C23 119.83(12) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C12 H12 108.0 . . ?
C7 C12 C13 109.79(12) . . ?
C7 C12 C14 112.90(12) . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C14 C12 C13 109.89(12) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.46(13) . . ?
C9 C8 H8 119.3 . . ?
C23 C22 H22 119.1 . . ?
C21 C22 C23 121.86(13) . . ?
C21 C22 H22 119.1 . . ?
C6 C11 C15 120.80(12) . . ?
C10 C11 C6 119.35(13) . . ?
C10 C11 C15 119.80(13) . . ?
C18 C19 C24 122.36(12) . . ?
C20 C19 C18 119.11(13) . . ?
C20 C19 C24 118.52(13) . . ?
C23 C27 H27 107.4 . . ?
C23 C27 C28 112.83(12) . . ?
C23 C27 C29 111.25(13) . . ?
C28 C27 H27 107.4 . . ?
C28 C27 C29 110.30(12) . . ?
C29 C27 H27 107.4 . . ?
C19 C24 H24 108.0 . . ?
C19 C24 C25 110.11(13) . . ?
C19 C24 C26 112.07(12) . . ?
C25 C24 H24 108.0 . . ?
C25 C24 C26 110.39(13) . . ?
C26 C24 H24 108.0 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.36(14) . . ?
C21 C20 H20 119.3 . . ?
C11 C10 H10 119.3 . . ?
C9 C10 C11 121.42(13) . . ?
C9 C10 H10 119.3 . . ?
C11 C15 H15 107.9 . . ?
C11 C15 C17 110.78(12) . . ?
C11 C15 C16 112.76(12) . . ?
C17 C15 H15 107.9 . . ?
C16 C15 H15 107.9 . . ?
C16 C15 C17 109.40(14) . . ?
C8 C9 C10 119.18(13) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C22 C21 C20 119.09(13) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C31 H31A 109.7 . . ?
N3 C31 H31B 109.7 . . ?
N3 C31 C34 109.8(6) . . ?
H31A C31 H31B 108.2 . . ?
C34 C31 H31A 109.7 . . ?
C34 C31 H31B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
N4 C35 H35A 109.7 . . ?
N4 C35 H35B 109.7 . . ?
N4 C35 C32 109.7(5) . . ?
C32 C35 H35A 109.7 . . ?
C32 C35 H35B 109.7 . . ?
C35 N4 C33 105.8(8) . . ?
C34 N4 C35 107.9(8) . . ?
C34 N4 C33 109.0(6) . . ?
N4 C33 H33A 109.7 . . ?
N4 C33 H33B 109.7 . . ?
N4 C33 C30 109.6(5) . . ?
H33A C33 H33B 108.2 . . ?
C30 C33 H33A 109.7 . . ?
C30 C33 H33B 109.7 . . ?
C31 C34 H34A 109.4 . . ?
C31 C34 H34B 109.4 . . ?
N4 C34 C31 111.2(6) . . ?
N4 C34 H34A 109.4 . . ?
N4 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
N3 C30 C33 109.8(5) . . ?
N3 C30 H30A 109.7 . . ?
N3 C30 H30B 109.7 . . ?
C33 C30 H30A 109.7 . . ?
C33 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
N3 C32 C35 110.4(6) . . ?
N3 C32 H32A 109.6 . . ?
N3 C32 H32B 109.6 . . ?
C35 C32 H32A 109.6 . . ?
C35 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 N2 C4 C3 23.37(16) . . . . ?
Ca1 N2 C4 C5 -159.74(10) . . . . ?
Ca1 N2 C18 C23 63.63(16) . . . . ?
Ca1 N2 C18 C19 -113.59(12) . . . . ?
Ca1 N1 C2 C3 -24.86(16) . . . . ?
Ca1 N1 C2 C1 157.79(9) . . . . ?
Ca1 N1 C6 C7 -84.49(15) . . . . ?
Ca1 N1 C6 C11 94.48(13) . . . . ?
Ca1 N3 C31 C34 174.1(3) . . . . ?
Ca1 N3 C30 C33 -158.6(4) . . . . ?
Ca1 N3 C32 C35 -167.4(3) . . . . ?
N2 C4 C3 C2 24.3(2) . . . . ?
N2 C18 C19 C24 -2.2(2) . . . . ?
N2 C18 C19 C20 176.59(12) . . . . ?
N1 C2 C3 C4 -23.2(2) . . . . ?
N1 C6 C11 C10 179.34(12) . . . . ?
N1 C6 C11 C15 1.76(19) . . . . ?
N3 C31 C34 N4 -15.9(4) . . . . ?
C2 N1 C6 C7 79.83(16) . . . . ?
C2 N1 C6 C11 -101.20(14) . . . . ?
C4 N2 C18 C23 -100.80(15) . . . . ?
C4 N2 C18 C19 81.98(16) . . . . ?
C7 C6 C11 C10 -1.65(19) . . . . ?
C7 C6 C11 C15 -179.23(12) . . . . ?
C7 C8 C9 C10 -0.8(2) . . . . ?
C6 N1 C2 C3 168.05(12) . . . . ?
C6 N1 C2 C1 -9.30(17) . . . . ?
C6 C7 C12 C13 105.28(15) . . . . ?
C6 C7 C12 C14 -131.74(14) . . . . ?
C6 C7 C8 C9 -0.4(2) . . . . ?
C6 C11 C10 C9 0.4(2) . . . . ?
C6 C11 C15 C17 82.08(16) . . . . ?
C6 C11 C15 C16 -154.93(15) . . . . ?
C23 C18 C19 C24 -179.48(13) . . . . ?
C23 C18 C19 C20 -0.6(2) . . . . ?
C23 C22 C21 C20 -1.0(2) . . . . ?
C18 N2 C4 C3 -169.99(12) . . . . ?
C18 N2 C4 C5 6.90(18) . . . . ?
C18 C23 C22 C21 1.4(2) . . . . ?
C18 C23 C27 C28 -134.97(14) . . . . ?
C18 C23 C27 C29 100.44(16) . . . . ?
C18 C19 C24 C25 112.87(15) . . . . ?
C18 C19 C24 C26 -123.84(15) . . . . ?
C18 C19 C20 C21 1.0(2) . . . . ?
C1 C2 C3 C4 154.33(14) . . . . ?
C12 C7 C6 N1 2.6(2) . . . . ?
C12 C7 C6 C11 -176.41(12) . . . . ?
C12 C7 C8 C9 177.73(13) . . . . ?
C5 C4 C3 C2 -152.82(14) . . . . ?
C8 C7 C6 N1 -179.39(12) . . . . ?
C8 C7 C6 C11 1.65(19) . . . . ?
C8 C7 C12 C13 -72.81(16) . . . . ?
C8 C7 C12 C14 50.17(17) . . . . ?
C22 C23 C18 N2 -177.75(13) . . . . ?
C22 C23 C18 C19 -0.5(2) . . . . ?
C22 C23 C27 C28 48.48(18) . . . . ?
C22 C23 C27 C29 -76.10(17) . . . . ?
C11 C10 C9 C8 0.8(2) . . . . ?
C19 C20 C21 C22 -0.2(2) . . . . ?
C27 C23 C18 N2 5.7(2) . . . . ?
C27 C23 C18 C19 -177.07(13) . . . . ?
C27 C23 C22 C21 178.05(14) . . . . ?
C24 C19 C20 C21 179.90(14) . . . . ?
C20 C19 C24 C25 -65.97(17) . . . . ?
C20 C19 C24 C26 57.32(18) . . . . ?
C10 C11 C15 C17 -95.49(15) . . . . ?
C10 C11 C15 C16 27.5(2) . . . . ?
C15 C11 C10 C9 178.05(13) . . . . ?
C31 N3 C30 C33 67.7(7) . . . . ?
C31 N3 C32 C35 -49.6(9) . . . . ?
C35 N4 C33 C30 69.7(7) . . . . ?
C35 N4 C34 C31 -48.9(8) . . . . ?
N4 C35 C32 N3 -15.2(4) . . . . ?
N4 C33 C30 N3 -17.3(4) . . . . ?
C33 N4 C34 C31 65.5(8) . . . . ?
C34 N4 C33 C30 -46.0(8) . . . . ?
C30 N3 C31 C34 -49.0(7) . . . . ?
C30 N3 C32 C35 68.0(8) . . . . ?
C32 N3 C31 C34 67.0(9) . . . . ?
C32 N3 C30 C33 -49.0(9) . . . . ?
C32 C35 N4 C33 -50.9(8) . . . . ?
C32 C35 N4 C34 65.6(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 9 -6 0.0272 0.0016 8.9913 -5.9912 0.2342 0.8889 -0.4105
0 -9 6 0.0344 -0.0016 -8.9913 5.9912 -0.2342 -0.8889 0.4105
-5 2 7 0.1950 -4.9955 1.9998 6.9943 0.0962 0.4077 0.8761
5 -2 -7 0.2082 4.9955 -1.9998 -6.9943 -0.0962 -0.4077 -0.8761
0 -4 13 0.0219 -0.0021 -3.9972 12.9891 0.4197 -0.6881 0.5795
-6 0 2 0.2206 -5.9939 0.0029 1.9963 -0.3525 0.4791 0.8533
0 4 -13 0.0272 0.0021 3.9972 -12.9891 -0.4197 0.6881 -0.5795
6 0 -1 0.2370 5.9938 -0.0030 -0.9970 0.4032 -0.5074 -0.8149
0 -2 -14 0.0264 0.0017 -1.9965 -13.9915 -0.8293 0.2373 -0.4980
0 2 14 0.0225 -0.0017 1.9965 13.9915 0.8293 -0.2373 0.4980
0 -9 -6 0.0266 -0.0000 -8.9901 -6.0006 -0.8425 -0.5486 -0.0506
0 9 6 0.0266 0.0000 8.9901 6.0006 0.8425 0.5486 0.0506
3 -4 -10 0.1260 2.9978 -3.9964 -9.9941 -0.5192 -0.3038 -0.6925
2 -9 2 0.0951 1.9968 -8.9919 1.9947 -0.2857 -0.9541 -0.0020
3 -9 2 0.0934 2.9957 -8.9924 1.9951 -0.2100 -1.0434 -0.1314

_olex2_date_sample_data_collection 2016-06-13
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hasj160715a
_database_code_depnum_ccdc_archive 'CCDC 1520545'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_audit_creation_date             2016-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H92 Ca2 N4 O2, C6 H6'
_chemical_formula_sum            'C68 H98 Ca2 N4 O2'
_chemical_formula_weight         1083.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.3510(5)
_cell_length_b                   16.3688(6)
_cell_length_c                   15.0996(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.888(3)
_cell_angle_gamma                90
_cell_volume                     3240.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5165
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      4.2810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.7101
_exptl_crystal_size_mid          0.2148
_exptl_crystal_size_min          0.168
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11176
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         4.321
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00  31.00   1.00    1.00    --  -41.69  38.00   0.00   93
  2  ω    -74.00  21.00   1.00    1.00    --  -41.69  19.00 -90.00   95
  3  ω    113.00 149.00   1.00    1.50    --  106.00  61.00-180.00   36
  4  ω    130.00 174.00   1.00    1.50    --  106.00  61.00-120.00   44
  5  ω     99.00 165.00   1.00    1.50    --  106.00 125.00   0.00   66
  6  ω     89.00 173.00   1.00    1.50    --  106.00  45.00 -90.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113151000
_diffrn_orient_matrix_UB_12      -0.0623625000
_diffrn_orient_matrix_UB_13      -0.0740635000
_diffrn_orient_matrix_UB_21      0.0924633000
_diffrn_orient_matrix_UB_22      -0.0381170000
_diffrn_orient_matrix_UB_23      0.0628447000
_diffrn_orient_matrix_UB_31      -0.0716509000
_diffrn_orient_matrix_UB_32      -0.0589106000
_diffrn_orient_matrix_UB_33      0.0371194000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5429
_reflns_number_total             5890
_reflns_odcompleteness_completeness 78.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5890
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0399
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²+0.9470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C24(H24), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C9(H9), C22(H22), C20(H20), C21(H21), C33(H33), C32(H32),
 C34(H34)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.48559(2) 0.43159(2) 0.58018(2) 0.02295(11) Uani 1 1 d . . . . .
O1 O 0.53844(9) 0.55834(7) 0.56999(8) 0.0298(3) Uani 1 1 d . . . . .
N2 N 0.58955(9) 0.33640(7) 0.66731(7) 0.0176(2) Uani 1 1 d . . . . .
N1 N 0.36779(9) 0.38384(7) 0.66534(7) 0.0169(2) Uani 1 1 d . . . . .
C3 C 0.55436(10) 0.26687(8) 0.69456(9) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.45158(11) 0.25293(9) 0.70059(9) 0.0195(3) Uani 1 1 d . . . . .
C1 C 0.36901(10) 0.30778(9) 0.69577(9) 0.0183(3) Uani 1 1 d . . . . .
C6 C 0.28229(11) 0.43461(8) 0.67250(9) 0.0178(3) Uani 1 1 d . . . . .
C11 C 0.29325(11) 0.49319(9) 0.74245(9) 0.0197(3) Uani 1 1 d . . . . .
C7 C 0.19062(11) 0.42973(8) 0.60879(10) 0.0205(3) Uani 1 1 d . . . . .
C18 C 0.69726(11) 0.35134(9) 0.68540(10) 0.0213(3) Uani 1 1 d . . . . .
C15 C 0.39423(11) 0.50246(9) 0.80828(9) 0.0229(3) Uani 1 1 d . . . . .
H15 H 0.4498 0.4885 0.7748 0.027 Uiso 1 1 calc R . . . .
C10 C 0.20949(12) 0.54119(9) 0.75085(10) 0.0243(3) Uani 1 1 d . . . . .
H10 H 0.2154 0.5796 0.7987 0.029 Uiso 1 1 calc R . . . .
C8 C 0.10931(11) 0.47964(9) 0.61966(10) 0.0251(3) Uani 1 1 d . . . . .
H8 H 0.0469 0.4763 0.5774 0.030 Uiso 1 1 calc R . . . .
C5 C 0.62766(11) 0.19678(9) 0.72379(10) 0.0247(3) Uani 1 1 d . . . . .
H5A H 0.6599 0.1805 0.6734 0.037 Uiso 1 1 calc GR . . . .
H5B H 0.5901 0.1503 0.7423 0.037 Uiso 1 1 calc GR . . . .
H5C H 0.6802 0.2143 0.7746 0.037 Uiso 1 1 calc GR . . . .
C9 C 0.11778(12) 0.53408(10) 0.69091(11) 0.0267(3) Uani 1 1 d . . . . .
H9 H 0.0609 0.5664 0.6986 0.032 Uiso 1 1 calc R . . . .
C4 C 0.27715(12) 0.27445(9) 0.73036(11) 0.0265(3) Uani 1 1 d . . . . .
H4A H 0.2535 0.3152 0.7693 0.040 Uiso 1 1 calc GR . . . .
H4B H 0.2965 0.2243 0.7649 0.040 Uiso 1 1 calc GR . . . .
H4C H 0.2222 0.2623 0.6792 0.040 Uiso 1 1 calc GR . . . .
C12 C 0.18054(11) 0.37538(10) 0.52566(10) 0.0244(3) Uani 1 1 d . . . . .
H12 H 0.2369 0.3343 0.5366 0.029 Uiso 1 1 calc R . . . .
C23 C 0.75910(12) 0.33177(9) 0.62247(10) 0.0262(3) Uani 1 1 d . . . . .
C24 C 0.67627(13) 0.41245(11) 0.83698(11) 0.0311(4) Uani 1 1 d . . . . .
H24 H 0.6031 0.4017 0.8101 0.037 Uiso 1 1 calc R . . . .
C17 C 0.41353(13) 0.59007(10) 0.84353(11) 0.0305(4) Uani 1 1 d . . . . .
H17A H 0.4034 0.6282 0.7926 0.046 Uiso 1 1 calc GR . . . .
H17B H 0.4837 0.5947 0.8771 0.046 Uiso 1 1 calc GR . . . .
H17C H 0.3658 0.6033 0.8834 0.046 Uiso 1 1 calc GR . . . .
C19 C 0.73985(12) 0.39176(10) 0.76658(10) 0.0265(3) Uani 1 1 d . . . . .
C27 C 0.71601(13) 0.29014(10) 0.53329(11) 0.0306(4) Uani 1 1 d . . . . .
H27 H 0.6453 0.2714 0.5359 0.037 Uiso 1 1 calc R . . . .
C16 C 0.40207(15) 0.44233(11) 0.88686(11) 0.0347(4) Uani 1 1 d . . . . .
H16A H 0.3451 0.4512 0.9182 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.4667 0.4510 0.9290 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.3995 0.3863 0.8637 0.052 Uiso 1 1 calc GR . . . .
C22 C 0.86222(13) 0.35249(11) 0.64265(12) 0.0355(4) Uani 1 1 d . . . . .
H22 H 0.9046 0.3396 0.6007 0.043 Uiso 1 1 calc R . . . .
C20 C 0.84328(13) 0.41106(12) 0.78335(12) 0.0354(4) Uani 1 1 d . . . . .
H20 H 0.8723 0.4382 0.8378 0.043 Uiso 1 1 calc R . . . .
C14 C 0.07915(12) 0.32907(11) 0.50493(13) 0.0346(4) Uani 1 1 d . . . . .
H14A H 0.0708 0.2967 0.5577 0.052 Uiso 1 1 calc GR . . . .
H14B H 0.0789 0.2927 0.4534 0.052 Uiso 1 1 calc GR . . . .
H14C H 0.0229 0.3682 0.4905 0.052 Uiso 1 1 calc GR . . . .
C13 C 0.19406(13) 0.42762(11) 0.44473(11) 0.0319(4) Uani 1 1 d . . . . .
H13A H 0.1396 0.4685 0.4328 0.048 Uiso 1 1 calc GR . . . .
H13B H 0.1909 0.3926 0.3916 0.048 Uiso 1 1 calc GR . . . .
H13C H 0.2604 0.4552 0.4579 0.048 Uiso 1 1 calc GR . . . .
C21 C 0.90424(13) 0.39148(12) 0.72249(13) 0.0390(4) Uani 1 1 d . . . . .
H21 H 0.9748 0.4046 0.7351 0.047 Uiso 1 1 calc R . . . .
C25 C 0.68598(15) 0.50219(12) 0.86518(12) 0.0397(4) Uani 1 1 d . . . . .
H25A H 0.7569 0.5140 0.8930 0.060 Uiso 1 1 calc GR . . . .
H25B H 0.6417 0.5132 0.9087 0.060 Uiso 1 1 calc GR . . . .
H25C H 0.6655 0.5369 0.8120 0.060 Uiso 1 1 calc GR . . . .
C26 C 0.70550(16) 0.35783(12) 0.92052(12) 0.0423(4) Uani 1 1 d . . . . .
H26A H 0.6986 0.3003 0.9023 0.063 Uiso 1 1 calc GR . . . .
H26B H 0.6603 0.3695 0.9631 0.063 Uiso 1 1 calc GR . . . .
H26C H 0.7763 0.3688 0.9495 0.063 Uiso 1 1 calc GR . . . .
C29 C 0.70859(14) 0.34968(12) 0.45421(11) 0.0369(4) Uani 1 1 d . . . . .
H29A H 0.6647 0.3957 0.4633 0.055 Uiso 1 1 calc GR . . . .
H29B H 0.6795 0.3215 0.3980 0.055 Uiso 1 1 calc GR . . . .
H29C H 0.7768 0.3699 0.4507 0.055 Uiso 1 1 calc GR . . . .
C33 C 1.03466(16) 0.55629(14) 0.94546(14) 0.0488(6) Uani 1 1 d . . . . .
H33 H 1.0582 0.5956 0.9079 0.059 Uiso 1 1 calc R . . . .
C30 C 0.57239(14) 0.61904(13) 0.63493(11) 0.0395(4) Uani 1 1 d . . . . .
H30A H 0.6399 0.6032 0.6700 0.047 Uiso 1 1 calc R . . . .
H30B H 0.5243 0.6226 0.6773 0.047 Uiso 1 1 calc R . . . .
C32 C 1.06919(15) 0.47785(15) 0.94675(14) 0.0489(5) Uani 1 1 d . . . . .
H32 H 1.1168 0.4622 0.9104 0.059 Uiso 1 1 calc R . . . .
C28 C 0.77792(17) 0.21496(13) 0.51644(15) 0.0477(5) Uani 1 1 d . . . . .
H28A H 0.8456 0.2321 0.5074 0.072 Uiso 1 1 calc GR . . . .
H28B H 0.7426 0.1862 0.4626 0.072 Uiso 1 1 calc GR . . . .
H28C H 0.7852 0.1783 0.5686 0.072 Uiso 1 1 calc GR . . . .
C34 C 0.96602(17) 0.57884(13) 0.99820(15) 0.0518(6) Uani 1 1 d . . . . .
H34 H 0.9425 0.6337 0.9969 0.062 Uiso 1 1 calc R . . . .
C31 C 0.58068(16) 0.70164(12) 0.59273(15) 0.0474(5) Uani 1 1 d . . . . .
H31A H 0.6294 0.6987 0.5518 0.071 Uiso 1 1 calc GR . . . .
H31B H 0.6043 0.7419 0.6401 0.071 Uiso 1 1 calc GR . . . .
H31C H 0.5137 0.7180 0.5588 0.071 Uiso 1 1 calc GR . . . .
H2 H 0.4380(12) 0.1983(11) 0.7219(11) 0.019(4) 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
Ca1 Ca1 3.3733(5) 3_666 ?
Ca1 O1 2.2062(12) . ?
Ca1 O1 2.2354(11) 3_666 ?
Ca1 N2 2.3228(11) . ?
Ca1 N1 2.3456(12) . ?
O1 Ca1 2.2353(12) 3_666 ?
O1 C30 1.409(2) . ?
N2 C3 1.3261(18) . ?
N2 C18 1.4332(18) . ?
N1 C1 1.3261(19) . ?
N1 C6 1.4324(18) . ?
C3 C2 1.411(2) . ?
C3 C5 1.5184(19) . ?
C2 C1 1.413(2) . ?
C2 H2 0.980(18) . ?
C1 C4 1.5221(19) . ?
C6 C11 1.4136(19) . ?
C6 C7 1.409(2) . ?
C11 C15 1.524(2) . ?
C11 C10 1.392(2) . ?
C7 C8 1.393(2) . ?
C7 C12 1.5235(19) . ?
C18 C23 1.408(2) . ?
C18 C19 1.414(2) . ?
C15 H15 1.0000 . ?
C15 C17 1.534(2) . ?
C15 C16 1.530(2) . ?
C10 H10 0.9500 . ?
C10 C9 1.383(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C9 H9 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C12 H12 1.0000 . ?
C12 C14 1.531(2) . ?
C12 C13 1.530(2) . ?
C23 C27 1.522(2) . ?
C23 C22 1.395(2) . ?
C24 H24 1.0000 . ?
C24 C19 1.519(2) . ?
C24 C25 1.528(3) . ?
C24 C26 1.535(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 C20 1.392(2) . ?
C27 H27 1.0000 . ?
C27 C29 1.530(2) . ?
C27 C28 1.530(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.376(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 H21 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C33 H33 0.9500 . ?
C33 C32 1.363(3) . ?
C33 C34 1.373(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.508(3) . ?
C32 H32 0.9500 . ?
C32 C34 1.386(3) 3_767 ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C34 C32 1.386(3) 3_767 ?
C34 H34 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 Ca1 40.26(3) 3_666 3_666 ?
O1 Ca1 Ca1 40.90(3) . 3_666 ?
O1 Ca1 O1 81.16(5) . 3_666 ?
O1 Ca1 N2 120.37(4) . . ?
O1 Ca1 N2 125.45(4) 3_666 . ?
O1 Ca1 N1 126.73(4) 3_666 . ?
O1 Ca1 N1 127.45(4) . . ?
N2 Ca1 Ca1 135.64(3) . 3_666 ?
N2 Ca1 N1 81.76(4) . . ?
N1 Ca1 Ca1 142.56(3) . 3_666 ?
Ca1 O1 Ca1 98.84(5) . 3_666 ?
C30 O1 Ca1 132.80(10) . . ?
C30 O1 Ca1 128.28(10) . 3_666 ?
C3 N2 Ca1 122.87(9) . . ?
C3 N2 C18 119.27(11) . . ?
C18 N2 Ca1 117.66(8) . . ?
C1 N1 Ca1 122.49(9) . . ?
C1 N1 C6 118.44(11) . . ?
C6 N1 Ca1 118.33(8) . . ?
N2 C3 C2 124.38(13) . . ?
N2 C3 C5 119.47(12) . . ?
C2 C3 C5 116.13(12) . . ?
C3 C2 C1 130.75(13) . . ?
C3 C2 H2 114.3(10) . . ?
C1 C2 H2 114.0(10) . . ?
N1 C1 C2 124.95(13) . . ?
N1 C1 C4 119.83(12) . . ?
C2 C1 C4 115.21(12) . . ?
C11 C6 N1 118.58(12) . . ?
C7 C6 N1 121.16(12) . . ?
C7 C6 C11 120.17(13) . . ?
C6 C11 C15 120.59(12) . . ?
C10 C11 C6 118.64(13) . . ?
C10 C11 C15 120.76(13) . . ?
C6 C7 C12 121.72(13) . . ?
C8 C7 C6 118.83(13) . . ?
C8 C7 C12 119.35(13) . . ?
C23 C18 N2 121.84(13) . . ?
C23 C18 C19 120.01(14) . . ?
C19 C18 N2 118.01(13) . . ?
C11 C15 H15 107.3 . . ?
C11 C15 C17 112.91(12) . . ?
C11 C15 C16 111.36(12) . . ?
C17 C15 H15 107.3 . . ?
C16 C15 H15 107.3 . . ?
C16 C15 C17 110.47(12) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 C11 121.34(13) . . ?
C9 C10 H10 119.3 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.19(14) . . ?
C9 C8 H8 119.4 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C10 C9 C8 119.65(14) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C12 H12 108.0 . . ?
C7 C12 C14 113.24(13) . . ?
C7 C12 C13 109.04(13) . . ?
C14 C12 H12 108.0 . . ?
C13 C12 H12 108.0 . . ?
C13 C12 C14 110.28(13) . . ?
C18 C23 C27 121.81(14) . . ?
C22 C23 C18 118.53(15) . . ?
C22 C23 C27 119.66(14) . . ?
C19 C24 H24 107.9 . . ?
C19 C24 C25 112.35(15) . . ?
C19 C24 C26 110.87(15) . . ?
C25 C24 H24 107.9 . . ?
C25 C24 C26 109.62(14) . . ?
C26 C24 H24 107.9 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C19 C24 121.64(13) . . ?
C20 C19 C18 119.10(15) . . ?
C20 C19 C24 119.24(14) . . ?
C23 C27 H27 107.7 . . ?
C23 C27 C29 111.31(14) . . ?
C23 C27 C28 112.42(15) . . ?
C29 C27 H27 107.7 . . ?
C29 C27 C28 109.88(14) . . ?
C28 C27 H27 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C23 C22 H22 119.2 . . ?
C21 C22 C23 121.53(16) . . ?
C21 C22 H22 119.2 . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.15(16) . . ?
C21 C20 H20 119.4 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C22 C21 H21 120.2 . . ?
C20 C21 C22 119.68(15) . . ?
C20 C21 H21 120.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C33 H33 119.8 . . ?
C32 C33 C34 120.4(2) . . ?
C34 C33 H33 119.8 . . ?
O1 C30 H30A 109.2 . . ?
O1 C30 H30B 109.2 . . ?
O1 C30 C31 112.20(14) . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C33 C32 H32 120.4 . . ?
C33 C32 C34 119.2(2) . 3_767 ?
C34 C32 H32 120.4 3_767 . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C33 C34 C32 120.5(2) . 3_767 ?
C33 C34 H34 119.8 . . ?
C32 C34 H34 119.8 3_767 . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C30 C31 7.3(2) 3_666 . . . ?
Ca1 O1 C30 C31 -168.70(11) . . . . ?
Ca1 N2 C3 C2 -21.30(18) . . . . ?
Ca1 N2 C3 C5 160.16(10) . . . . ?
Ca1 N2 C18 C23 -81.54(15) . . . . ?
Ca1 N2 C18 C19 94.29(13) . . . . ?
Ca1 N1 C1 C2 15.84(18) . . . . ?
Ca1 N1 C1 C4 -165.23(10) . . . . ?
Ca1 N1 C6 C11 -87.86(13) . . . . ?
Ca1 N1 C6 C7 88.85(13) . . . . ?
N2 C3 C2 C1 -12.1(2) . . . . ?
N2 C18 C23 C27 -2.8(2) . . . . ?
N2 C18 C23 C22 176.28(14) . . . . ?
N2 C18 C19 C24 5.3(2) . . . . ?
N2 C18 C19 C20 -176.44(14) . . . . ?
N1 C6 C11 C15 0.49(19) . . . . ?
N1 C6 C11 C10 -178.44(12) . . . . ?
N1 C6 C7 C8 179.06(13) . . . . ?
N1 C6 C7 C12 -4.8(2) . . . . ?
C3 N2 C18 C23 93.35(16) . . . . ?
C3 N2 C18 C19 -90.82(16) . . . . ?
C3 C2 C1 N1 15.0(2) . . . . ?
C3 C2 C1 C4 -163.94(14) . . . . ?
C1 N1 C6 C11 101.76(15) . . . . ?
C1 N1 C6 C7 -81.53(16) . . . . ?
C6 N1 C1 C2 -174.20(12) . . . . ?
C6 N1 C1 C4 4.73(18) . . . . ?
C6 C11 C15 C17 149.33(13) . . . . ?
C6 C11 C15 C16 -85.71(16) . . . . ?
C6 C11 C10 C9 -1.9(2) . . . . ?
C6 C7 C8 C9 0.8(2) . . . . ?
C6 C7 C12 C14 137.97(15) . . . . ?
C6 C7 C12 C13 -98.86(16) . . . . ?
C11 C6 C7 C8 -4.3(2) . . . . ?
C11 C6 C7 C12 171.89(13) . . . . ?
C11 C10 C9 C8 -1.6(2) . . . . ?
C7 C6 C11 C15 -176.26(12) . . . . ?
C7 C6 C11 C10 4.8(2) . . . . ?
C7 C8 C9 C10 2.2(2) . . . . ?
C18 N2 C3 C2 164.09(13) . . . . ?
C18 N2 C3 C5 -14.45(18) . . . . ?
C18 C23 C27 C29 106.91(16) . . . . ?
C18 C23 C27 C28 -129.33(16) . . . . ?
C18 C23 C22 C21 0.0(2) . . . . ?
C18 C19 C20 C21 0.0(3) . . . . ?
C15 C11 C10 C9 179.21(14) . . . . ?
C10 C11 C15 C17 -31.76(19) . . . . ?
C10 C11 C15 C16 93.20(17) . . . . ?
C8 C7 C12 C14 -45.9(2) . . . . ?
C8 C7 C12 C13 77.28(17) . . . . ?
C5 C3 C2 C1 166.52(14) . . . . ?
C12 C7 C8 C9 -175.49(14) . . . . ?
C23 C18 C19 C24 -178.78(14) . . . . ?
C23 C18 C19 C20 -0.5(2) . . . . ?
C23 C22 C21 C20 -0.6(3) . . . . ?
C24 C19 C20 C21 178.27(16) . . . . ?
C19 C18 C23 C27 -178.51(14) . . . . ?
C19 C18 C23 C22 0.5(2) . . . . ?
C19 C20 C21 C22 0.6(3) . . . . ?
C27 C23 C22 C21 179.07(16) . . . . ?
C22 C23 C27 C29 -72.13(19) . . . . ?
C22 C23 C27 C28 51.6(2) . . . . ?
C25 C24 C19 C18 -128.56(16) . . . . ?
C25 C24 C19 C20 53.2(2) . . . . ?
C26 C24 C19 C18 108.39(17) . . . . ?
C26 C24 C19 C20 -69.9(2) . . . . ?
C32 C33 C34 C32 -0.1(3) . . . 3_767 ?
C34 C33 C32 C34 0.1(3) . . . 3_767 ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
9 0 -1 0.3326 9.0084 0.0076 -1.0030 0.1783 0.7695 -0.6818
0 6 8 0.1060 -0.0472 6.0058 7.9970 -0.9673 0.2658 -0.0605
-1 6 8 0.1104 -1.0480 6.0047 7.9973 -0.9788 0.1733 0.0111
5 9 1 0.2251 4.9447 8.9891 0.9966 -0.5728 0.1744 -0.8528
6 4 -8 0.2761 5.9873 3.9801 -8.0006 0.4188 -0.1003 -0.9597
-1 10 4 0.0883 -1.0698 9.9873 3.9978 -0.9275 -0.2319 -0.3717
-7 -2 7 0.3026 -7.0001 -1.9876 7.0009 -0.4793 -0.1324 0.8766
0 10 4 0.0893 -0.0690 9.9884 3.9974 -0.9160 -0.1395 -0.4434
5 9 -3 0.2136 4.9489 8.9800 -3.0023 -0.2744 -0.0752 -0.9996
4 -6 -7 0.2063 4.0494 -5.9992 -6.9987 0.9388 0.1664 -0.1895
1 -10 -4 0.1133 1.0698 -9.9873 -3.9978 0.9275 0.2319 0.3717
-6 7 2 0.2646 -6.0524 6.9835 2.0006 -0.6507 -0.7021 0.0903
0 10 -2 0.0807 -0.0627 9.9747 -2.0009 -0.4684 -0.5139 -0.6636
8 -4 -4 0.3017 8.0366 -3.9921 -4.0012 0.6376 0.6455 -0.4841
5 -7 3 0.2275 5.0463 -6.9732 2.9984 0.2662 0.9217 0.1648
-2 10 -2 0.1482 -2.0644 9.9725 -2.0002 -0.4915 -0.6987 -0.5202
0 -7 7 0.0893 0.0381 -6.9695 6.9992 -0.0898 0.7092 0.6700
0 7 -7 0.0880 -0.0381 6.9695 -6.9992 0.0898 -0.7092 -0.6700
-8 -4 0 0.3428 -7.9806 -4.0005 0.0035 0.1548 -0.5838 0.8095
0 -2 -9 0.0917 0.0223 -2.0164 -8.9973 0.7948 -0.4838 -0.2122
-6 -8 0 0.2577 -5.9531 -7.9900 0.0034 0.4249 -0.2433 0.9022
0 -10 -3 0.0860 0.0679 -9.9862 -2.9977 0.8414 0.2019 0.4801
-6 -8 4 0.2523 -5.9572 -7.9809 4.0023 0.1266 0.0063 1.0490
0 -10 3 0.0847 0.0617 -9.9725 3.0007 0.3938 0.5763 0.7003
6 -8 0 0.2142 6.0568 -7.9769 -0.0010 0.5632 0.8658 0.0421
7 6 0 0.2853 6.9669 5.9953 -0.0034 -0.2899 0.4136 -0.8558
0 -7 -7 0.0858 0.0526 -7.0015 -6.9971 0.9545 -0.1645 0.1563

_olex2_date_sample_data_collection 2016-07-15
_olex2_submission_original_sample_id hasj160715a
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.740
_oxdiff_exptl_absorpt_empirical_full_min 0.653
####################################################################### 
# 
# 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_hasj150130c
_database_code_depnum_ccdc_archive 'CCDC 1520540'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT305_hasj150130c         
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??)            H Check
RESPONSE: This is a calcium hydride - distances too long to be recognized as bonding
;
# Added during the CSD deposition process: Friday 02 December 2016 04:36 PM
# end Validation Reply Form

_audit_creation_date             2016-08-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H104 Ca2 N4 O2'
_chemical_formula_sum            'C66 H104 Ca2 N4 O2'
_chemical_formula_weight         1065.69
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ca N H C'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.98073(15)
_cell_length_b                   15.11446(17)
_cell_length_c                   18.0466(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.5028(12)
_cell_angle_gamma                90
_cell_volume                     3239.93(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7112
_cell_measurement_temperature    291.81(10)
_cell_measurement_theta_max      73.5630
_cell_measurement_theta_min      3.8180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.2716
_exptl_crystal_size_mid          0.1884
_exptl_crystal_size_min          0.1097
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11551
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         3.828
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.81(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -90.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   19.0000 -150.0000 116

#__ type_ start__ end____ width___ exp.time_
  3 omega  -94.00  -56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 38

#__ type_ start__ end____ width___ exp.time_
  4 omega   39.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  -90.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   50.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -150.0000 60

#__ type_ start__ end____ width___ exp.time_
  7 omega   31.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega   52.00   89.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  150.0000 37

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 10 omega   25.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -95.0000  100.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0467746000
_diffrn_orient_matrix_UB_12      0.0234316000
_diffrn_orient_matrix_UB_13      0.0730994000
_diffrn_orient_matrix_UB_21      -0.1169063000
_diffrn_orient_matrix_UB_22      -0.0343142000
_diffrn_orient_matrix_UB_23      -0.0334503000
_diffrn_orient_matrix_UB_31      0.0312056000
_diffrn_orient_matrix_UB_32      -0.0930742000
_diffrn_orient_matrix_UB_33      0.0307768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5302
_reflns_number_total             5888
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0660P)²+1.0980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1222
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C15(H15), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C10(H10), C21(H21), C8(H8), C9(H9), C20(H20)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C28(H28A,H28B,H28C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.47523(3) 0.58450(2) 0.43075(2) 0.02043(11) Uani 1 1 d . . . . .
O1 O 0.29115(11) 0.57049(9) 0.36050(8) 0.0338(3) Uani 1 1 d . . . . .
N2 N 0.47142(11) 0.74195(9) 0.43949(7) 0.0188(3) Uani 1 1 d . . . . .
N1 N 0.57383(12) 0.62323(9) 0.32919(8) 0.0204(3) Uani 1 1 d . . . . .
C3 C 0.47678(14) 0.76360(11) 0.30679(9) 0.0205(3) Uani 1 1 d . . . . .
C4 C 0.54307(14) 0.69264(11) 0.28621(9) 0.0208(3) Uani 1 1 d . . . . .
C2 C 0.45259(13) 0.79021(10) 0.37786(9) 0.0189(3) Uani 1 1 d . . . . .
C22 C 0.84488(16) 0.50998(12) 0.31294(11) 0.0281(4) Uani 1 1 d . . . . .
H22 H 0.9198 0.5132 0.3342 0.034 Uiso 1 1 calc R . . . .
C23 C 0.76620(15) 0.56731(11) 0.33776(10) 0.0235(4) Uani 1 1 d . . . . .
C6 C 0.46719(15) 0.78666(11) 0.50916(9) 0.0218(3) Uani 1 1 d . . . . .
C27 C 0.80287(14) 0.63560(11) 0.39806(10) 0.0245(4) Uani 1 1 d . . . . .
H27 H 0.7396 0.6445 0.4266 0.029 Uiso 1 1 calc R . . . .
C18 C 0.65351(15) 0.56267(11) 0.30459(10) 0.0233(4) Uani 1 1 d . . . . .
C12 C 0.67164(16) 0.83639(13) 0.50720(10) 0.0297(4) Uani 1 1 d . . . . .
H12 H 0.6607 0.8012 0.4612 0.036 Uiso 1 1 calc R . . . .
C7 C 0.56222(15) 0.83379(12) 0.54178(9) 0.0253(4) Uani 1 1 d . . . . .
C11 C 0.36979(16) 0.78217(12) 0.54550(9) 0.0264(4) Uani 1 1 d . . . . .
C15 C 0.26621(16) 0.73058(13) 0.51295(10) 0.0294(4) Uani 1 1 d . . . . .
H15 H 0.2798 0.7076 0.4641 0.035 Uiso 1 1 calc R . . . .
C29 C 0.90388(16) 0.60648(14) 0.45316(11) 0.0330(4) Uani 1 1 d . . . . .
H29A H 0.8915 0.5476 0.4702 0.050 Uiso 1 1 calc GR . . . .
H29B H 0.9132 0.6461 0.4951 0.050 Uiso 1 1 calc GR . . . .
H29C H 0.9705 0.6074 0.4288 0.050 Uiso 1 1 calc GR . . . .
C1 C 0.40393(16) 0.88266(11) 0.38104(10) 0.0267(4) Uani 1 1 d . . . . .
H1A H 0.3427 0.8818 0.4105 0.040 Uiso 1 1 calc GR . . . .
H1B H 0.3770 0.9023 0.3313 0.040 Uiso 1 1 calc GR . . . .
H1C H 0.4613 0.9223 0.4034 0.040 Uiso 1 1 calc GR . . . .
C5 C 0.58068(17) 0.70231(13) 0.20952(10) 0.0295(4) Uani 1 1 d . . . . .
H5A H 0.6614 0.7009 0.2142 0.044 Uiso 1 1 calc GR . . . .
H5B H 0.5540 0.7576 0.1878 0.044 Uiso 1 1 calc GR . . . .
H5C H 0.5504 0.6546 0.1780 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.36945(18) 0.82788(14) 0.61273(10) 0.0345(4) Uani 1 1 d . . . . .
H10 H 0.3058 0.8254 0.6371 0.041 Uiso 1 1 calc R . . . .
C21 C 0.81351(18) 0.44857(13) 0.25743(11) 0.0335(4) Uani 1 1 d . . . . .
H21 H 0.8672 0.4118 0.2406 0.040 Uiso 1 1 calc R . . . .
C28 C 0.82736(18) 0.72454(13) 0.36315(12) 0.0344(4) Uani 1 1 d . . . . .
H28A H 0.8849 0.7170 0.3313 0.052 Uiso 1 1 calc GR . . . .
H28B H 0.8525 0.7661 0.4020 0.052 Uiso 1 1 calc GR . . . .
H28C H 0.7600 0.7464 0.3343 0.052 Uiso 1 1 calc GR . . . .
C19 C 0.62030(17) 0.49775(13) 0.25052(12) 0.0332(4) Uani 1 1 d . . . . .
C8 C 0.55670(18) 0.87864(13) 0.60876(10) 0.0324(4) Uani 1 1 d . . . . .
H8 H 0.6188 0.9107 0.6303 0.039 Uiso 1 1 calc R . . . .
C9 C 0.46080(19) 0.87639(14) 0.64377(10) 0.0366(5) Uani 1 1 d . . . . .
H9 H 0.4581 0.9075 0.6880 0.044 Uiso 1 1 calc R . . . .
C20 C 0.70234(19) 0.44223(13) 0.22731(12) 0.0364(5) Uani 1 1 d . . . . .
H20 H 0.6812 0.4000 0.1906 0.044 Uiso 1 1 calc R . . . .
C14 C 0.7036(2) 0.93029(15) 0.48641(15) 0.0453(5) Uani 1 1 d . . . . .
H14A H 0.6428 0.9560 0.4536 0.068 Uiso 1 1 calc GR . . . .
H14B H 0.7699 0.9283 0.4617 0.068 Uiso 1 1 calc GR . . . .
H14C H 0.7184 0.9655 0.5309 0.068 Uiso 1 1 calc GR . . . .
C31 C 0.25264(18) 0.61517(14) 0.29090(11) 0.0359(4) Uani 1 1 d . . . . .
H31A H 0.2165 0.5722 0.2557 0.043 Uiso 1 1 calc R . . . .
H31B H 0.3175 0.6383 0.2703 0.043 Uiso 1 1 calc R . . . .
C32 C 0.20621(18) 0.51770(15) 0.38931(12) 0.0380(5) Uani 1 1 d . . . . .
H32A H 0.1427 0.5554 0.3959 0.046 Uiso 1 1 calc R . . . .
H32B H 0.2367 0.4952 0.4381 0.046 Uiso 1 1 calc R . . . .
C17 C 0.16128(18) 0.78973(16) 0.50074(13) 0.0422(5) Uani 1 1 d . . . . .
H17A H 0.1438 0.8106 0.5481 0.063 Uiso 1 1 calc GR . . . .
H17B H 0.0989 0.7563 0.4764 0.063 Uiso 1 1 calc GR . . . .
H17C H 0.1755 0.8393 0.4701 0.063 Uiso 1 1 calc GR . . . .
C16 C 0.2459(2) 0.65209(15) 0.56218(13) 0.0444(5) Uani 1 1 d . . . . .
H16A H 0.3098 0.6132 0.5661 0.067 Uiso 1 1 calc GR . . . .
H16B H 0.1800 0.6207 0.5405 0.067 Uiso 1 1 calc GR . . . .
H16C H 0.2352 0.6728 0.6110 0.067 Uiso 1 1 calc GR . . . .
C13 C 0.7668(2) 0.79450(18) 0.55942(14) 0.0500(6) Uani 1 1 d . . . . .
H13A H 0.7797 0.8281 0.6049 0.075 Uiso 1 1 calc GR . . . .
H13B H 0.8340 0.7939 0.5358 0.075 Uiso 1 1 calc GR . . . .
H13C H 0.7467 0.7350 0.5706 0.075 Uiso 1 1 calc GR . . . .
C33 C 0.1655(2) 0.44228(16) 0.34097(13) 0.0459(5) Uani 1 1 d . . . . .
H33A H 0.1287 0.4641 0.2941 0.069 Uiso 1 1 calc GR . . . .
H33B H 0.1133 0.4079 0.3651 0.069 Uiso 1 1 calc GR . . . .
H33C H 0.2282 0.4058 0.3324 0.069 Uiso 1 1 calc GR . . . .
C24 C 0.49898(19) 0.48500(16) 0.21729(15) 0.0511(6) Uani 1 1 d . . . . .
H24 H 0.4566 0.5367 0.2309 0.061 Uiso 1 1 calc R . . . .
C30 C 0.1719(2) 0.68951(18) 0.29798(14) 0.0536(6) Uani 1 1 d . . . . .
H30A H 0.1541 0.7182 0.2504 0.080 Uiso 1 1 calc GR . . . .
H30B H 0.2058 0.7315 0.3341 0.080 Uiso 1 1 calc GR . . . .
H30C H 0.1043 0.6665 0.3140 0.080 Uiso 1 1 calc GR . . . .
C25 C 0.4515(2) 0.4039(2) 0.2528(2) 0.0713(9) Uani 1 1 d . . . . .
H25A H 0.4955 0.3528 0.2440 0.107 Uiso 1 1 calc GR . . . .
H25B H 0.3749 0.3947 0.2311 0.107 Uiso 1 1 calc GR . . . .
H25C H 0.4543 0.4131 0.3057 0.107 Uiso 1 1 calc GR . . . .
C26 C 0.4831(3) 0.4787(2) 0.13149(18) 0.0704(9) Uani 1 1 d . . . . .
H26A H 0.5190 0.5282 0.1112 0.106 Uiso 1 1 calc GR . . . .
H26B H 0.4042 0.4791 0.1131 0.106 Uiso 1 1 calc GR . . . .
H26C H 0.5162 0.4248 0.1166 0.106 Uiso 1 1 calc GR . . . .
H3 H 0.4558(19) 0.8061(16) 0.2688(13) 0.036(6) Uiso 1 1 d . . . . .
H H 0.442(2) 0.4434(19) 0.4568(16) 0.060(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
Ca1 Ca1 3.5689(6) 3_666 ?
Ca1 O1 2.4054(14) . ?
Ca1 N2 2.3858(14) . ?
Ca1 N1 2.3796(14) . ?
Ca1 H 2.23(3) . ?
O1 C31 1.447(2) . ?
O1 C32 1.443(2) . ?
N2 C2 1.325(2) . ?
N2 C6 1.434(2) . ?
N1 C4 1.328(2) . ?
N1 C18 1.434(2) . ?
C3 C4 1.413(2) . ?
C3 C2 1.410(2) . ?
C3 H3 0.95(2) . ?
C4 C5 1.518(2) . ?
C2 C1 1.518(2) . ?
C22 H22 0.9300 . ?
C22 C23 1.397(2) . ?
C22 C21 1.381(3) . ?
C23 C27 1.522(3) . ?
C23 C18 1.405(3) . ?
C6 C7 1.405(3) . ?
C6 C11 1.413(2) . ?
C27 H27 0.9800 . ?
C27 C29 1.527(3) . ?
C27 C28 1.529(2) . ?
C18 C19 1.404(3) . ?
C12 H12 0.9800 . ?
C12 C7 1.524(3) . ?
C12 C14 1.530(3) . ?
C12 C13 1.519(3) . ?
C7 C8 1.395(3) . ?
C11 C15 1.518(3) . ?
C11 C10 1.397(3) . ?
C15 H15 0.9800 . ?
C15 C17 1.535(3) . ?
C15 C16 1.521(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C10 H10 0.9300 . ?
C10 C9 1.375(3) . ?
C21 H21 0.9300 . ?
C21 C20 1.375(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C19 C20 1.398(3) . ?
C19 C24 1.511(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.382(3) . ?
C9 H9 0.9300 . ?
C20 H20 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C30 1.499(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.479(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C24 H24 0.9800 . ?
C24 C25 1.528(4) . ?
C24 C26 1.538(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ca1 Ca1 H 35.5(7) 3_666 . ?
O1 Ca1 Ca1 111.30(4) . 3_666 ?
O1 Ca1 H 81.5(7) . . ?
N2 Ca1 Ca1 132.11(4) . 3_666 ?
N2 Ca1 O1 95.65(5) . . ?
N2 Ca1 H 159.1(7) . . ?
N1 Ca1 Ca1 131.42(4) . 3_666 ?
N1 Ca1 O1 97.41(5) . . ?
N1 Ca1 N2 79.70(5) . . ?
N1 Ca1 H 121.2(7) . . ?
C31 O1 Ca1 125.64(11) . . ?
C32 O1 Ca1 120.01(12) . . ?
C32 O1 C31 114.26(15) . . ?
C2 N2 Ca1 119.77(10) . . ?
C2 N2 C6 117.07(13) . . ?
C6 N2 Ca1 122.08(10) . . ?
C4 N1 Ca1 121.09(11) . . ?
C4 N1 C18 117.94(14) . . ?
C18 N1 Ca1 119.93(10) . . ?
C4 C3 H3 115.4(14) . . ?
C2 C3 C4 130.17(15) . . ?
C2 C3 H3 113.4(14) . . ?
N1 C4 C3 124.67(15) . . ?
N1 C4 C5 121.07(15) . . ?
C3 C4 C5 114.25(15) . . ?
N2 C2 C3 125.03(15) . . ?
N2 C2 C1 119.95(14) . . ?
C3 C2 C1 115.00(14) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.22(18) . . ?
C22 C23 C27 120.40(16) . . ?
C22 C23 C18 118.92(17) . . ?
C18 C23 C27 120.65(15) . . ?
C7 C6 N2 119.12(15) . . ?
C7 C6 C11 120.19(15) . . ?
C11 C6 N2 120.67(16) . . ?
C23 C27 H27 107.4 . . ?
C23 C27 C29 113.58(15) . . ?
C23 C27 C28 110.77(15) . . ?
C29 C27 H27 107.4 . . ?
C29 C27 C28 110.08(16) . . ?
C28 C27 H27 107.4 . . ?
C23 C18 N1 118.52(15) . . ?
C19 C18 N1 121.43(16) . . ?
C19 C18 C23 120.01(16) . . ?
C7 C12 H12 107.8 . . ?
C7 C12 C14 112.39(16) . . ?
C14 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C13 C12 C7 110.55(17) . . ?
C13 C12 C14 110.31(19) . . ?
C6 C7 C12 122.31(15) . . ?
C8 C7 C6 118.80(17) . . ?
C8 C7 C12 118.88(17) . . ?
C6 C11 C15 121.89(15) . . ?
C10 C11 C6 118.41(18) . . ?
C10 C11 C15 119.70(17) . . ?
C11 C15 H15 107.9 . . ?
C11 C15 C17 111.67(16) . . ?
C11 C15 C16 111.09(17) . . ?
C17 C15 H15 107.9 . . ?
C16 C15 H15 107.9 . . ?
C16 C15 C17 110.36(17) . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.69(18) . . ?
C9 C10 H10 119.2 . . ?
C22 C21 H21 120.3 . . ?
C20 C21 C22 119.44(17) . . ?
C20 C21 H21 120.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C18 C19 C24 122.38(17) . . ?
C20 C19 C18 118.77(19) . . ?
C20 C19 C24 118.84(18) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.36(19) . . ?
C9 C8 H8 119.3 . . ?
C10 C9 C8 119.48(17) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C21 C20 C19 121.51(19) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C31 H31A 108.7 . . ?
O1 C31 H31B 108.7 . . ?
O1 C31 C30 114.32(18) . . ?
H31A C31 H31B 107.6 . . ?
C30 C31 H31A 108.7 . . ?
C30 C31 H31B 108.7 . . ?
O1 C32 H32A 108.7 . . ?
O1 C32 H32B 108.7 . . ?
O1 C32 C33 114.04(17) . . ?
H32A C32 H32B 107.6 . . ?
C33 C32 H32A 108.7 . . ?
C33 C32 H32B 108.7 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C19 C24 H24 107.6 . . ?
C19 C24 C25 109.1(2) . . ?
C19 C24 C26 113.2(2) . . ?
C25 C24 H24 107.6 . . ?
C25 C24 C26 111.6(2) . . ?
C26 C24 H24 107.6 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C31 C30 -106.18(19) . . . . ?
Ca1 O1 C32 C33 -119.03(18) . . . . ?
Ca1 N2 C2 C3 -26.2(2) . . . . ?
Ca1 N2 C2 C1 155.34(12) . . . . ?
Ca1 N2 C6 C7 110.02(15) . . . . ?
Ca1 N2 C6 C11 -68.76(18) . . . . ?
Ca1 N1 C4 C3 19.9(2) . . . . ?
Ca1 N1 C4 C5 -161.61(13) . . . . ?
Ca1 N1 C18 C23 -89.39(17) . . . . ?
Ca1 N1 C18 C19 88.38(18) . . . . ?
N2 C6 C7 C12 -2.3(2) . . . . ?
N2 C6 C7 C8 178.68(15) . . . . ?
N2 C6 C11 C15 -0.1(3) . . . . ?
N2 C6 C11 C10 -179.15(16) . . . . ?
N1 C18 C19 C20 178.26(17) . . . . ?
N1 C18 C19 C24 -2.6(3) . . . . ?
C4 N1 C18 C23 102.16(19) . . . . ?
C4 N1 C18 C19 -80.1(2) . . . . ?
C4 C3 C2 N2 -13.8(3) . . . . ?
C4 C3 C2 C1 164.70(17) . . . . ?
C2 N2 C6 C7 -81.94(19) . . . . ?
C2 N2 C6 C11 99.28(19) . . . . ?
C2 C3 C4 N1 17.7(3) . . . . ?
C2 C3 C4 C5 -160.83(17) . . . . ?
C22 C23 C27 C29 -30.2(2) . . . . ?
C22 C23 C27 C28 94.28(19) . . . . ?
C22 C23 C18 N1 -178.53(15) . . . . ?
C22 C23 C18 C19 3.7(3) . . . . ?
C22 C21 C20 C19 1.3(3) . . . . ?
C23 C22 C21 C20 -1.6(3) . . . . ?
C23 C18 C19 C20 -4.0(3) . . . . ?
C23 C18 C19 C24 175.2(2) . . . . ?
C6 N2 C2 C3 165.44(16) . . . . ?
C6 N2 C2 C1 -13.0(2) . . . . ?
C6 C7 C8 C9 1.0(3) . . . . ?
C6 C11 C15 C17 -122.24(19) . . . . ?
C6 C11 C15 C16 114.08(19) . . . . ?
C6 C11 C10 C9 0.0(3) . . . . ?
C27 C23 C18 N1 -0.4(2) . . . . ?
C27 C23 C18 C19 -178.24(16) . . . . ?
C18 N1 C4 C3 -171.76(16) . . . . ?
C18 N1 C4 C5 6.7(2) . . . . ?
C18 C23 C27 C29 151.73(16) . . . . ?
C18 C23 C27 C28 -83.79(19) . . . . ?
C18 C19 C20 C21 1.5(3) . . . . ?
C18 C19 C24 C25 -103.1(2) . . . . ?
C18 C19 C24 C26 131.9(2) . . . . ?
C12 C7 C8 C9 -178.06(18) . . . . ?
C7 C6 C11 C15 -178.83(16) . . . . ?
C7 C6 C11 C10 2.1(3) . . . . ?
C7 C8 C9 C10 1.1(3) . . . . ?
C11 C6 C7 C12 176.46(16) . . . . ?
C11 C6 C7 C8 -2.5(3) . . . . ?
C11 C10 C9 C8 -1.5(3) . . . . ?
C15 C11 C10 C9 -179.14(18) . . . . ?
C10 C11 C15 C17 56.8(2) . . . . ?
C10 C11 C15 C16 -66.8(2) . . . . ?
C21 C22 C23 C27 -178.93(16) . . . . ?
C21 C22 C23 C18 -0.8(3) . . . . ?
C20 C19 C24 C25 76.1(3) . . . . ?
C20 C19 C24 C26 -48.9(3) . . . . ?
C14 C12 C7 C6 119.0(2) . . . . ?
C14 C12 C7 C8 -62.0(2) . . . . ?
C31 O1 C32 C33 64.2(2) . . . . ?
C32 O1 C31 C30 70.4(2) . . . . ?
C13 C12 C7 C6 -117.2(2) . . . . ?
C13 C12 C7 C8 61.8(2) . . . . ?
C24 C19 C20 C21 -177.7(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 9 -4 0.0847 -1.0097 8.9868 -3.9940 -0.0342 -0.0568 -0.9908
7 -3 3 0.1104 7.0038 -2.9824 3.0056 -0.1778 -0.8170 0.5886
-5 -8 2 0.0540 -4.9918 -8.0000 1.9879 0.1914 0.7916 0.6500
2 -9 -2 0.0837 2.0127 -8.9880 -2.0073 -0.4515 0.1403 0.8375
2 -5 -10 0.0942 2.0114 -4.9961 -10.0066 -0.9426 0.2710 0.2198
-3 9 -2 0.0735 -3.0110 8.9841 -1.9953 0.2055 0.1105 -0.9915
2 6 -9 0.1112 1.9970 5.9930 -8.9957 -0.6106 -0.1382 -0.7723
5 -1 -10 0.0963 5.0069 -0.9947 -9.9997 -0.9885 -0.2167 -0.0590
5 -6 -6 0.0756 5.0114 -5.9875 -6.0029 -0.8135 -0.1796 0.5289
6 5 -6 0.1420 5.9977 5.0030 -5.9913 -0.6013 -0.6724 -0.4629
8 0 -4 0.1294 8.0035 0.0129 -3.9933 -0.6660 -0.8025 0.1256
4 8 -1 0.1270 3.9912 7.9986 -0.9886 -0.0715 -0.7080 -0.6503
-7 -2 -2 0.1227 -6.9979 -2.0119 -2.0100 0.1333 0.9544 -0.0929
5 -6 4 0.1122 5.0067 -5.9825 4.0010 -0.0819 -0.5139 0.8361
6 1 7 0.0873 5.9967 1.0136 7.0099 0.2557 -0.9703 0.3085
3 9 2 0.1041 2.9883 8.9972 2.0125 0.2182 -0.7254 -0.6822
0 7 8 0.0366 -0.0125 6.9967 8.0099 0.7500 -0.5066 -0.4051
-1 10 0 0.0637 -1.0128 9.9878 0.0086 0.2820 -0.2246 -0.9609
-3 7 7 0.0232 -3.0127 6.9907 7.0063 0.8169 -0.1220 -0.5290
-3 9 2 0.0388 -3.0129 8.9861 2.0063 0.4981 -0.0232 -0.8686
-3 5 10 0.0392 -3.0116 4.9942 10.0056 0.9893 -0.1540 -0.2509
-6 3 8 0.0263 -6.0087 2.9897 7.9998 0.9359 0.3323 -0.2195
-7 -2 7 0.0300 -7.0021 -2.0074 6.9936 0.7917 0.6536 0.1836
0 -10 2 0.0818 0.0117 -9.9886 1.9912 -0.0890 0.2748 0.9913
-5 3 -7 0.1391 -5.0015 2.9841 -7.0051 -0.2082 0.7166 -0.6494
4 -3 -10 0.0816 4.0092 -2.9944 -10.0027 -0.9889 -0.0314 0.0959

_olex2_date_sample_data_collection 2015-01-30
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hasj160518a
_database_code_depnum_ccdc_archive 'CCDC 1520546'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_audit_creation_date             2016-10-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H92 Ca2 N4 O2'
_chemical_formula_sum            'C62 H92 Ca2 N4 O2'
_chemical_formula_weight         1005.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.2642(3)
_cell_length_b                   15.2818(3)
_cell_length_c                   16.5278(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.457(2)
_cell_angle_gamma                90
_cell_volume                     3012.58(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5983
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4490
_cell_measurement_theta_min      4.0490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.4098
_exptl_crystal_size_min          0.2824
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9482
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         4.069
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  25.00   1.00    1.00    --  -41.88  77.00 -60.00   89
  2  ω   -107.00 -22.00   1.00    1.00    --  -41.88 -57.00 150.00   85
  3  ω     46.00 134.00   1.00    1.10    --  106.00 -61.00 120.00   88
  4  ω     89.00 176.00   1.00    1.10    --  106.00  45.00   0.00   87
  5  ω     94.00 178.00   1.00    1.10    --  106.00 125.00-180.00   84
  6  ω     75.00 170.00   1.00    1.10    --  106.00  77.00 -90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0482507000
_diffrn_orient_matrix_UB_12      -0.0885118000
_diffrn_orient_matrix_UB_13      -0.0196223000
_diffrn_orient_matrix_UB_21      0.0488351000
_diffrn_orient_matrix_UB_22      -0.0153044000
_diffrn_orient_matrix_UB_23      0.0935281000
_diffrn_orient_matrix_UB_31      -0.1095299000
_diffrn_orient_matrix_UB_32      -0.0457127000
_diffrn_orient_matrix_UB_33      0.0067950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4976
_reflns_number_total             5446
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²+1.1630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1181
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C20(H20), C21(H21), C22(H22), C8(H8), C10(H10), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.47993(3) 0.41283(2) 0.56011(2) 0.02309(12) Uani 1 1 d . . . . .
O1 O 0.40048(11) 0.47658(8) 0.43947(8) 0.0293(3) Uani 1 1 d . . . . .
N1 N 0.50715(11) 0.26064(9) 0.56493(8) 0.0190(3) Uani 1 1 d . . . . .
N2 N 0.40288(11) 0.37912(9) 0.67473(8) 0.0184(3) Uani 1 1 d . . . . .
C3 C 0.44211(13) 0.31442(11) 0.72717(10) 0.0190(3) Uani 1 1 d . . . . .
C1 C 0.53665(13) 0.21833(10) 0.63680(10) 0.0192(3) Uani 1 1 d . . . . .
C2 C 0.51369(13) 0.24735(11) 0.71174(10) 0.0204(3) Uani 1 1 d . . . . .
H2 H 0.5527 0.2168 0.7599 0.024 Uiso 1 1 calc R . . . .
C18 C 0.32349(14) 0.43908(11) 0.69501(10) 0.0205(3) Uani 1 1 d . . . . .
C19 C 0.21035(14) 0.43298(11) 0.65089(10) 0.0215(3) Uani 1 1 d . . . . .
C23 C 0.35779(15) 0.50503(11) 0.75489(11) 0.0238(4) Uani 1 1 d . . . . .
C6 C 0.51266(14) 0.21580(11) 0.48991(10) 0.0222(3) Uani 1 1 d . . . . .
C27 C 0.47973(15) 0.51904(12) 0.79877(11) 0.0283(4) Uani 1 1 d . . . . .
H27 H 0.5229 0.4665 0.7880 0.034 Uiso 1 1 calc R . . . .
C20 C 0.13250(15) 0.49082(12) 0.67070(12) 0.0267(4) Uani 1 1 d . . . . .
H20 H 0.0561 0.4870 0.6416 0.032 Uiso 1 1 calc R . . . .
C5 C 0.40767(14) 0.30612(12) 0.80936(10) 0.0246(4) Uani 1 1 d . . . . .
H5A H 0.4666 0.3305 0.8541 0.037 Uiso 1 1 calc GR . . . .
H5B H 0.3965 0.2442 0.8208 0.037 Uiso 1 1 calc GR . . . .
H5C H 0.3376 0.3382 0.8062 0.037 Uiso 1 1 calc GR . . . .
C7 C 0.42207(15) 0.16356(12) 0.44948(11) 0.0282(4) Uani 1 1 d . . . . .
C21 C 0.16437(16) 0.55360(12) 0.73185(12) 0.0303(4) Uani 1 1 d . . . . .
H21 H 0.1100 0.5914 0.7458 0.036 Uiso 1 1 calc R . . . .
C24 C 0.17343(14) 0.36174(11) 0.58618(11) 0.0235(4) Uani 1 1 d . . . . .
H24 H 0.2380 0.3492 0.5605 0.028 Uiso 1 1 calc R . . . .
C22 C 0.27584(16) 0.56098(12) 0.77255(11) 0.0285(4) Uani 1 1 d . . . . .
H22 H 0.2975 0.6051 0.8136 0.034 Uiso 1 1 calc R . . . .
C12 C 0.32138(16) 0.14648(14) 0.48667(12) 0.0332(4) Uani 1 1 d . . . . .
H12 H 0.3337 0.1787 0.5407 0.040 Uiso 1 1 calc R . . . .
C11 C 0.60535(15) 0.22880(12) 0.45436(11) 0.0280(4) Uani 1 1 d . . . . .
C4 C 0.59539(16) 0.13041(12) 0.64130(12) 0.0287(4) Uani 1 1 d . . . . .
H4A H 0.5393 0.0838 0.6274 0.043 Uiso 1 1 calc GR . . . .
H4B H 0.6410 0.1212 0.6977 0.043 Uiso 1 1 calc GR . . . .
H4C H 0.6437 0.1295 0.6017 0.043 Uiso 1 1 calc GR . . . .
C26 C 0.07391(15) 0.38745(13) 0.51617(12) 0.0312(4) Uani 1 1 d . . . . .
H26A H 0.0067 0.3930 0.5383 0.047 Uiso 1 1 calc GR . . . .
H26B H 0.0616 0.3423 0.4728 0.047 Uiso 1 1 calc GR . . . .
H26C H 0.0895 0.4435 0.4924 0.047 Uiso 1 1 calc GR . . . .
C15 C 0.70556(15) 0.28254(14) 0.49789(12) 0.0329(4) Uani 1 1 d . . . . .
H15 H 0.6912 0.3034 0.5518 0.040 Uiso 1 1 calc R . . . .
C8 C 0.42523(18) 0.12512(14) 0.37333(13) 0.0380(5) Uani 1 1 d . . . . .
H8 H 0.3646 0.0894 0.3456 0.046 Uiso 1 1 calc R . . . .
C28 C 0.52707(17) 0.59894(14) 0.76257(13) 0.0369(5) Uani 1 1 d . . . . .
H28A H 0.5202 0.5902 0.7029 0.055 Uiso 1 1 calc GR . . . .
H28B H 0.6063 0.6064 0.7905 0.055 Uiso 1 1 calc GR . . . .
H28C H 0.4851 0.6513 0.7713 0.055 Uiso 1 1 calc GR . . . .
C25 C 0.14799(18) 0.27770(13) 0.62856(13) 0.0372(5) Uani 1 1 d . . . . .
H25A H 0.2153 0.2589 0.6694 0.056 Uiso 1 1 calc GR . . . .
H25B H 0.1251 0.2318 0.5867 0.056 Uiso 1 1 calc GR . . . .
H25C H 0.0873 0.2886 0.6568 0.056 Uiso 1 1 calc GR . . . .
C10 C 0.60396(18) 0.18934(15) 0.37794(13) 0.0373(5) Uani 1 1 d . . . . .
H10 H 0.6657 0.1979 0.3531 0.045 Uiso 1 1 calc R . . . .
C29 C 0.49667(18) 0.52846(14) 0.89322(12) 0.0369(5) Uani 1 1 d . . . . .
H29A H 0.4615 0.5828 0.9058 0.055 Uiso 1 1 calc GR . . . .
H29B H 0.5771 0.5300 0.9192 0.055 Uiso 1 1 calc GR . . . .
H29C H 0.4623 0.4785 0.9150 0.055 Uiso 1 1 calc GR . . . .
C9 C 0.5155(2) 0.13837(16) 0.33772(13) 0.0427(5) Uani 1 1 d . . . . .
H9 H 0.5163 0.1123 0.2857 0.051 Uiso 1 1 calc R . . . .
C30 C 0.29706(18) 0.45368(16) 0.38731(14) 0.0402(5) Uani 1 1 d . . . . .
C14 C 0.21365(18) 0.18124(16) 0.42984(15) 0.0464(6) Uani 1 1 d . . . . .
H14A H 0.2210 0.2443 0.4215 0.070 Uiso 1 1 calc GR . . . .
H14B H 0.1505 0.1705 0.4555 0.070 Uiso 1 1 calc GR . . . .
H14C H 0.2003 0.1513 0.3760 0.070 Uiso 1 1 calc GR . . . .
C13 C 0.30897(18) 0.04907(16) 0.50461(15) 0.0450(5) Uani 1 1 d . . . . .
H13A H 0.2923 0.0164 0.4521 0.067 Uiso 1 1 calc GR . . . .
H13B H 0.2477 0.0412 0.5329 0.067 Uiso 1 1 calc GR . . . .
H13C H 0.3790 0.0273 0.5403 0.067 Uiso 1 1 calc GR . . . .
C17 C 0.72259(19) 0.36286(15) 0.44762(15) 0.0441(5) Uani 1 1 d . . . . .
H17A H 0.7392 0.3443 0.3950 0.066 Uiso 1 1 calc GR . . . .
H17B H 0.7853 0.3976 0.4794 0.066 Uiso 1 1 calc GR . . . .
H17C H 0.6542 0.3984 0.4361 0.066 Uiso 1 1 calc GR . . . .
C16 C 0.81281(18) 0.22649(18) 0.51785(16) 0.0495(6) Uani 1 1 d . . . . .
H16A H 0.7999 0.1741 0.5485 0.074 Uiso 1 1 calc GR . . . .
H16B H 0.8744 0.2606 0.5519 0.074 Uiso 1 1 calc GR . . . .
H16C H 0.8323 0.2092 0.4659 0.074 Uiso 1 1 calc GR . . . .
C31 C 0.2494(3) 0.52665(18) 0.32808(16) 0.0625(8) Uani 1 1 d . . . . .
H31A H 0.2464 0.5806 0.3596 0.094 Uiso 1 1 calc GR . . . .
H31B H 0.1736 0.5110 0.2973 0.094 Uiso 1 1 calc GR . . . .
H31C H 0.2972 0.5358 0.2889 0.094 Uiso 1 1 calc GR . . . .
H30A H 0.304(3) 0.394(2) 0.3541(19) 0.070(9) Uiso 1 1 d . . . . .
H30B H 0.236(3) 0.446(3) 0.418(2) 0.102(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
Ca1 O1 2.2294(13) . ?
Ca1 O1 2.2367(13) 3_666 ?
Ca1 N1 2.3482(14) . ?
Ca1 N2 2.3624(13) . ?
O1 Ca1 2.2367(13) 3_666 ?
O1 C30 1.402(2) . ?
N1 C1 1.327(2) . ?
N1 C6 1.432(2) . ?
N2 C3 1.329(2) . ?
N2 C18 1.432(2) . ?
C3 C2 1.411(2) . ?
C3 C5 1.519(2) . ?
C1 C2 1.404(2) . ?
C1 C4 1.518(2) . ?
C2 H2 0.9500 . ?
C18 C19 1.412(2) . ?
C18 C23 1.406(2) . ?
C19 C20 1.395(2) . ?
C19 C24 1.519(2) . ?
C23 C27 1.518(3) . ?
C23 C22 1.401(2) . ?
C6 C7 1.405(3) . ?
C6 C11 1.410(2) . ?
C27 H27 1.0000 . ?
C27 C28 1.532(3) . ?
C27 C29 1.533(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C12 1.524(3) . ?
C7 C8 1.398(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.381(3) . ?
C24 H24 1.0000 . ?
C24 C26 1.525(2) . ?
C24 C25 1.529(2) . ?
C22 H22 0.9500 . ?
C12 H12 1.0000 . ?
C12 C14 1.527(3) . ?
C12 C13 1.532(3) . ?
C11 C15 1.514(3) . ?
C11 C10 1.396(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C17 1.524(3) . ?
C15 C16 1.540(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C9 1.375(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C9 H9 0.9500 . ?
C30 C31 1.509(3) . ?
C30 H30A 1.08(3) . ?
C30 H30B 1.00(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 79.77(5) . 3_666 ?
O1 Ca1 N1 131.32(5) 3_666 . ?
O1 Ca1 N1 119.49(5) . . ?
O1 Ca1 N2 129.75(5) . . ?
O1 Ca1 N2 123.14(5) 3_666 . ?
N1 Ca1 N2 80.62(5) . . ?
Ca1 O1 Ca1 100.23(5) . 3_666 ?
C30 O1 Ca1 125.84(12) . . ?
C30 O1 Ca1 133.57(12) . 3_666 ?
C1 N1 Ca1 121.34(11) . . ?
C1 N1 C6 118.95(14) . . ?
C6 N1 Ca1 118.66(10) . . ?
C3 N2 Ca1 122.25(10) . . ?
C3 N2 C18 119.07(13) . . ?
C18 N2 Ca1 117.95(10) . . ?
N2 C3 C2 124.65(15) . . ?
N2 C3 C5 120.77(14) . . ?
C2 C3 C5 114.54(14) . . ?
N1 C1 C2 124.54(15) . . ?
N1 C1 C4 120.17(15) . . ?
C2 C1 C4 115.24(14) . . ?
C3 C2 H2 114.7 . . ?
C1 C2 C3 130.53(15) . . ?
C1 C2 H2 114.7 . . ?
C19 C18 N2 118.46(15) . . ?
C23 C18 N2 120.98(15) . . ?
C23 C18 C19 120.50(15) . . ?
C18 C19 C24 120.44(15) . . ?
C20 C19 C18 118.74(16) . . ?
C20 C19 C24 120.74(16) . . ?
C18 C23 C27 122.51(15) . . ?
C22 C23 C18 118.18(16) . . ?
C22 C23 C27 119.29(16) . . ?
C7 C6 N1 119.51(15) . . ?
C7 C6 C11 120.46(16) . . ?
C11 C6 N1 119.90(15) . . ?
C23 C27 H27 107.8 . . ?
C23 C27 C28 110.28(16) . . ?
C23 C27 C29 112.63(16) . . ?
C28 C27 H27 107.8 . . ?
C28 C27 C29 110.42(16) . . ?
C29 C27 H27 107.8 . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.26(17) . . ?
C21 C20 H20 119.4 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 C7 C12 122.06(16) . . ?
C8 C7 C6 118.86(17) . . ?
C8 C7 C12 119.07(17) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.49(16) . . ?
C22 C21 H21 120.3 . . ?
C19 C24 H24 107.5 . . ?
C19 C24 C26 113.85(15) . . ?
C19 C24 C25 109.79(15) . . ?
C26 C24 H24 107.5 . . ?
C26 C24 C25 110.56(15) . . ?
C25 C24 H24 107.5 . . ?
C23 C22 H22 119.1 . . ?
C21 C22 C23 121.72(17) . . ?
C21 C22 H22 119.1 . . ?
C7 C12 H12 107.9 . . ?
C7 C12 C14 111.01(18) . . ?
C7 C12 C13 111.75(16) . . ?
C14 C12 H12 107.9 . . ?
C14 C12 C13 110.26(17) . . ?
C13 C12 H12 107.9 . . ?
C6 C11 C15 121.50(16) . . ?
C10 C11 C6 118.35(18) . . ?
C10 C11 C15 120.13(16) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C11 C15 H15 107.7 . . ?
C11 C15 C17 112.15(17) . . ?
C11 C15 C16 111.02(18) . . ?
C17 C15 H15 107.7 . . ?
C17 C15 C16 110.26(17) . . ?
C16 C15 H15 107.7 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(2) . . ?
C9 C8 H8 119.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.62(18) . . ?
C9 C10 H10 119.2 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.77(18) . . ?
C10 C9 H9 120.1 . . ?
O1 C30 C31 111.90(19) . . ?
O1 C30 H30A 110.7(16) . . ?
O1 C30 H30B 113(2) . . ?
C31 C30 H30A 111.2(16) . . ?
C31 C30 H30B 101(2) . . ?
H30A C30 H30B 109(3) . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C30 C31 160.15(16) . . . . ?
Ca1 O1 C30 C31 -11.5(3) 3_666 . . . ?
Ca1 N1 C1 C2 25.7(2) . . . . ?
Ca1 N1 C1 C4 -156.84(12) . . . . ?
Ca1 N1 C6 C7 -106.76(16) . . . . ?
Ca1 N1 C6 C11 69.15(18) . . . . ?
Ca1 N2 C3 C2 -15.1(2) . . . . ?
Ca1 N2 C3 C5 167.29(11) . . . . ?
Ca1 N2 C18 C19 82.99(16) . . . . ?
Ca1 N2 C18 C23 -94.30(16) . . . . ?
N1 C1 C2 C3 12.2(3) . . . . ?
N1 C6 C7 C12 -5.3(3) . . . . ?
N1 C6 C7 C8 175.58(17) . . . . ?
N1 C6 C11 C15 6.0(3) . . . . ?
N1 C6 C11 C10 -175.18(16) . . . . ?
N2 C3 C2 C1 -18.4(3) . . . . ?
N2 C18 C19 C20 179.60(14) . . . . ?
N2 C18 C19 C24 2.7(2) . . . . ?
N2 C18 C23 C27 2.4(3) . . . . ?
N2 C18 C23 C22 -179.31(15) . . . . ?
C3 N2 C18 C19 -106.57(17) . . . . ?
C3 N2 C18 C23 76.1(2) . . . . ?
C1 N1 C6 C7 84.8(2) . . . . ?
C1 N1 C6 C11 -99.27(19) . . . . ?
C18 N2 C3 C2 174.94(15) . . . . ?
C18 N2 C3 C5 -2.7(2) . . . . ?
C18 C19 C20 C21 0.4(3) . . . . ?
C18 C19 C24 C26 -150.54(16) . . . . ?
C18 C19 C24 C25 84.91(19) . . . . ?
C18 C23 C27 C28 103.79(19) . . . . ?
C18 C23 C27 C29 -132.35(18) . . . . ?
C18 C23 C22 C21 -1.2(3) . . . . ?
C19 C18 C23 C27 -174.81(16) . . . . ?
C19 C18 C23 C22 3.5(2) . . . . ?
C19 C20 C21 C22 1.9(3) . . . . ?
C23 C18 C19 C20 -3.1(2) . . . . ?
C23 C18 C19 C24 179.95(15) . . . . ?
C6 N1 C1 C2 -166.15(15) . . . . ?
C6 N1 C1 C4 11.3(2) . . . . ?
C6 C7 C12 C14 118.7(2) . . . . ?
C6 C7 C12 C13 -117.8(2) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C6 C11 C15 C17 -117.94(19) . . . . ?
C6 C11 C15 C16 118.22(19) . . . . ?
C6 C11 C10 C9 -0.4(3) . . . . ?
C27 C23 C22 C21 177.15(17) . . . . ?
C20 C19 C24 C26 32.6(2) . . . . ?
C20 C19 C24 C25 -91.98(19) . . . . ?
C20 C21 C22 C23 -1.5(3) . . . . ?
C5 C3 C2 C1 159.37(17) . . . . ?
C7 C6 C11 C15 -178.13(17) . . . . ?
C7 C6 C11 C10 0.7(3) . . . . ?
C7 C8 C9 C10 0.6(4) . . . . ?
C24 C19 C20 C21 177.33(16) . . . . ?
C22 C23 C27 C28 -74.5(2) . . . . ?
C22 C23 C27 C29 49.4(2) . . . . ?
C12 C7 C8 C9 -179.5(2) . . . . ?
C11 C6 C7 C12 178.80(17) . . . . ?
C11 C6 C7 C8 -0.3(3) . . . . ?
C11 C10 C9 C8 -0.2(3) . . . . ?
C4 C1 C2 C3 -165.32(17) . . . . ?
C15 C11 C10 C9 178.4(2) . . . . ?
C8 C7 C12 C14 -62.2(2) . . . . ?
C8 C7 C12 C13 61.4(2) . . . . ?
C10 C11 C15 C17 63.3(2) . . . . ?
C10 C11 C15 C16 -60.6(2) . . . . ?

_shelx_SHELXL_version_number     2014/7

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6 0 -5 0.1799 -5.9916 0.0013 -5.0116 0.1902 0.7624 -0.6210
-1 5 9 0.2116 -0.9848 5.0014 8.9930 -0.2186 -0.8691 -0.3991
4 2 7 0.1477 4.0000 1.9996 7.0057 -0.2321 -0.8818 0.2976
2 -5 -9 0.2037 1.9837 -5.0017 -8.9910 0.1705 0.8199 0.5084
7 -3 0 0.1965 6.9819 -3.0022 0.0165 -0.0705 -0.2981 0.9014
0 -9 4 0.1385 -0.0321 -8.9996 4.0060 0.8766 -0.2353 0.3799
-2 -9 5 0.1456 -2.0302 -8.9989 5.0017 0.9923 -0.2304 0.1541
-3 -8 6 0.1617 -3.0260 -7.9985 5.9988 0.9714 -0.2901 -0.0075
-8 1 5 0.3121 -7.9893 1.0031 4.9822 0.3940 -0.0893 -0.9552
-5 7 1 0.2461 -4.9708 7.0017 0.9845 -0.3607 0.0446 -0.8710
0 9 -4 0.2439 0.0321 8.9996 -4.0060 -0.8766 0.2353 -0.3799
5 7 -6 0.2131 5.0204 6.9978 -5.9940 -0.9788 0.2072 0.2716
7 2 -6 0.1667 7.0011 1.9972 -5.9863 -0.6316 0.1858 0.7169
0 -10 -2 0.1857 -0.0335 -10.0003 -1.9925 0.8474 0.3409 0.4673
-3 -9 -1 0.2084 -3.0271 -8.9993 -0.9995 0.9226 0.3796 0.0869
-6 -6 1 0.2075 -6.0142 -5.9981 0.9919 0.8401 0.2940 -0.3912
-5 8 3 0.2503 -4.9681 8.0020 2.9835 -0.4101 -0.1577 -0.9304
0 10 2 0.2405 0.0335 10.0003 1.9925 -0.8474 -0.3409 -0.4673
5 8 0 0.2146 5.0218 7.9985 0.0044 -0.9497 -0.3691 0.1842
7 3 -1 0.1393 7.0028 2.9977 -0.9877 -0.6221 -0.2970 0.6365
7 4 -1 0.1372 7.0062 3.9978 -0.9884 -0.7108 -0.3124 0.5912
0 -8 -7 0.1950 -0.0250 -8.0009 -6.9932 0.5719 0.7775 0.4117
-2 -7 -6 0.1891 -2.0197 -7.0001 -5.9982 0.5990 0.7670 0.1407
-6 -4 -4 0.1916 -6.0057 -3.9986 -4.0088 0.5645 0.7305 -0.4467
-6 -3 -3 0.1842 -6.0026 -2.9985 -3.0097 0.4955 0.6217 -0.4991
-8 0 -1 0.2506 -7.9907 0.0024 -1.0162 0.3649 0.4869 -0.8678
-3 8 6 0.2379 -2.9713 8.0017 5.9872 -0.4473 -0.5365 -0.7327
-5 7 6 0.2576 -4.9725 7.0023 5.9838 -0.2625 -0.4227 -0.9061
0 8 7 0.2146 0.0250 8.0009 6.9932 -0.5719 -0.7775 -0.4117
1 7 6 0.1947 1.0208 7.0004 5.9961 -0.5509 -0.7178 -0.2500
4 6 5 0.1661 4.0144 5.9994 5.0031 -0.6261 -0.7565 0.1304
6 4 4 0.1321 6.0057 3.9986 4.0088 -0.5645 -0.7305 0.4467
-1 -4 -9 0.1812 -1.0096 -4.0007 -8.9979 0.2260 0.9520 0.1351
-4 -2 -8 0.1644 -3.9997 -1.9997 -8.0056 0.2125 0.9753 -0.2906
-3 5 9 0.2236 -2.9826 5.0020 8.9889 -0.1224 -0.7707 -0.6178
1 4 9 0.1768 1.0096 4.0007 8.9979 -0.2260 -0.9520 -0.1351
-7 1 -3 0.1957 -6.9878 1.0018 -3.0146 0.1889 0.6093 -0.7897
-5 -1 -7 0.1565 -4.9955 -0.9992 -7.0085 0.1915 0.9156 -0.4523
-6 3 -4 0.1816 -5.9817 3.0014 -4.0139 -0.0562 0.6228 -0.7640
-4 2 -7 0.1642 -3.9863 2.0005 -7.0086 -0.1225 0.8202 -0.4789
-3 0 -9 0.1664 -2.9936 -0.0001 -9.0049 -0.0325 0.9888 -0.2649
-1 -1 -10 0.1748 -0.9989 -1.0008 -9.9999 -0.0596 0.9993 0.0061
1 -2 -10 0.1983 0.9954 -2.0015 -9.9951 -0.0671 0.9163 0.2701
5 -2 6 0.1583 4.9856 -2.0009 6.0108 0.0548 -0.7759 0.5953
4 -1 8 0.1376 3.9894 -1.0003 8.0078 0.0535 -0.9291 0.4266
0 1 10 0.1701 0.0001 1.0011 9.9978 0.1077 -0.9501 -0.1155
3 -5 7 0.1136 2.9772 -5.0002 7.0088 0.4366 -0.7249 0.5056
1 -4 9 0.1212 0.9822 -3.9993 9.0037 0.4833 -0.8288 0.2275
0 -3 10 0.1520 -0.0136 -2.9989 10.0007 0.4624 -0.8885 0.0658
-1 -3 10 0.1639 -1.0125 -2.9986 9.9987 0.5104 -0.8394 -0.0435
-3 5 -7 0.1866 -2.9772 5.0002 -7.0088 -0.4366 0.7249 -0.5056
-1 4 -9 0.2021 -0.9822 3.9993 -9.0037 -0.4833 0.8288 -0.2275
3 1 -11 0.2041 3.0038 0.9978 -10.9930 -0.4489 0.8653 0.3599
1 -7 7 0.0926 0.9726 -6.9996 7.0061 0.7101 -0.5957 0.3775
0 -6 8 0.1010 -0.0232 -5.9992 8.0032 0.6891 -0.6554 0.2158
-1 7 -7 0.2099 -0.9726 6.9996 -7.0061 -0.7101 0.5957 -0.3775
2 5 -9 0.2214 2.0179 4.9984 -8.9982 -0.7162 0.6659 0.0552
5 3 -9 0.2039 5.0077 2.9975 -8.9906 -0.6831 0.5492 0.4739
0 -8 7 0.0829 -0.0297 -7.9993 7.0048 0.8468 -0.5311 0.3135
0 -9 -5 0.1883 -0.0291 -9.0006 -4.9928 0.6998 0.6059 0.4430
1 -9 -5 0.1958 0.9698 -9.0010 -4.9907 0.6518 0.5568 0.5523
-1 -9 -5 0.1856 -1.0280 -9.0003 -4.9948 0.7479 0.6551 0.3336
-6 -5 -2 0.1917 -6.0097 -4.9984 -2.0084 0.6925 0.5590 -0.4154
-6 -3 -4 0.1603 -6.0022 -2.9986 -4.0095 0.4759 0.7151 -0.4921
-1 -7 -7 0.1753 -1.0205 -7.0005 -6.9960 0.5313 0.8113 0.2570
1 -7 -7 0.1905 0.9773 -7.0012 -6.9919 0.4352 0.7129 0.4757
0 -6 -9 0.1757 -0.0175 -6.0011 -8.9944 0.3553 0.9336 0.3351
-2 -4 -8 0.1634 -2.0088 -4.0003 -8.0001 0.2937 0.9077 0.0187
-6 -1 -6 0.1470 -5.9947 -0.9988 -6.0107 0.2592 0.8713 -0.5687
-5 1 -7 0.1418 -4.9887 1.0008 -7.0100 0.0142 0.8848 -0.5430
-2 -1 -9 0.1519 -1.9982 -1.0004 -9.0021 0.0081 0.9550 -0.1102
2 -3 -10 0.1884 1.9909 -3.0018 -9.9923 -0.0265 0.8826 0.4248
4 -5 -9 0.2255 3.9815 -5.0023 -8.9869 0.0744 0.7215 0.7271
1 0 -11 0.1845 1.0026 -0.0015 -10.9964 -0.2641 0.9790 0.1865
-2 2 -9 0.1654 -1.9879 1.9996 -9.0043 -0.2579 0.9088 -0.2462
-3 3 -8 0.1572 -2.9837 3.0001 -8.0072 -0.2789 0.8491 -0.4079
-5 4 -6 0.1689 -4.9787 4.0009 -6.0123 -0.2322 0.7451 -0.6859
1 7 -7 0.2139 1.0252 6.9990 -7.0020 -0.8062 0.4973 -0.1588

_olex2_date_sample_data_collection 2016-05-18
_olex2_submission_original_sample_id hasj160518a
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.785
####################################################################### 
# 
# 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_hasj161012a
_database_code_depnum_ccdc_archive 'CCDC 1520543'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT305_hasj161012a         
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??)            H Check
RESPONSE: This is a calcium hydride - distances too long to be recognized as bonding
;
# Added during the CSD deposition process: Friday 02 December 2016 04:36 PM
# end Validation Reply Form

_audit_creation_date             2016-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C68 H106 Ca2 N6 O2'
_chemical_formula_sum            'C68 H106 Ca2 N6 O2'
_chemical_formula_weight         1119.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca O Si '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.4825(2)
_cell_length_b                   13.02210(10)
_cell_length_c                   18.2443(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.2860(10)
_cell_angle_gamma                90
_cell_volume                     3385.44(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17845
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4220
_cell_measurement_theta_min      3.5420
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.3828
_exptl_crystal_size_mid          0.3238
_exptl_crystal_size_min          0.1131
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.100
_diffrn_reflns_theta_min         3.599
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -90.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -68.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000   60.0000 96

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000 -120.0000 74

#__ type_ start__ end____ width___ exp.time_
  5 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000    0.0000 99

#__ type_ start__ end____ width___ exp.time_
  6 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -90.0000 99

#__ type_ start__ end____ width___ exp.time_
  7 omega   94.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  8 omega   25.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -180.0000 99

#__ type_ start__ end____ width___ exp.time_
 10 omega   34.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  -90.0000 87

#__ type_ start__ end____ width___ exp.time_
 11 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 99

#__ type_ start__ end____ width___ exp.time_
 12 omega   25.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
 13 omega   32.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 14 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
 15 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000    0.0000 97

#__ type_ start__ end____ width___ exp.time_
 16 omega -116.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000 -120.0000 106

#__ type_ start__ end____ width___ exp.time_
 17 omega -116.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000   90.0000 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0721071000
_diffrn_orient_matrix_UB_12      0.0224118000
_diffrn_orient_matrix_UB_13      0.0506540000
_diffrn_orient_matrix_UB_21      0.0107831000
_diffrn_orient_matrix_UB_22      -0.1107073000
_diffrn_orient_matrix_UB_23      0.0300683000
_diffrn_orient_matrix_UB_31      0.0798301000
_diffrn_orient_matrix_UB_32      0.0351076000
_diffrn_orient_matrix_UB_33      0.0624251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5756
_reflns_number_total             6166
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²+0.9850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C15(H15), C12(H12), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C9(H9), C22(H22), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C),
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C34(H34A,H34B,
 H34C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.41010(2) 0.52590(2) 0.55080(2) 0.01577(10) Uani 1 1 d . . . . .
O1 O 0.45372(7) 0.57540(8) 0.68186(5) 0.0240(2) Uani 1 1 d . . . . .
N2 N 0.27245(8) 0.43563(9) 0.56399(6) 0.0159(2) Uani 1 1 d . . . . .
N1 N 0.29739(8) 0.65588(8) 0.51864(6) 0.0157(2) Uani 1 1 d . . . . .
N3 N 0.49339(10) 0.58446(11) 0.84055(7) 0.0293(3) Uani 1 1 d . . . . .
C3 C 0.20196(10) 0.47970(11) 0.58937(8) 0.0188(3) Uani 1 1 d . . . . .
C1 C 0.22426(10) 0.66656(11) 0.55237(7) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.18615(10) 0.58665(11) 0.59021(8) 0.0193(3) Uani 1 1 d . . . . .
C6 C 0.31726(10) 0.73930(10) 0.47265(8) 0.0173(3) Uani 1 1 d . . . . .
C11 C 0.27588(10) 0.73946(11) 0.39648(8) 0.0195(3) Uani 1 1 d . . . . .
C18 C 0.26919(10) 0.32686(11) 0.55272(8) 0.0183(3) Uani 1 1 d . . . . .
C19 C 0.21711(10) 0.28672(11) 0.48620(8) 0.0216(3) Uani 1 1 d . . . . .
C24 C 0.16623(11) 0.35652(12) 0.42543(8) 0.0247(3) Uani 1 1 d . . . . .
H24 H 0.1706 0.4283 0.4452 0.030 Uiso 1 1 calc R . . . .
C23 C 0.32117(10) 0.26069(11) 0.60556(8) 0.0213(3) Uani 1 1 d . . . . .
C7 C 0.37945(10) 0.81808(11) 0.50227(8) 0.0194(3) Uani 1 1 d . . . . .
C15 C 0.22082(11) 0.64642(12) 0.36201(8) 0.0240(3) Uani 1 1 d . . . . .
H15 H 0.2482 0.5848 0.3906 0.029 Uiso 1 1 calc R . . . .
C12 C 0.43723(11) 0.81040(11) 0.58029(8) 0.0226(3) Uani 1 1 d . . . . .
H12 H 0.4132 0.7504 0.6055 0.027 Uiso 1 1 calc R . . . .
C10 C 0.28908(10) 0.82507(12) 0.35369(8) 0.0232(3) Uani 1 1 d . . . . .
H10 H 0.2598 0.8273 0.3028 0.028 Uiso 1 1 calc R . . . .
C8 C 0.39084(11) 0.90190(11) 0.45694(9) 0.0239(3) Uani 1 1 d . . . . .
H8 H 0.4315 0.9564 0.4766 0.029 Uiso 1 1 calc R . . . .
C9 C 0.34411(11) 0.90709(12) 0.38399(9) 0.0254(3) Uani 1 1 d . . . . .
H9 H 0.3497 0.9664 0.3548 0.030 Uiso 1 1 calc R . . . .
C22 C 0.31616(12) 0.15513(12) 0.59239(9) 0.0272(3) Uani 1 1 d . . . . .
H22 H 0.3502 0.1099 0.6282 0.033 Uiso 1 1 calc R . . . .
C30 C 0.54883(11) 0.57615(13) 0.72231(9) 0.0284(3) Uani 1 1 d . . . . .
H30A H 0.5721 0.6477 0.7274 0.034 Uiso 1 1 calc R . . . .
H30B H 0.5895 0.5370 0.6941 0.034 Uiso 1 1 calc R . . . .
C27 C 0.38259(11) 0.30095(11) 0.67611(8) 0.0241(3) Uani 1 1 d . . . . .
H27 H 0.3783 0.3776 0.6755 0.029 Uiso 1 1 calc R . . . .
C4 C 0.17549(11) 0.76984(11) 0.55185(9) 0.0251(3) Uani 1 1 d . . . . .
H4A H 0.2190 0.8202 0.5789 0.038 Uiso 1 1 calc GR . . . .
H4B H 0.1205 0.7632 0.5760 0.038 Uiso 1 1 calc GR . . . .
H4C H 0.1555 0.7928 0.5003 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.55447(12) 0.52916(13) 0.79889(9) 0.0293(4) Uani 1 1 d . . . . .
H31A H 0.5353 0.4562 0.7939 0.035 Uiso 1 1 calc R . . . .
H31B H 0.6200 0.5321 0.8261 0.035 Uiso 1 1 calc R . . . .
C5 C 0.12965(11) 0.41442(12) 0.61883(10) 0.0293(4) Uani 1 1 d . . . . .
H5A H 0.0843 0.3873 0.5769 0.044 Uiso 1 1 calc GR . . . .
H5B H 0.0967 0.4566 0.6505 0.044 Uiso 1 1 calc GR . . . .
H5C H 0.1612 0.3573 0.6481 0.044 Uiso 1 1 calc GR . . . .
C20 C 0.21488(11) 0.18067(12) 0.47531(9) 0.0271(3) Uani 1 1 d . . . . .
H20 H 0.1799 0.1530 0.4307 0.032 Uiso 1 1 calc R . . . .
C21 C 0.26296(12) 0.11498(12) 0.52861(10) 0.0302(4) Uani 1 1 d . . . . .
H21 H 0.2593 0.0428 0.5212 0.036 Uiso 1 1 calc R . . . .
C33 C 0.39719(12) 0.58168(14) 0.79992(9) 0.0300(4) Uani 1 1 d . . . . .
H33A H 0.3558 0.6202 0.8278 0.036 Uiso 1 1 calc R . . . .
H33B H 0.3749 0.5097 0.7947 0.036 Uiso 1 1 calc R . . . .
C14 C 0.42994(13) 0.90521(12) 0.62837(9) 0.0303(4) Uani 1 1 d . . . . .
H14A H 0.4554 0.9650 0.6061 0.045 Uiso 1 1 calc GR . . . .
H14B H 0.4658 0.8937 0.6785 0.045 Uiso 1 1 calc GR . . . .
H14C H 0.3640 0.9177 0.6313 0.045 Uiso 1 1 calc GR . . . .
C32 C 0.39300(12) 0.62899(13) 0.72379(9) 0.0293(4) Uani 1 1 d . . . . .
H32A H 0.3276 0.6265 0.6962 0.035 Uiso 1 1 calc R . . . .
H32B H 0.4122 0.7019 0.7294 0.035 Uiso 1 1 calc R . . . .
C17 C 0.23141(13) 0.63004(14) 0.28077(9) 0.0332(4) Uani 1 1 d . . . . .
H17A H 0.1997 0.6858 0.2500 0.050 Uiso 1 1 calc GR . . . .
H17B H 0.2031 0.5642 0.2630 0.050 Uiso 1 1 calc GR . . . .
H17C H 0.2982 0.6297 0.2773 0.050 Uiso 1 1 calc GR . . . .
C16 C 0.11702(12) 0.65051(14) 0.36808(10) 0.0331(4) Uani 1 1 d . . . . .
H16A H 0.1108 0.6483 0.4207 0.050 Uiso 1 1 calc GR . . . .
H16B H 0.0843 0.5916 0.3419 0.050 Uiso 1 1 calc GR . . . .
H16C H 0.0893 0.7143 0.3455 0.050 Uiso 1 1 calc GR . . . .
C25 C 0.21378(14) 0.35388(15) 0.35725(10) 0.0377(4) Uani 1 1 d . . . . .
H25A H 0.2784 0.3787 0.3710 0.057 Uiso 1 1 calc GR . . . .
H25B H 0.1792 0.3980 0.3182 0.057 Uiso 1 1 calc GR . . . .
H25C H 0.2142 0.2833 0.3388 0.057 Uiso 1 1 calc GR . . . .
C13 C 0.54011(12) 0.78894(13) 0.57584(9) 0.0309(4) Uani 1 1 d . . . . .
H13A H 0.5447 0.7237 0.5499 0.046 Uiso 1 1 calc GR . . . .
H13B H 0.5771 0.7849 0.6263 0.046 Uiso 1 1 calc GR . . . .
H13C H 0.5644 0.8445 0.5484 0.046 Uiso 1 1 calc GR . . . .
C34 C 0.49950(16) 0.54184(16) 0.91488(9) 0.0424(5) Uani 1 1 d . . . . .
H34A H 0.4791 0.4700 0.9112 0.064 Uiso 1 1 calc GR . . . .
H34B H 0.4590 0.5812 0.9422 0.064 Uiso 1 1 calc GR . . . .
H34C H 0.5646 0.5456 0.9413 0.064 Uiso 1 1 calc GR . . . .
C29 C 0.48544(12) 0.27154(16) 0.67844(11) 0.0385(4) Uani 1 1 d . . . . .
H29A H 0.4917 0.1966 0.6803 0.058 Uiso 1 1 calc GR . . . .
H29B H 0.5242 0.3015 0.7228 0.058 Uiso 1 1 calc GR . . . .
H29C H 0.5063 0.2976 0.6337 0.058 Uiso 1 1 calc GR . . . .
C28 C 0.34955(14) 0.26269(16) 0.74604(10) 0.0411(4) Uani 1 1 d . . . . .
H28A H 0.2832 0.2801 0.7433 0.062 Uiso 1 1 calc GR . . . .
H28B H 0.3868 0.2953 0.7900 0.062 Uiso 1 1 calc GR . . . .
H28C H 0.3574 0.1880 0.7498 0.062 Uiso 1 1 calc GR . . . .
C26 C 0.06250(13) 0.32955(18) 0.40362(12) 0.0480(5) Uani 1 1 d . . . . .
H26A H 0.0562 0.2597 0.3834 0.072 Uiso 1 1 calc GR . . . .
H26B H 0.0321 0.3781 0.3658 0.072 Uiso 1 1 calc GR . . . .
H26C H 0.0326 0.3336 0.4476 0.072 Uiso 1 1 calc GR . . . .
H2 H 0.1356(12) 0.6062(13) 0.6139(10) 0.020(4) Uiso 1 1 d . . . . .
H H 0.5587(17) 0.4959(19) 0.5636(14) 0.058(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
Ca1 Ca1 3.5208(5) 3_666 ?
Ca1 O1 2.4479(10) . ?
Ca1 N2 2.3633(11) . ?
Ca1 N1 2.3519(11) . ?
Ca1 H 2.16(2) . ?
O1 C30 1.4419(19) . ?
O1 C32 1.4442(19) . ?
N2 C3 1.3246(18) . ?
N2 C18 1.4309(18) . ?
N1 C1 1.3238(18) . ?
N1 C6 1.4328(17) . ?
N3 C31 1.456(2) . ?
N3 C33 1.457(2) . ?
N3 C34 1.453(2) . ?
C3 C2 1.412(2) . ?
C3 C5 1.520(2) . ?
C1 C2 1.414(2) . ?
C1 C4 1.5184(19) . ?
C2 H2 0.950(18) . ?
C6 C11 1.412(2) . ?
C6 C7 1.408(2) . ?
C11 C15 1.523(2) . ?
C11 C10 1.394(2) . ?
C18 C19 1.410(2) . ?
C18 C23 1.407(2) . ?
C19 C24 1.519(2) . ?
C19 C20 1.395(2) . ?
C24 H24 1.0000 . ?
C24 C25 1.526(2) . ?
C24 C26 1.525(2) . ?
C23 C22 1.395(2) . ?
C23 C27 1.521(2) . ?
C7 C12 1.520(2) . ?
C7 C8 1.397(2) . ?
C15 H15 1.0000 . ?
C15 C17 1.532(2) . ?
C15 C16 1.528(2) . ?
C12 H12 1.0000 . ?
C12 C14 1.529(2) . ?
C12 C13 1.532(2) . ?
C10 H10 0.9500 . ?
C10 C9 1.387(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(2) . ?
C9 H9 0.9500 . ?
C22 H22 0.9500 . ?
C22 C21 1.379(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.514(2) . ?
C27 H27 1.0000 . ?
C27 C29 1.531(2) . ?
C27 C28 1.524(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C21 1.386(2) . ?
C21 H21 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.511(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ca1 Ca1 H 37.4(7) 3_666 . ?
O1 Ca1 Ca1 118.59(3) . 3_666 ?
O1 Ca1 H 82.1(7) . . ?
N2 Ca1 Ca1 132.45(3) . 3_666 ?
N2 Ca1 O1 96.13(4) . . ?
N2 Ca1 H 137.9(7) . . ?
N1 Ca1 Ca1 123.51(3) . 3_666 ?
N1 Ca1 O1 95.79(4) . . ?
N1 Ca1 N2 79.80(4) . . ?
N1 Ca1 H 142.3(7) . . ?
C30 O1 Ca1 123.92(9) . . ?
C30 O1 C32 110.00(12) . . ?
C32 O1 Ca1 124.70(9) . . ?
C3 N2 Ca1 122.47(9) . . ?
C3 N2 C18 118.12(11) . . ?
C18 N2 Ca1 118.98(8) . . ?
C1 N1 Ca1 122.46(9) . . ?
C1 N1 C6 116.98(11) . . ?
C6 N1 Ca1 119.25(8) . . ?
C31 N3 C33 109.71(13) . . ?
C34 N3 C31 110.91(14) . . ?
C34 N3 C33 111.01(14) . . ?
N2 C3 C2 124.59(13) . . ?
N2 C3 C5 120.27(12) . . ?
C2 C3 C5 115.13(13) . . ?
N1 C1 C2 124.34(13) . . ?
N1 C1 C4 120.00(12) . . ?
C2 C1 C4 115.66(12) . . ?
C3 C2 C1 129.96(13) . . ?
C3 C2 H2 114.2(10) . . ?
C1 C2 H2 115.1(10) . . ?
C11 C6 N1 118.90(12) . . ?
C7 C6 N1 120.62(12) . . ?
C7 C6 C11 120.45(13) . . ?
C6 C11 C15 120.27(13) . . ?
C10 C11 C6 118.43(13) . . ?
C10 C11 C15 121.27(13) . . ?
C19 C18 N2 119.31(13) . . ?
C23 C18 N2 120.53(13) . . ?
C23 C18 C19 120.08(13) . . ?
C18 C19 C24 121.44(13) . . ?
C20 C19 C18 119.00(14) . . ?
C20 C19 C24 119.52(14) . . ?
C19 C24 H24 107.8 . . ?
C19 C24 C25 110.54(13) . . ?
C19 C24 C26 112.31(14) . . ?
C25 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C26 C24 C25 110.42(15) . . ?
C18 C23 C27 121.95(13) . . ?
C22 C23 C18 118.72(14) . . ?
C22 C23 C27 119.33(14) . . ?
C6 C7 C12 121.26(12) . . ?
C8 C7 C6 118.50(13) . . ?
C8 C7 C12 120.16(13) . . ?
C11 C15 H15 107.1 . . ?
C11 C15 C17 112.01(13) . . ?
C11 C15 C16 113.06(13) . . ?
C17 C15 H15 107.1 . . ?
C16 C15 H15 107.1 . . ?
C16 C15 C17 110.17(13) . . ?
C7 C12 H12 107.6 . . ?
C7 C12 C14 113.65(12) . . ?
C7 C12 C13 109.89(13) . . ?
C14 C12 H12 107.6 . . ?
C14 C12 C13 110.19(13) . . ?
C13 C12 H12 107.6 . . ?
C11 C10 H10 119.4 . . ?
C9 C10 C11 121.28(13) . . ?
C9 C10 H10 119.4 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.25(14) . . ?
C9 C8 H8 119.4 . . ?
C10 C9 H9 120.2 . . ?
C8 C9 C10 119.57(14) . . ?
C8 C9 H9 120.2 . . ?
C23 C22 H22 119.2 . . ?
C21 C22 C23 121.54(15) . . ?
C21 C22 H22 119.2 . . ?
O1 C30 H30A 109.4 . . ?
O1 C30 H30B 109.4 . . ?
O1 C30 C31 111.02(13) . . ?
H30A C30 H30B 108.0 . . ?
C31 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
C23 C27 H27 107.9 . . ?
C23 C27 C29 110.86(13) . . ?
C23 C27 C28 111.84(13) . . ?
C29 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C28 C27 C29 110.14(14) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C31 C30 110.13(13) . . ?
N3 C31 H31A 109.6 . . ?
N3 C31 H31B 109.6 . . ?
C30 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.02(15) . . ?
C21 C20 H20 119.5 . . ?
C22 C21 C20 119.55(14) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
N3 C33 H33A 109.8 . . ?
N3 C33 H33B 109.8 . . ?
N3 C33 C32 109.59(13) . . ?
H33A C33 H33B 108.2 . . ?
C32 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C32 C33 111.20(13) . . ?
O1 C32 H32A 109.4 . . ?
O1 C32 H32B 109.4 . . ?
C33 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C30 C31 -135.95(11) . . . . ?
Ca1 O1 C32 C33 135.40(11) . . . . ?
Ca1 N2 C3 C2 19.94(19) . . . . ?
Ca1 N2 C3 C5 -161.44(11) . . . . ?
Ca1 N2 C18 C19 -104.50(12) . . . . ?
Ca1 N2 C18 C23 72.26(14) . . . . ?
Ca1 N1 C1 C2 -23.26(19) . . . . ?
Ca1 N1 C1 C4 156.88(10) . . . . ?
Ca1 N1 C6 C11 102.42(12) . . . . ?
Ca1 N1 C6 C7 -75.49(14) . . . . ?
O1 C30 C31 N3 -57.80(17) . . . . ?
N2 C3 C2 C1 15.2(2) . . . . ?
N2 C18 C19 C24 1.5(2) . . . . ?
N2 C18 C19 C20 179.48(13) . . . . ?
N2 C18 C23 C22 -179.90(13) . . . . ?
N2 C18 C23 C27 -0.1(2) . . . . ?
N1 C1 C2 C3 -13.4(2) . . . . ?
N1 C6 C11 C15 -7.3(2) . . . . ?
N1 C6 C11 C10 174.55(12) . . . . ?
N1 C6 C7 C12 8.3(2) . . . . ?
N1 C6 C7 C8 -174.94(13) . . . . ?
N3 C33 C32 O1 58.63(18) . . . . ?
C3 N2 C18 C19 82.79(16) . . . . ?
C3 N2 C18 C23 -100.45(16) . . . . ?
C1 N1 C6 C11 -90.30(16) . . . . ?
C1 N1 C6 C7 91.79(16) . . . . ?
C6 N1 C1 C2 169.90(13) . . . . ?
C6 N1 C1 C4 -9.96(19) . . . . ?
C6 C11 C15 C17 -146.15(14) . . . . ?
C6 C11 C15 C16 88.66(16) . . . . ?
C6 C11 C10 C9 2.2(2) . . . . ?
C6 C7 C12 C14 -129.26(14) . . . . ?
C6 C7 C12 C13 106.75(16) . . . . ?
C6 C7 C8 C9 -1.5(2) . . . . ?
C11 C6 C7 C12 -169.59(13) . . . . ?
C11 C6 C7 C8 7.2(2) . . . . ?
C11 C10 C9 C8 3.4(2) . . . . ?
C18 N2 C3 C2 -167.62(13) . . . . ?
C18 N2 C3 C5 11.0(2) . . . . ?
C18 C19 C24 C25 110.29(16) . . . . ?
C18 C19 C24 C26 -125.89(16) . . . . ?
C18 C19 C20 C21 -0.1(2) . . . . ?
C18 C23 C22 C21 1.1(2) . . . . ?
C18 C23 C27 C29 -118.85(16) . . . . ?
C18 C23 C27 C28 117.80(16) . . . . ?
C19 C18 C23 C22 -3.2(2) . . . . ?
C19 C18 C23 C27 176.61(13) . . . . ?
C19 C20 C21 C22 -2.0(2) . . . . ?
C24 C19 C20 C21 177.96(14) . . . . ?
C23 C18 C19 C24 -175.32(13) . . . . ?
C23 C18 C19 C20 2.7(2) . . . . ?
C23 C22 C21 C20 1.5(2) . . . . ?
C7 C6 C11 C15 170.60(13) . . . . ?
C7 C6 C11 C10 -7.5(2) . . . . ?
C7 C8 C9 C10 -3.8(2) . . . . ?
C15 C11 C10 C9 -175.92(14) . . . . ?
C12 C7 C8 C9 175.34(14) . . . . ?
C10 C11 C15 C17 31.9(2) . . . . ?
C10 C11 C15 C16 -93.25(17) . . . . ?
C8 C7 C12 C14 54.0(2) . . . . ?
C8 C7 C12 C13 -69.97(17) . . . . ?
C22 C23 C27 C29 60.93(19) . . . . ?
C22 C23 C27 C28 -62.42(19) . . . . ?
C30 O1 C32 C33 -57.61(17) . . . . ?
C27 C23 C22 C21 -178.72(14) . . . . ?
C4 C1 C2 C3 166.45(15) . . . . ?
C31 N3 C33 C32 -58.54(17) . . . . ?
C5 C3 C2 C1 -163.46(15) . . . . ?
C20 C19 C24 C25 -67.72(19) . . . . ?
C20 C19 C24 C26 56.1(2) . . . . ?
C33 N3 C31 C30 58.30(17) . . . . ?
C32 O1 C30 C31 56.93(17) . . . . ?
C34 N3 C31 C30 -178.71(14) . . . . ?
C34 N3 C33 C32 178.53(15) . . . . ?

_shelx_SHELXL_version_number     2014/7

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -7 7 0.1209 -0.0080 -7.0046 6.9848 0.1974 0.9854 0.1895
-9 3 5 0.1043 -9.0114 2.9931 4.9942 0.9698 -0.2784 -0.3025
4 -4 -10 0.1161 4.0096 -3.9886 -9.9911 -0.8846 0.1844 -0.4436
-5 -3 -8 0.2082 -5.0005 -2.9919 -7.9955 -0.1115 0.0369 -1.0034
-7 3 8 0.1041 -7.0115 2.9905 7.9914 0.9774 -0.1664 0.0441
-5 4 9 0.1280 -5.0098 3.9894 8.9919 0.9061 -0.2253 0.3014
1 4 10 0.1817 0.9955 3.9892 9.9928 0.5238 -0.1304 0.8433
9 0 1 0.1395 9.0083 0.0001 1.0019 -0.5988 0.1272 0.7817
9 -3 -5 0.0792 9.0114 -2.9931 -4.9942 -0.9698 0.2784 0.3025
-7 3 7 0.1076 -7.0108 2.9914 6.9925 0.9268 -0.1965 -0.0181
-8 0 8 0.0517 -8.0138 -0.0087 7.9880 0.9823 0.1547 -0.1414
9 1 -5 0.0799 9.0131 1.0056 -4.9901 -0.8801 -0.1642 0.4433
-6 1 10 0.0980 -6.0128 0.9893 9.9874 0.9616 0.1259 0.1782
8 0 -9 0.0599 8.0145 0.0097 -8.9868 -1.0329 -0.1849 0.0791
6 -1 -10 0.0711 6.0128 -0.9893 -9.9874 -0.9616 -0.1259 -0.1782
5 3 -10 0.1009 5.0135 3.0093 -9.9837 -0.7998 -0.5793 -0.1173
8 4 -4 0.1108 8.0126 4.0036 -3.9886 -0.6901 -0.4768 0.5312
6 3 6 0.1822 6.0030 2.9940 5.9981 -0.0619 -0.0864 0.9588
-1 -1 12 0.1669 -1.0101 -1.0114 11.9847 0.6572 0.4614 0.6320
-8 -4 1 0.1550 -8.0105 -4.0007 0.9920 0.5382 0.3864 -0.7180
-6 -3 -6 0.2071 -6.0030 -2.9940 -5.9981 0.0619 0.0864 -0.9588
7 0 7 0.1667 7.0020 -0.0059 6.9943 -0.1507 0.2865 0.9954
3 7 5 0.1575 3.0024 6.9933 5.0023 0.1936 -0.5914 0.7975
-5 6 -3 0.1725 -5.0003 6.0004 -2.9921 0.3435 -0.8082 -0.3753
-4 -5 -6 0.1887 -4.0018 -4.9931 -5.9995 -0.1272 0.3292 -0.8693
0 -8 -3 0.1756 -0.0012 -7.9946 -3.0046 -0.3313 0.7947 -0.4683
-5 6 7 0.1480 -5.0075 5.9907 6.9963 0.8497 -0.5069 0.2473
4 -6 -7 0.1333 4.0065 -5.9909 -6.9966 -0.7776 0.4961 -0.3272
-1 -5 -9 0.1693 -0.9966 -4.9899 -8.9950 -0.4956 0.2712 -0.8163
9 -1 -6 0.0623 9.0130 -0.9928 -5.9910 -0.9756 0.0270 0.3107
8 -2 -8 0.0571 8.0130 -1.9907 -7.9900 -1.0271 0.0665 0.0710
5 -2 -10 0.0833 5.0114 -1.9891 -9.9887 -0.9119 -0.0261 -0.2933
5 0 -11 0.0871 5.0130 0.0112 -10.9855 -0.9177 -0.2775 -0.2852
7 1 -9 0.0589 7.0140 1.0092 -8.9862 -0.9383 -0.3063 0.0344
-7 -1 9 0.0663 -7.0140 -1.0092 8.9862 0.9383 0.3063 -0.0344
8 2 -7 0.0751 8.0139 2.0071 -6.9871 -0.8868 -0.3459 0.2740
-2 6 -7 0.1741 -1.9944 6.0046 -6.9865 -0.0755 -0.8963 -0.3845
-1 8 -5 0.1940 -0.9940 8.0022 -4.9864 -0.0016 -1.0466 -0.1097
-7 3 -4 0.1971 -7.0029 3.0021 -3.9947 0.3699 -0.5280 -0.7030
-2 8 4 0.1699 -2.0015 7.9934 4.0028 0.5262 -0.7862 0.3707

_olex2_date_sample_data_collection 2016-10-12
_olex2_submission_original_sample_id hasj161012a
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hasj160615a
_database_code_depnum_ccdc_archive 'CCDC 1520542'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_hasj160615a         
;
PROBLEM: Hirshfeld Test Diff for    Si1    --  C30     ..        5.3 s.u.
RESPONSE: Slight disorder in TMS group - not resolved
;
# Added during the CSD deposition process: Friday 02 December 2016 04:36 PM
# end Validation Reply Form

_audit_creation_date             2016-08-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H69 Ca N3 O2 Si2, C3 H3'
_chemical_formula_sum            'C42 H72 Ca N3 O2 Si2'
_chemical_formula_weight         747.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca Si O '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.68700(18)
_cell_length_b                   18.0806(2)
_cell_length_c                   21.8110(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.3719(17)
_cell_angle_gamma                90
_cell_volume                     4443.95(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26866
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6060
_cell_measurement_theta_min      3.8780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.4381
_exptl_crystal_size_mid          0.2622
_exptl_crystal_size_min          0.1163
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44083
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.116
_diffrn_reflns_theta_min         3.923
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -112.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -68.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
  3 omega  -68.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -180.0000 96

#__ type_ start__ end____ width___ exp.time_
  4 omega   82.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  120.0000 96

#__ type_ start__ end____ width___ exp.time_
  5 omega   78.00  176.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  -60.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega   34.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
  7 omega   82.00  177.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
  8 omega   36.00  134.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   30.0000 98

#__ type_ start__ end____ width___ exp.time_
  9 omega   31.00  130.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  150.0000 99

#__ type_ start__ end____ width___ exp.time_
 10 omega   34.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  150.0000 87

#__ type_ start__ end____ width___ exp.time_
 11 omega   94.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000  150.0000 84

#__ type_ start__ end____ width___ exp.time_
 12 omega   94.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 13 omega   32.00  137.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
 14 omega -116.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000 -150.0000 106

#__ type_ start__ end____ width___ exp.time_
 15 omega -112.00  -15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   90.0000 97

#__ type_ start__ end____ width___ exp.time_
 16 omega -116.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000  -60.0000 106

#__ type_ start__ end____ width___ exp.time_
 17 omega   78.00  144.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
 18 omega   82.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000   30.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0987632000
_diffrn_orient_matrix_UB_12      0.0439499000
_diffrn_orient_matrix_UB_13      0.0185312000
_diffrn_orient_matrix_UB_21      0.0717612000
_diffrn_orient_matrix_UB_22      0.0718293000
_diffrn_orient_matrix_UB_23      0.0017756000
_diffrn_orient_matrix_UB_31      -0.0614081000
_diffrn_orient_matrix_UB_32      0.0132823000
_diffrn_orient_matrix_UB_33      -0.0708190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7716
_reflns_number_total             8111
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+1.1370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0982
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C15(H15), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C20(H20), C9(H9), C21(H21), C22(H22), C8(H8), C10(H10), C40(H40),
 C42(H42), C41(H41)
2.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C33(H33A,H33B,H33C),
 C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C29(H29A,
 H29B,H29C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C35(H35A,H35B,H35C),
 C25(H25A,H25B,H25C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.71929(2) 0.70247(2) 0.71697(2) 0.01612(8) Uani 1 1 d . . . . .
Si2 Si 0.42257(3) 0.75170(2) 0.63889(2) 0.02043(10) Uani 1 1 d . . . . .
Si1 Si 0.51137(3) 0.62144(2) 0.58612(2) 0.02094(10) Uani 1 1 d . . . . .
O2 O 0.89302(8) 0.65940(5) 0.67772(5) 0.0229(2) Uani 1 1 d . . . . .
O1 O 0.77133(9) 0.57449(5) 0.73897(5) 0.0254(2) Uani 1 1 d . . . . .
N2 N 0.81439(9) 0.82127(6) 0.73924(5) 0.0168(2) Uani 1 1 d . . . . .
N1 N 0.73236(10) 0.71850(6) 0.83034(5) 0.0176(2) Uani 1 1 d . . . . .
N3 N 0.53590(10) 0.69177(6) 0.64045(5) 0.0199(2) Uani 1 1 d . . . . .
C6 C 0.73275(12) 0.65339(7) 0.86843(6) 0.0183(3) Uani 1 1 d . . . . .
C23 C 0.85398(12) 0.87375(7) 0.64223(6) 0.0191(3) Uani 1 1 d . . . . .
C11 C 0.84363(12) 0.62310(7) 0.90220(6) 0.0197(3) Uani 1 1 d . . . . .
C2 C 0.72894(11) 0.85267(7) 0.82587(6) 0.0184(3) Uani 1 1 d . . . . .
H2 H 0.6952 0.8938 0.8419 0.022 Uiso 1 1 calc R . . . .
C18 C 0.89564(11) 0.84563(7) 0.70441(6) 0.0175(3) Uani 1 1 d . . . . .
C20 C 1.09726(12) 0.85674(7) 0.69627(7) 0.0213(3) Uani 1 1 d . . . . .
H20 H 1.1801 0.8504 0.7143 0.026 Uiso 1 1 calc R . . . .
C9 C 0.74073(13) 0.51775(7) 0.93158(6) 0.0220(3) Uani 1 1 d . . . . .
H9 H 0.7434 0.4711 0.9520 0.026 Uiso 1 1 calc R . . . .
C3 C 0.78669(11) 0.87006(7) 0.77877(6) 0.0175(3) Uani 1 1 d . . . . .
C21 C 1.05693(12) 0.88482(7) 0.63513(7) 0.0221(3) Uani 1 1 d . . . . .
H21 H 1.1117 0.8979 0.6116 0.026 Uiso 1 1 calc R . . . .
C7 C 0.62688(12) 0.61676(7) 0.86931(6) 0.0202(3) Uani 1 1 d . . . . .
C1 C 0.71308(11) 0.78404(7) 0.85311(6) 0.0184(3) Uani 1 1 d . . . . .
C22 C 0.93635(12) 0.89355(7) 0.60875(6) 0.0219(3) Uani 1 1 d . . . . .
H22 H 0.9089 0.9134 0.5671 0.026 Uiso 1 1 calc R . . . .
C8 C 0.63319(12) 0.54897(8) 0.90068(6) 0.0221(3) Uani 1 1 d . . . . .
H8 H 0.5619 0.5238 0.9008 0.027 Uiso 1 1 calc R . . . .
C10 C 0.84506(12) 0.55514(7) 0.93256(6) 0.0210(3) Uani 1 1 d . . . . .
H10 H 0.9190 0.5339 0.9544 0.025 Uiso 1 1 calc R . . . .
C27 C 0.72258(12) 0.88117(8) 0.60935(6) 0.0226(3) Uani 1 1 d . . . . .
H27 H 0.6769 0.8645 0.6397 0.027 Uiso 1 1 calc R . . . .
C12 C 0.50456(12) 0.64930(8) 0.83941(7) 0.0232(3) Uani 1 1 d . . . . .
H12 H 0.5159 0.6991 0.8219 0.028 Uiso 1 1 calc R . . . .
C36 C 0.93753(13) 0.68607(8) 0.62609(7) 0.0276(3) Uani 1 1 d . . . . .
H36A H 0.9133 0.6522 0.5899 0.041 Uiso 1 1 calc GR . . . .
H36B H 1.0243 0.6887 0.6400 0.041 Uiso 1 1 calc GR . . . .
H36C H 0.9052 0.7354 0.6134 0.041 Uiso 1 1 calc GR . . . .
C19 C 1.01860(12) 0.83759(7) 0.73174(6) 0.0197(3) Uani 1 1 d . . . . .
C15 C 0.95930(12) 0.66491(8) 0.90764(7) 0.0236(3) Uani 1 1 d . . . . .
H15 H 0.9548 0.6878 0.8654 0.028 Uiso 1 1 calc R . . . .
C5 C 0.82227(13) 0.95058(7) 0.77712(7) 0.0234(3) Uani 1 1 d . . . . .
H5A H 0.9074 0.9558 0.7974 0.035 Uiso 1 1 calc GR . . . .
H5B H 0.7773 0.9807 0.8000 0.035 Uiso 1 1 calc GR . . . .
H5C H 0.8052 0.9673 0.7329 0.035 Uiso 1 1 calc GR . . . .
C4 C 0.67202(14) 0.79139(8) 0.91342(7) 0.0249(3) Uani 1 1 d . . . . .
H4A H 0.5877 0.8047 0.9023 0.037 Uiso 1 1 calc GR . . . .
H4B H 0.7184 0.8300 0.9405 0.037 Uiso 1 1 calc GR . . . .
H4C H 0.6835 0.7442 0.9363 0.037 Uiso 1 1 calc GR . . . .
C24 C 1.06785(12) 0.80599(8) 0.79800(7) 0.0246(3) Uani 1 1 d . . . . .
H24 H 0.9995 0.7961 0.8164 0.029 Uiso 1 1 calc R . . . .
C33 C 0.27413(13) 0.70628(8) 0.63215(7) 0.0275(3) Uani 1 1 d . . . . .
H33A H 0.2483 0.6804 0.5913 0.041 Uiso 1 1 calc GR . . . .
H33B H 0.2155 0.7441 0.6347 0.041 Uiso 1 1 calc GR . . . .
H33C H 0.2816 0.6708 0.6669 0.041 Uiso 1 1 calc GR . . . .
C32 C 0.42131(14) 0.64749(9) 0.50351(7) 0.0298(3) Uani 1 1 d . . . . .
H32A H 0.3425 0.6644 0.5052 0.045 Uiso 1 1 calc GR . . . .
H32B H 0.4131 0.6043 0.4755 0.045 Uiso 1 1 calc GR . . . .
H32C H 0.4617 0.6873 0.4870 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.43593(13) 0.66010(9) 0.89005(7) 0.0273(3) Uani 1 1 d . . . . .
H14A H 0.4181 0.6117 0.9056 0.041 Uiso 1 1 calc GR . . . .
H14B H 0.3617 0.6865 0.8712 0.041 Uiso 1 1 calc GR . . . .
H14C H 0.4843 0.6890 0.9256 0.041 Uiso 1 1 calc GR . . . .
C38 C 0.89677(13) 0.56234(8) 0.75179(7) 0.0284(3) Uani 1 1 d . . . . .
H38A H 0.9150 0.5093 0.7607 0.034 Uiso 1 1 calc R . . . .
H38B H 0.9392 0.5913 0.7895 0.034 Uiso 1 1 calc R . . . .
C13 C 0.43147(13) 0.60210(9) 0.78472(7) 0.0297(3) Uani 1 1 d . . . . .
H13A H 0.4656 0.6055 0.7483 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.3494 0.6201 0.7723 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.4326 0.5505 0.7985 0.044 Uiso 1 1 calc GR . . . .
C28 C 0.68849(13) 0.83127(9) 0.55039(7) 0.0277(3) Uani 1 1 d . . . . .
H28A H 0.7366 0.8443 0.5214 0.042 Uiso 1 1 calc GR . . . .
H28B H 0.6043 0.8382 0.5287 0.042 Uiso 1 1 calc GR . . . .
H28C H 0.7028 0.7795 0.5634 0.042 Uiso 1 1 calc GR . . . .
C30 C 0.43249(14) 0.53896(8) 0.60909(7) 0.0299(3) Uani 1 1 d . . . . .
H30A H 0.4796 0.5190 0.6497 0.045 Uiso 1 1 calc GR . . . .
H30B H 0.4225 0.5008 0.5762 0.045 Uiso 1 1 calc GR . . . .
H30C H 0.3545 0.5543 0.6133 0.045 Uiso 1 1 calc GR . . . .
C31 C 0.65344(13) 0.58338(9) 0.57384(7) 0.0316(3) Uani 1 1 d . . . . .
H31A H 0.6977 0.6232 0.5600 0.047 Uiso 1 1 calc GR . . . .
H31B H 0.6351 0.5446 0.5413 0.047 Uiso 1 1 calc GR . . . .
H31C H 0.7015 0.5625 0.6139 0.047 Uiso 1 1 calc GR . . . .
C16 C 1.06960(13) 0.61509(9) 0.92495(8) 0.0318(3) Uani 1 1 d . . . . .
H16A H 1.0810 0.5961 0.9682 0.048 Uiso 1 1 calc GR . . . .
H16B H 1.1395 0.6438 0.9226 0.048 Uiso 1 1 calc GR . . . .
H16C H 1.0587 0.5736 0.8951 0.048 Uiso 1 1 calc GR . . . .
C29 C 0.68815(14) 0.96140(9) 0.59089(7) 0.0296(3) Uani 1 1 d . . . . .
H29A H 0.7068 0.9923 0.6292 0.044 Uiso 1 1 calc GR . . . .
H29B H 0.6029 0.9641 0.5702 0.044 Uiso 1 1 calc GR . . . .
H29C H 0.7327 0.9791 0.5615 0.044 Uiso 1 1 calc GR . . . .
C34 C 0.38958(13) 0.82165(9) 0.57198(8) 0.0301(3) Uani 1 1 d . . . . .
H34A H 0.4524 0.8591 0.5801 0.045 Uiso 1 1 calc GR . . . .
H34B H 0.3132 0.8455 0.5695 0.045 Uiso 1 1 calc GR . . . .
H34C H 0.3861 0.7965 0.5317 0.045 Uiso 1 1 calc GR . . . .
C40 C 0.01832(15) 0.44293(9) 0.54393(8) 0.0344(3) Uani 1 1 d . . . . .
H40 H 0.0309 0.4039 0.5741 0.041 Uiso 1 1 calc R . . . .
C39 C 0.70839(14) 0.51368(8) 0.75640(7) 0.0276(3) Uani 1 1 d . . . . .
H39A H 0.7426 0.5018 0.8014 0.041 Uiso 1 1 calc GR . . . .
H39B H 0.7148 0.4706 0.7303 0.041 Uiso 1 1 calc GR . . . .
H39C H 0.6246 0.5270 0.7495 0.041 Uiso 1 1 calc GR . . . .
C37 C 0.93603(13) 0.58602(8) 0.69459(7) 0.0265(3) Uani 1 1 d . . . . .
H37A H 1.0237 0.5852 0.7044 0.032 Uiso 1 1 calc R . . . .
H37B H 0.9039 0.5518 0.6587 0.032 Uiso 1 1 calc R . . . .
C35 C 0.45370(14) 0.81045(9) 0.71272(8) 0.0309(3) Uani 1 1 d . . . . .
H35A H 0.4458 0.7803 0.7487 0.046 Uiso 1 1 calc GR . . . .
H35B H 0.3969 0.8515 0.7062 0.046 Uiso 1 1 calc GR . . . .
H35C H 0.5346 0.8302 0.7217 0.046 Uiso 1 1 calc GR . . . .
C25 C 1.13101(14) 0.73285(9) 0.79523(8) 0.0321(3) Uani 1 1 d . . . . .
H25A H 1.0759 0.6981 0.7679 0.048 Uiso 1 1 calc GR . . . .
H25B H 1.1586 0.7122 0.8382 0.048 Uiso 1 1 calc GR . . . .
H25C H 1.1991 0.7412 0.7779 0.048 Uiso 1 1 calc GR . . . .
C17 C 0.97511(14) 0.72756(9) 0.95680(8) 0.0330(3) Uani 1 1 d . . . . .
H17A H 0.9090 0.7625 0.9438 0.049 Uiso 1 1 calc GR . . . .
H17B H 1.0500 0.7534 0.9595 0.049 Uiso 1 1 calc GR . . . .
H17C H 0.9765 0.7067 0.9985 0.049 Uiso 1 1 calc GR . . . .
C42 C 0.09586(15) 0.53336(10) 0.48527(8) 0.0394(4) Uani 1 1 d . . . . .
H42 H 0.1618 0.5563 0.4753 0.047 Uiso 1 1 calc R . . . .
C41 C 0.11358(15) 0.47628(10) 0.52900(8) 0.0380(4) Uani 1 1 d . . . . .
H41 H 0.1919 0.4599 0.5489 0.046 Uiso 1 1 calc R . . . .
C26 C 1.15239(16) 0.85938(10) 0.84262(7) 0.0358(4) Uani 1 1 d . . . . .
H26A H 1.2225 0.8677 0.8269 0.054 Uiso 1 1 calc GR . . . .
H26B H 1.1768 0.8380 0.8854 0.054 Uiso 1 1 calc GR . . . .
H26C H 1.1119 0.9066 0.8441 0.054 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O2 2.5266(9) . ?
Ca1 O1 2.4083(10) . ?
Ca1 N2 2.4082(11) . ?
Ca1 N1 2.4539(11) . ?
Ca1 N3 2.3494(11) . ?
Si2 N3 1.7045(11) . ?
Si2 C33 1.8896(15) . ?
Si2 C34 1.8920(15) . ?
Si2 C35 1.8824(15) . ?
Si1 N3 1.7097(12) . ?
Si1 C32 1.8898(15) . ?
Si1 C30 1.8893(15) . ?
Si1 C31 1.8810(15) . ?
O2 C36 1.4429(17) . ?
O2 C37 1.4319(17) . ?
O1 C38 1.4347(18) . ?
O1 C39 1.4293(17) . ?
N2 C18 1.4335(16) . ?
N2 C3 1.3320(17) . ?
N1 C6 1.4401(16) . ?
N1 C1 1.3270(18) . ?
C6 C11 1.4197(19) . ?
C6 C7 1.4080(19) . ?
C23 C18 1.4088(19) . ?
C23 C22 1.4003(18) . ?
C23 C27 1.5188(19) . ?
C11 C10 1.3938(19) . ?
C11 C15 1.5257(19) . ?
C2 H2 0.9500 . ?
C2 C3 1.4062(18) . ?
C2 C1 1.4091(18) . ?
C18 C19 1.4098(19) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(2) . ?
C20 C19 1.3932(18) . ?
C9 H9 0.9500 . ?
C9 C8 1.380(2) . ?
C9 C10 1.389(2) . ?
C3 C5 1.5172(18) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(2) . ?
C7 C8 1.3961(19) . ?
C7 C12 1.5234(19) . ?
C1 C4 1.5210(17) . ?
C22 H22 0.9500 . ?
C8 H8 0.9500 . ?
C10 H10 0.9500 . ?
C27 H27 1.0000 . ?
C27 C28 1.535(2) . ?
C27 C29 1.531(2) . ?
C12 H12 1.0000 . ?
C12 C14 1.5398(18) . ?
C12 C13 1.530(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C19 C24 1.5182(19) . ?
C15 H15 1.0000 . ?
C15 C16 1.535(2) . ?
C15 C17 1.537(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C24 H24 1.0000 . ?
C24 C25 1.524(2) . ?
C24 C26 1.531(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.501(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C40 H40 0.9500 . ?
C40 C42 1.385(2) 3_566 ?
C40 C41 1.379(2) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C42 C40 1.385(2) 3_566 ?
C42 H42 0.9500 . ?
C42 C41 1.383(2) . ?
C41 H41 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O2 65.68(3) . . ?
O1 Ca1 N1 88.15(4) . . ?
N2 Ca1 O2 88.50(3) . . ?
N2 Ca1 O1 137.58(4) . . ?
N2 Ca1 N1 77.84(4) . . ?
N1 Ca1 O2 122.47(4) . . ?
N3 Ca1 O2 113.43(4) . . ?
N3 Ca1 O1 101.36(4) . . ?
N3 Ca1 N2 120.14(4) . . ?
N3 Ca1 N1 121.80(4) . . ?
N3 Si2 C33 114.69(6) . . ?
N3 Si2 C34 116.03(6) . . ?
N3 Si2 C35 111.63(6) . . ?
C33 Si2 C34 103.61(7) . . ?
C35 Si2 C33 106.09(7) . . ?
C35 Si2 C34 103.67(7) . . ?
N3 Si1 C32 115.10(6) . . ?
N3 Si1 C30 114.03(6) . . ?
N3 Si1 C31 112.25(6) . . ?
C30 Si1 C32 105.19(7) . . ?
C31 Si1 C32 104.17(7) . . ?
C31 Si1 C30 105.08(7) . . ?
C36 O2 Ca1 130.53(8) . . ?
C37 O2 Ca1 117.22(8) . . ?
C37 O2 C36 109.61(10) . . ?
C38 O1 Ca1 112.15(8) . . ?
C39 O1 Ca1 132.18(8) . . ?
C39 O1 C38 113.69(11) . . ?
C18 N2 Ca1 120.15(8) . . ?
C3 N2 Ca1 122.88(8) . . ?
C3 N2 C18 116.64(11) . . ?
C6 N1 Ca1 118.33(8) . . ?
C1 N1 Ca1 120.74(8) . . ?
C1 N1 C6 119.28(10) . . ?
Si2 N3 Ca1 121.30(6) . . ?
Si2 N3 Si1 118.18(7) . . ?
Si1 N3 Ca1 120.49(6) . . ?
C11 C6 N1 118.52(11) . . ?
C7 C6 N1 121.60(12) . . ?
C7 C6 C11 119.74(12) . . ?
C18 C23 C27 122.32(11) . . ?
C22 C23 C18 118.97(12) . . ?
C22 C23 C27 118.69(12) . . ?
C6 C11 C15 121.15(12) . . ?
C10 C11 C6 118.75(12) . . ?
C10 C11 C15 120.06(12) . . ?
C3 C2 H2 114.8 . . ?
C3 C2 C1 130.32(12) . . ?
C1 C2 H2 114.8 . . ?
C23 C18 N2 120.83(11) . . ?
C23 C18 C19 119.85(11) . . ?
C19 C18 N2 119.23(11) . . ?
C21 C20 H20 119.4 . . ?
C21 C20 C19 121.24(13) . . ?
C19 C20 H20 119.4 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.37(12) . . ?
C10 C9 H9 120.3 . . ?
N2 C3 C2 124.82(12) . . ?
N2 C3 C5 120.33(11) . . ?
C2 C3 C5 114.80(11) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 C20 119.40(12) . . ?
C22 C21 H21 120.3 . . ?
C6 C7 C12 122.74(12) . . ?
C8 C7 C6 119.16(12) . . ?
C8 C7 C12 118.06(12) . . ?
N1 C1 C2 125.05(11) . . ?
N1 C1 C4 121.70(12) . . ?
C2 C1 C4 113.24(11) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 C23 121.30(12) . . ?
C21 C22 H22 119.4 . . ?
C9 C8 C7 121.44(13) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C11 C10 H10 119.3 . . ?
C9 C10 C11 121.44(13) . . ?
C9 C10 H10 119.3 . . ?
C23 C27 H27 108.1 . . ?
C23 C27 C28 110.44(11) . . ?
C23 C27 C29 111.73(12) . . ?
C28 C27 H27 108.1 . . ?
C29 C27 H27 108.1 . . ?
C29 C27 C28 110.19(12) . . ?
C7 C12 H12 107.9 . . ?
C7 C12 C14 110.50(11) . . ?
C7 C12 C13 112.64(12) . . ?
C14 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C13 C12 C14 109.92(11) . . ?
O2 C36 H36A 109.5 . . ?
O2 C36 H36B 109.5 . . ?
O2 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C18 C19 C24 121.87(11) . . ?
C20 C19 C18 119.22(12) . . ?
C20 C19 C24 118.87(12) . . ?
C11 C15 H15 107.8 . . ?
C11 C15 C16 113.41(12) . . ?
C11 C15 C17 111.08(11) . . ?
C16 C15 H15 107.8 . . ?
C16 C15 C17 108.84(12) . . ?
C17 C15 H15 107.8 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C19 C24 H24 107.9 . . ?
C19 C24 C25 110.75(12) . . ?
C19 C24 C26 112.68(12) . . ?
C25 C24 H24 107.9 . . ?
C25 C24 C26 109.55(13) . . ?
C26 C24 H24 107.9 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
Si1 C32 H32A 109.5 . . ?
Si1 C32 H32B 109.5 . . ?
Si1 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 C38 H38A 110.0 . . ?
O1 C38 H38B 110.0 . . ?
O1 C38 C37 108.42(12) . . ?
H38A C38 H38B 108.4 . . ?
C37 C38 H38A 110.0 . . ?
C37 C38 H38B 110.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si2 C34 H34A 109.5 . . ?
Si2 C34 H34B 109.5 . . ?
Si2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C40 H40 120.1 3_566 . ?
C41 C40 H40 120.1 . . ?
C41 C40 C42 119.72(16) . 3_566 ?
O1 C39 H39A 109.5 . . ?
O1 C39 H39B 109.5 . . ?
O1 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O2 C37 C38 108.30(11) . . ?
O2 C37 H37A 110.0 . . ?
O2 C37 H37B 110.0 . . ?
C38 C37 H37A 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
Si2 C35 H35A 109.5 . . ?
Si2 C35 H35B 109.5 . . ?
Si2 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C40 C42 H42 120.1 3_566 . ?
C41 C42 C40 119.86(16) . 3_566 ?
C41 C42 H42 120.1 . . ?
C40 C41 C42 120.43(16) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O2 C37 C38 -21.15(14) . . . . ?
Ca1 O1 C38 C37 -59.80(13) . . . . ?
Ca1 N2 C18 C23 78.12(13) . . . . ?
Ca1 N2 C18 C19 -98.56(12) . . . . ?
Ca1 N2 C3 C2 20.15(17) . . . . ?
Ca1 N2 C3 C5 -162.63(9) . . . . ?
Ca1 N1 C6 C11 94.08(12) . . . . ?
Ca1 N1 C6 C7 -81.50(13) . . . . ?
Ca1 N1 C1 C2 -25.63(17) . . . . ?
Ca1 N1 C1 C4 155.17(10) . . . . ?
O1 C38 C37 O2 51.39(15) . . . . ?
N2 C18 C19 C20 175.82(12) . . . . ?
N2 C18 C19 C24 -1.93(19) . . . . ?
N1 C6 C11 C10 -171.99(11) . . . . ?
N1 C6 C11 C15 10.30(18) . . . . ?
N1 C6 C7 C8 172.10(11) . . . . ?
N1 C6 C7 C12 -10.23(19) . . . . ?
C6 N1 C1 C2 169.27(12) . . . . ?
C6 N1 C1 C4 -9.93(19) . . . . ?
C6 C11 C10 C9 -1.50(19) . . . . ?
C6 C11 C15 C16 -160.36(12) . . . . ?
C6 C11 C15 C17 76.67(15) . . . . ?
C6 C7 C8 C9 0.99(19) . . . . ?
C6 C7 C12 C14 -119.45(14) . . . . ?
C6 C7 C12 C13 117.18(14) . . . . ?
C23 C18 C19 C20 -0.90(19) . . . . ?
C23 C18 C19 C24 -178.64(12) . . . . ?
C11 C6 C7 C8 -3.43(18) . . . . ?
C11 C6 C7 C12 174.24(12) . . . . ?
C18 N2 C3 C2 -166.46(12) . . . . ?
C18 N2 C3 C5 10.76(17) . . . . ?
C18 C23 C22 C21 1.1(2) . . . . ?
C18 C23 C27 C28 -116.59(14) . . . . ?
C18 C23 C27 C29 120.38(13) . . . . ?
C18 C19 C24 C25 115.02(14) . . . . ?
C18 C19 C24 C26 -121.88(14) . . . . ?
C20 C21 C22 C23 -0.8(2) . . . . ?
C20 C19 C24 C25 -62.73(16) . . . . ?
C20 C19 C24 C26 60.37(17) . . . . ?
C3 N2 C18 C23 -95.46(14) . . . . ?
C3 N2 C18 C19 87.86(15) . . . . ?
C3 C2 C1 N1 -13.3(2) . . . . ?
C3 C2 C1 C4 165.96(13) . . . . ?
C21 C20 C19 C18 1.2(2) . . . . ?
C21 C20 C19 C24 179.05(12) . . . . ?
C7 C6 C11 C10 3.68(18) . . . . ?
C7 C6 C11 C15 -174.03(12) . . . . ?
C1 N1 C6 C11 -100.45(14) . . . . ?
C1 N1 C6 C7 83.96(16) . . . . ?
C1 C2 C3 N2 17.2(2) . . . . ?
C1 C2 C3 C5 -160.20(14) . . . . ?
C22 C23 C18 N2 -176.91(12) . . . . ?
C22 C23 C18 C19 -0.25(19) . . . . ?
C22 C23 C27 C28 61.46(16) . . . . ?
C22 C23 C27 C29 -61.57(16) . . . . ?
C8 C9 C10 C11 -0.9(2) . . . . ?
C8 C7 C12 C14 58.24(16) . . . . ?
C8 C7 C12 C13 -65.13(16) . . . . ?
C10 C11 C15 C16 21.96(18) . . . . ?
C10 C11 C15 C17 -101.00(15) . . . . ?
C10 C9 C8 C7 1.2(2) . . . . ?
C27 C23 C18 N2 1.14(19) . . . . ?
C27 C23 C18 C19 177.80(12) . . . . ?
C27 C23 C22 C21 -177.01(12) . . . . ?
C12 C7 C8 C9 -176.79(12) . . . . ?
C36 O2 C37 C38 175.32(12) . . . . ?
C19 C20 C21 C22 -0.4(2) . . . . ?
C15 C11 C10 C9 176.23(12) . . . . ?
C33 Si2 N3 Ca1 -132.04(7) . . . . ?
C33 Si2 N3 Si1 46.01(9) . . . . ?
C32 Si1 N3 Ca1 -141.91(7) . . . . ?
C32 Si1 N3 Si2 40.03(10) . . . . ?
C30 Si1 N3 Ca1 96.37(8) . . . . ?
C30 Si1 N3 Si2 -81.69(9) . . . . ?
C31 Si1 N3 Ca1 -22.98(9) . . . . ?
C31 Si1 N3 Si2 158.96(8) . . . . ?
C34 Si2 N3 Ca1 107.11(8) . . . . ?
C34 Si2 N3 Si1 -74.84(9) . . . . ?
C40 C42 C41 C40 -0.2(3) 3_566 . . . ?
C39 O1 C38 C37 134.20(12) . . . . ?
C35 Si2 N3 Ca1 -11.35(9) . . . . ?
C35 Si2 N3 Si1 166.70(8) . . . . ?
C42 C40 C41 C42 0.2(3) 3_566 . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3 6 8 0.1471 2.9901 6.0215 8.4896 0.1267 0.6622 -0.7049
2 11 -2 0.0778 1.9984 11.0023 -1.5076 0.2582 0.9310 0.1302
-1 3 -12 0.2205 -0.9898 2.9763 -12.4941 -0.0030 0.1206 0.9851
-3 -10 -3 0.1242 -2.9940 -10.0122 -2.9901 -0.1997 -0.9393 0.2626
-2 -11 0 0.1045 -1.9973 -11.0049 0.0086 -0.2862 -0.9338 -0.0241
7 -3 -9 0.1159 6.9989 -3.0013 -8.9934 -0.9898 0.2707 0.1673
6 -4 3 0.1666 5.9912 -3.9825 2.9999 -0.7111 0.1492 -0.6333
-2 0 14 0.1830 -2.0081 0.0202 13.9915 0.4585 -0.1178 -0.8673
-6 3 10 0.1000 -6.0011 3.0060 10.4923 0.9192 -0.1961 -0.3346
-5 4 -7 0.1887 -4.9894 3.9776 -6.9976 0.5379 -0.0848 0.8548
2 0 -14 0.2146 2.0084 -0.0211 -14.4912 -0.4678 0.1169 0.9026
-4 8 8 0.0823 -4.0021 8.0070 8.4894 0.9045 0.3030 -0.2491
-3 6 12 0.1315 -3.0061 6.0159 12.4882 0.7927 0.2386 -0.6199
5 -8 -7 0.0726 5.0002 -8.0032 -7.4903 -0.9844 -0.2293 0.1171
5 -9 -4 0.0856 4.9977 -8.9972 -3.9917 -0.9630 -0.2947 -0.1437
5 -8 -7 0.0686 4.9998 -8.0023 -6.9906 -0.9750 -0.2284 0.0817
4 -8 -8 0.0801 4.0017 -8.0062 -7.9898 -0.8951 -0.3021 0.2137
-2 11 6 0.0711 -2.0026 11.0070 5.9884 0.7925 0.6576 -0.1549
-3 11 -2 0.1020 -2.9956 10.9910 -2.0063 0.7417 0.5709 0.4720
2 -11 -5 0.0623 2.0022 -11.0062 -5.4887 -0.7832 -0.6566 0.1196
2 -11 -4 0.0466 2.0011 -11.0036 -3.9897 -0.7552 -0.6539 0.0135
-2 -6 -10 0.1893 -1.9898 -6.0229 -10.4885 -0.2626 -0.5940 0.7850
0 11 -3 0.0907 0.0014 10.9964 -2.5066 0.4367 0.7855 0.3235
-5 -8 6 0.1288 -4.9985 -8.0005 6.0031 0.2533 -0.9227 -0.2244
-4 -8 10 0.1429 -4.0022 -7.9923 9.5007 0.2201 -0.8444 -0.5332
5 8 -7 0.1279 4.9989 7.9996 -6.5028 -0.2626 0.9218 0.2598
-6 -7 -1 0.1648 -5.9919 -7.0156 -1.4927 0.2558 -0.9366 0.3805
-8 -1 3 0.1495 -7.9932 -1.0115 3.0004 0.8006 -0.6409 0.2649
-7 -2 9 0.1141 -6.9987 -1.9990 8.9971 0.7701 -0.6298 -0.2339
-7 6 3 0.1134 -6.9949 5.9919 3.4947 1.0189 -0.0654 0.2616
-6 5 9 0.0911 -6.0001 5.0035 8.9917 0.9791 -0.0552 -0.2019
-4 10 5 0.0703 -3.9996 10.0011 4.9902 0.9270 0.4402 0.0250
-4 10 1 0.0834 -3.9970 9.9950 1.4924 0.8617 0.4338 0.2725
-4 8 -6 0.1478 -3.9917 7.9826 -5.5017 0.6431 0.2772 0.7408
0 11 5 0.0701 -0.0041 11.0095 4.9887 0.5767 0.7994 -0.2068
-1 12 0 0.0625 -0.9997 11.9996 0.4910 0.6352 0.7911 0.1860

_olex2_date_sample_data_collection 2016-06-15
_olex2_submission_original_sample_id hasj160615a
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_hasj161128a
_database_code_depnum_ccdc_archive 'CCDC 1520544'
_audit_update_record             
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_audit_creation_date             2016-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C40 H70 Ca N4 O Si2)'
_chemical_formula_sum            'C160 H280 Ca4 N16 O4 Si8'
_chemical_formula_weight         2877.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Ca Si O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.30050(10)
_cell_length_b                   20.2024(2)
_cell_length_c                   39.1907(2)
_cell_angle_alpha                102.3440(10)
_cell_angle_beta                 90.1900(10)
_cell_angle_gamma                90.3460(10)
_cell_volume                     8740.03(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    44642
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6970
_cell_measurement_theta_min      3.4390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.3013
_exptl_crystal_size_mid          0.2119
_exptl_crystal_size_min          0.171
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            86599
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.118
_diffrn_reflns_theta_min         3.463
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5806
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -128.00   45.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909    0.0000  -30.0000 346

#__ type_ start__ end____ width___ exp.time_
  2 omega -114.00  -19.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  120.0000 190

#__ type_ start__ end____ width___ exp.time_
  3 omega  -96.00   -2.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 188

#__ type_ start__ end____ width___ exp.time_
  4 omega   23.00   97.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000  120.0000 148

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   82.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -99.0000    0.0000 162

#__ type_ start__ end____ width___ exp.time_
  6 omega   31.00  130.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 198

#__ type_ start__ end____ width___ exp.time_
  7 omega   25.00  109.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -180.0000 168

#__ type_ start__ end____ width___ exp.time_
  8 omega   26.00  151.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000  -30.0000 250

#__ type_ start__ end____ width___ exp.time_
  9 omega   32.00  137.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -30.0000 210

#__ type_ start__ end____ width___ exp.time_
 10 omega   25.00  109.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -90.0000 168

#__ type_ start__ end____ width___ exp.time_
 11 omega   31.00  130.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  120.0000 198

#__ type_ start__ end____ width___ exp.time_
 12 omega   82.00  177.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  150.0000 190

#__ type_ start__ end____ width___ exp.time_
 13 omega   34.00  121.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  150.0000 174

#__ type_ start__ end____ width___ exp.time_
 14 omega -112.00  -15.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000 -120.0000 194

#__ type_ start__ end____ width___ exp.time_
 15 omega -116.00  -10.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000   90.0000 212

#__ type_ start__ end____ width___ exp.time_
 16 omega -116.00  -10.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000    0.0000 212

#__ type_ start__ end____ width___ exp.time_
 17 omega   61.00  178.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   15.0000   30.0000 234
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1100421000
_diffrn_orient_matrix_UB_12      -0.0463356000
_diffrn_orient_matrix_UB_13      -0.0072661000
_diffrn_orient_matrix_UB_21      -0.0720463000
_diffrn_orient_matrix_UB_22      0.0528189000
_diffrn_orient_matrix_UB_23      0.0257158000
_diffrn_orient_matrix_UB_31      -0.0358645000
_diffrn_orient_matrix_UB_32      0.0340147000
_diffrn_orient_matrix_UB_33      -0.0300858000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                28862
_reflns_number_total             31761
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         31761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²+2.2710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1085
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C64(H64), C15(H15), C92(H92), C24(H24), C12(H12), C107(H107), C144(H144),
 C135(H135), C55(H55), C27(H27), C52(H52), C147(H147), C95(H95), C132(H132),
 C67(H67), C104(H104)
2.b Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C156(H15A,H15B), C76(H76A,H76B), C79(H79A,H79B), C38(H38A,
 H38B), C157(H15F,H15G), C159(H15N,H15O), C118(H11A,H11B), C119(H11C,H11D),
 C77(H77A,H77B), C36(H36A,H36B), C158(H15P,H15Q), C39(H39A,H39B), C37(H37A,
 H37B), C117(H11K,H11L), C116(H11M,H11N)
2.c Aromatic/amide H refined with riding coordinates:
 C122(H122), C90(H90), C9(H9), C8(H8), C88(H88), C140(H140), C89(H89),
 C10(H10), C42(H42), C62(H62), C20(H20), C48(H48), C49(H49), C22(H22), C60(H60),
  C141(H141), C100(H100), C142(H142), C130(H130), C61(H61), C102(H102),
 C129(H129), C101(H101), C21(H21), C50(H50), C128(H128)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C84(H84A,H84B,H84C), C45(H45A,H45B,H45C), C44(H44A,H44B,
 H44C), C125(H12D,H12E,H12F), C124(H12G,H12H,H12I), C154(H15C,H15D,H15E),
 C75(H75A,H75B,H75C), C155(H15H,H15I,H15J), C150(H15K,H15L,H15M), C72(H72A,H72B,
 H72C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C),
 C114(H11E,H11F,H11G), C5(H5A,H5B,H5C), C35(H35A,H35B,H35C), C146(H14D,H14E,
 H14F), C85(H85A,H85B,H85C), C112(H11H,H11I,H11J), C93(H93A,H93B,H93C),
 C109(H10A,H10B,H10C), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C17(H17A,H17B,
 H17C), C74(H74A,H74B,H74C), C32(H32A,H32B,H32C), C65(H65A,H65B,H65C), C53(H53A,
 H53B,H53C), C31(H31A,H31B,H31C), C115(H11O,H11P,H11Q), C80(H80A,H80B,H80C),
 C136(H13D,H13E,H13F), C111(H11R,H11S,H11T), C28(H28A,H28B,H28C), C160(H16D,
 H16E,H16F), C94(H94A,H94B,H94C), C66(H66A,H66B,H66C), C54(H54A,H54B,H54C),
 C96(H96A,H96B,H96C), C152(H15R,H15S,H15T), C153(H15U,H15V,H15W), C13(H13A,H13B,
 H13C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C113(H11U,H11V,H11W),
 C110(H11X,H11Y,H), C14(H14A,H14B,H14C), C137(H13G,H13H,H13I), C151(H15X,H15Y,
 HA), C145(H14G,H14H,H14I), C149(H14J,H14K,H14L), C25(H25A,H25B,H25C), C57(H57A,
 H57B,H57C), C120(H12A,H12B,H12C), C70(H70A,H70B,H70C), C97(H97A,H97B,H97C),
 C56(H56A,H56B,H56C), C148(H14M,H14N,H14O), C106(H10D,H10E,H10F), C108(H10G,
 H10H,H10I), C105(H10J,H10K,H10L), C40(H40A,H40B,H40C), C26(H26A,H26B,H26C),
 C69(H69A,H69B,H69C), C134(H13J,H13K,H13L), C68(H68A,H68B,H68C), C133(H13M,H13N,
 H13O)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.45373(2) -0.06580(2) 0.60885(2) 0.01421(6) Uani 1 1 d . . . . .
Ca2 Ca 0.44702(2) 0.33532(2) 0.85772(2) 0.01559(7) Uani 1 1 d . . . . .
Ca3 Ca -0.04747(2) 0.84541(2) 0.89093(2) 0.01502(7) Uani 1 1 d . . . . .
Ca4 Ca 0.95452(2) 0.45518(2) 0.64305(2) 0.01523(7) Uani 1 1 d . . . . .
Si8 Si 1.22839(3) 0.44184(2) 0.68781(2) 0.01899(9) Uani 1 1 d . . . . .
Si2 Si 0.15979(3) -0.07549(2) 0.57758(2) 0.01802(9) Uani 1 1 d . . . . .
Si4 Si 0.72406(3) 0.34088(2) 0.81424(2) 0.02037(9) Uani 1 1 d . . . . .
Si1 Si 0.20635(3) -0.06453(2) 0.65406(2) 0.01986(9) Uani 1 1 d . . . . .
Si6 Si -0.33381(3) 0.88222(2) 0.92840(2) 0.01942(9) Uani 1 1 d . . . . .
Si5 Si -0.29959(4) 0.85175(2) 0.85075(2) 0.02136(9) Uani 1 1 d . . . . .
Si7 Si 1.21252(3) 0.41221(2) 0.60931(2) 0.01980(9) Uani 1 1 d . . . . .
Si3 Si 0.70991(3) 0.36839(2) 0.89260(2) 0.02047(9) Uani 1 1 d . . . . .
O4 O 0.86831(9) 0.50164(5) 0.69958(3) 0.0219(2) Uani 1 1 d . . . . .
O1 O 0.54485(9) -0.08312(6) 0.55148(3) 0.0237(2) Uani 1 1 d . . . . .
O2 O 0.35921(9) 0.28884(6) 0.80112(3) 0.0221(2) Uani 1 1 d . . . . .
O3 O 0.03436(10) 0.84929(6) 0.94844(3) 0.0243(2) Uani 1 1 d . . . . .
N9 N 0.07857(10) 0.76310(6) 0.85996(3) 0.0153(2) Uani 1 1 d . . . . .
N14 N 0.83956(10) 0.36164(6) 0.61721(3) 0.0153(2) Uani 1 1 d . . . . .
N1 N 0.57887(10) 0.01687(6) 0.64071(3) 0.0149(2) Uani 1 1 d . . . . .
N5 N 0.33631(10) 0.27655(6) 0.89188(3) 0.0166(2) Uani 1 1 d . . . . .
N2 N 0.56303(11) -0.13776(6) 0.63583(3) 0.0170(2) Uani 1 1 d . . . . .
N10 N 0.06038(11) 0.91755(6) 0.86314(3) 0.0169(2) Uani 1 1 d . . . . .
N6 N 0.33664(11) 0.42822(6) 0.88671(3) 0.0171(2) Uani 1 1 d . . . . .
N11 N -0.24818(11) 0.86232(6) 0.89236(3) 0.0196(3) Uani 1 1 d . . . . .
N13 N 0.84125(11) 0.51075(6) 0.60732(3) 0.0173(2) Uani 1 1 d . . . . .
N3 N 0.25130(10) -0.06735(6) 0.61241(3) 0.0181(3) Uani 1 1 d . . . . .
N7 N 0.64804(10) 0.34961(6) 0.85211(3) 0.0196(3) Uani 1 1 d . . . . .
N15 N 1.15259(10) 0.43357(6) 0.64975(3) 0.0186(3) Uani 1 1 d . . . . .
N12 N 0.19819(12) 0.82324(8) 0.99955(4) 0.0284(3) Uani 1 1 d . . . . .
N8 N 0.19319(12) 0.21230(7) 0.75270(4) 0.0250(3) Uani 1 1 d . . . . .
N16 N 0.70242(12) 0.57537(7) 0.74811(4) 0.0272(3) Uani 1 1 d . . . . .
N4 N 0.71758(12) -0.11397(8) 0.49735(4) 0.0310(3) Uani 1 1 d . . . . .
C6 C 0.56370(12) 0.08604(7) 0.65806(4) 0.0163(3) Uani 1 1 d . . . . .
C123 C 0.72868(12) 0.38009(7) 0.62461(4) 0.0156(3) Uani 1 1 d . . . . .
C81 C 0.18453(12) 0.78471(7) 0.87295(4) 0.0164(3) Uani 1 1 d . . . . .
C43 C 0.22801(12) 0.28239(7) 0.87962(4) 0.0169(3) Uani 1 1 d . . . . .
C18 C 0.52513(12) -0.19721(8) 0.64724(4) 0.0197(3) Uani 1 1 d . . . . .
C87 C 0.12009(12) 0.66944(7) 0.81029(4) 0.0182(3) Uani 1 1 d . . . . .
C138 C 0.86464(12) 0.29190(7) 0.60299(4) 0.0169(3) Uani 1 1 d . . . . .
C1 C 0.68715(12) -0.00267(7) 0.62979(4) 0.0167(3) Uani 1 1 d . . . . .
C122 C 0.68905(12) 0.44826(7) 0.63089(4) 0.0179(3) Uani 1 1 d . . . . .
H122 H 0.6199 0.4565 0.6449 0.021 Uiso 1 1 calc R . . . .
C90 C -0.01693(13) 0.58190(8) 0.84059(4) 0.0207(3) Uani 1 1 d . . . . .
H90 H -0.0653 0.5523 0.8505 0.025 Uiso 1 1 calc R . . . .
C3 C 0.67485(13) -0.13124(8) 0.62680(4) 0.0185(3) Uani 1 1 d . . . . .
C41 C 0.22533(12) 0.41004(7) 0.87888(4) 0.0175(3) Uani 1 1 d . . . . .
C143 C 0.83329(14) 0.26439(8) 0.56794(4) 0.0229(3) Uani 1 1 d . . . . .
C58 C 0.36005(13) 0.22178(7) 0.90859(4) 0.0184(3) Uani 1 1 d . . . . .
C83 C 0.17221(13) 0.91173(7) 0.87198(4) 0.0174(3) Uani 1 1 d . . . . .
C11 C 0.61265(13) 0.10911(8) 0.69189(4) 0.0189(3) Uani 1 1 d . . . . .
C9 C 0.53691(14) 0.22154(8) 0.69232(4) 0.0219(3) Uani 1 1 d . . . . .
H9 H 0.5294 0.2678 0.7037 0.026 Uiso 1 1 calc R . . . .
C63 C 0.41595(13) 0.16235(8) 0.89070(4) 0.0202(3) Uani 1 1 d . . . . .
C121 C 0.73347(13) 0.50601(7) 0.62019(4) 0.0177(3) Uani 1 1 d . . . . .
C86 C 0.06619(12) 0.69339(7) 0.84313(4) 0.0164(3) Uani 1 1 d . . . . .
C103 C 0.02997(13) 0.97134(8) 0.81341(4) 0.0214(3) Uani 1 1 d . . . . .
C2 C 0.72422(12) -0.07075(8) 0.62025(4) 0.0183(3) Uani 1 1 d . . . . .
C82 C 0.22009(13) 0.85334(8) 0.88159(4) 0.0182(3) Uani 1 1 d . . . . .
C7 C 0.49854(12) 0.13040(7) 0.64223(4) 0.0174(3) Uani 1 1 d . . . . .
C126 C 0.86619(13) 0.56511(8) 0.59018(4) 0.0199(3) Uani 1 1 d . . . . .
C139 C 0.92502(13) 0.25225(8) 0.62284(4) 0.0197(3) Uani 1 1 d . . . . .
C51 C 0.32990(14) 0.52742(8) 0.93570(4) 0.0237(3) Uani 1 1 d . . . . .
C8 C 0.48558(13) 0.19781(8) 0.65991(4) 0.0200(3) Uani 1 1 d . . . . .
H8 H 0.4407 0.2278 0.6495 0.024 Uiso 1 1 calc R . . . .
C88 C 0.10642(13) 0.60108(8) 0.79437(4) 0.0207(3) Uani 1 1 d . . . . .
H88 H 0.1450 0.5840 0.7728 0.025 Uiso 1 1 calc R . . . .
C19 C 0.52644(13) -0.19670(8) 0.68313(4) 0.0230(3) Uani 1 1 d . . . . .
C98 C 0.02332(13) 0.97437(7) 0.84954(4) 0.0187(3) Uani 1 1 d . . . . .
C46 C 0.36438(12) 0.49799(7) 0.90124(4) 0.0188(3) Uani 1 1 d . . . . .
C91 C -0.00296(13) 0.64926(7) 0.85821(4) 0.0183(3) Uani 1 1 d . . . . .
C4 C 0.77994(13) 0.04950(8) 0.62567(4) 0.0225(3) Uani 1 1 d . . . . .
H4A H 0.7419 0.0934 0.6267 0.034 Uiso 1 1 calc GR . . . .
H4B H 0.8194 0.0351 0.6031 0.034 Uiso 1 1 calc GR . . . .
H4C H 0.8385 0.0538 0.6445 0.034 Uiso 1 1 calc GR . . . .
C140 C 0.94722(14) 0.18433(8) 0.60756(5) 0.0252(3) Uani 1 1 d . . . . .
H140 H 0.9878 0.1570 0.6207 0.030 Uiso 1 1 calc R . . . .
C89 C 0.03834(13) 0.55751(7) 0.80906(4) 0.0209(3) Uani 1 1 d . . . . .
H89 H 0.0296 0.5113 0.7976 0.025 Uiso 1 1 calc R . . . .
C10 C 0.59928(13) 0.17724(8) 0.70795(4) 0.0217(3) Uani 1 1 d . . . . .
H10 H 0.6341 0.1937 0.7303 0.026 Uiso 1 1 calc R . . . .
C84 C 0.27551(13) 0.73415(8) 0.87992(4) 0.0218(3) Uani 1 1 d . . . . .
H84A H 0.2352 0.6967 0.8875 0.033 Uiso 1 1 calc GR . . . .
H84B H 0.3303 0.7567 0.8983 0.033 Uiso 1 1 calc GR . . . .
H84C H 0.3197 0.7164 0.8585 0.033 Uiso 1 1 calc GR . . . .
C64 C 0.45481(14) 0.15346(8) 0.85291(4) 0.0239(3) Uani 1 1 d . . . . .
H64 H 0.4220 0.1920 0.8436 0.029 Uiso 1 1 calc R . . . .
C42 C 0.18444(12) 0.34171(8) 0.87052(4) 0.0178(3) Uani 1 1 d . . . . .
H42 H 0.1154 0.3347 0.8563 0.021 Uiso 1 1 calc R . . . .
C131 C 0.92749(13) 0.62338(8) 0.60801(4) 0.0226(3) Uani 1 1 d . . . . .
C23 C 0.47867(13) -0.25342(8) 0.62306(4) 0.0226(3) Uani 1 1 d . . . . .
C45 C 0.14366(13) 0.22222(8) 0.87340(5) 0.0240(3) Uani 1 1 d . . . . .
H45A H 0.1744 0.1864 0.8547 0.036 Uiso 1 1 calc GR . . . .
H45B H 0.0658 0.2364 0.8666 0.036 Uiso 1 1 calc GR . . . .
H45C H 0.1363 0.2051 0.8949 0.036 Uiso 1 1 calc GR . . . .
C99 C -0.02643(14) 1.03139(8) 0.87178(4) 0.0233(3) Uani 1 1 d . . . . .
C62 C 0.43916(14) 0.11092(8) 0.90836(4) 0.0234(3) Uani 1 1 d . . . . .
H62 H 0.4778 0.0710 0.8964 0.028 Uiso 1 1 calc R . . . .
C15 C 0.67530(14) 0.06210(8) 0.71149(4) 0.0230(3) Uani 1 1 d . . . . .
H15 H 0.6788 0.0161 0.6958 0.028 Uiso 1 1 calc R . . . .
C92 C 0.18689(14) 0.71610(8) 0.79115(4) 0.0223(3) Uani 1 1 d . . . . .
H92 H 0.1903 0.7623 0.8067 0.027 Uiso 1 1 calc R . . . .
C78 C 0.39235(14) 0.22768(9) 0.77661(4) 0.0259(3) Uani 1 1 d . . . . .
H78A H 0.4570 0.2050 0.7867 0.031 Uiso 1 1 calc R . . . .
H78B H 0.4220 0.2395 0.7549 0.031 Uiso 1 1 calc R . . . .
C156 C 0.90037(14) 0.56397(8) 0.72361(4) 0.0261(4) Uani 1 1 d . . . . .
H15A H 0.9630 0.5876 0.7131 0.031 Uiso 1 1 calc R . . . .
H15B H 0.9322 0.5535 0.7454 0.031 Uiso 1 1 calc R . . . .
C47 C 0.43245(13) 0.53530(8) 0.88175(4) 0.0211(3) Uani 1 1 d . . . . .
C24 C 0.57348(14) -0.13595(9) 0.70972(4) 0.0256(3) Uani 1 1 d . . . . .
H24 H 0.5690 -0.0958 0.6987 0.031 Uiso 1 1 calc R . . . .
C20 C 0.48237(15) -0.25331(9) 0.69427(5) 0.0292(4) Uani 1 1 d . . . . .
H20 H 0.4837 -0.2537 0.7185 0.035 Uiso 1 1 calc R . . . .
C127 C 0.83573(15) 0.55844(8) 0.55462(4) 0.0255(3) Uani 1 1 d . . . . .
C48 C 0.46274(14) 0.60222(8) 0.89702(5) 0.0259(3) Uani 1 1 d . . . . .
H48 H 0.5084 0.6279 0.8841 0.031 Uiso 1 1 calc R . . . .
C59 C 0.33222(14) 0.22931(8) 0.94426(4) 0.0228(3) Uani 1 1 d . . . . .
C44 C 0.13048(14) 0.46193(8) 0.87724(5) 0.0256(3) Uani 1 1 d . . . . .
H44A H 0.0721 0.4614 0.8956 0.038 Uiso 1 1 calc GR . . . .
H44B H 0.0912 0.4509 0.8544 0.038 Uiso 1 1 calc GR . . . .
H44C H 0.1667 0.5071 0.8807 0.038 Uiso 1 1 calc GR . . . .
C125 C 0.63394(13) 0.32876(8) 0.62858(4) 0.0224(3) Uani 1 1 d . . . . .
H12D H 0.6666 0.2830 0.6222 0.034 Uiso 1 1 calc GR . . . .
H12E H 0.5668 0.3326 0.6133 0.034 Uiso 1 1 calc GR . . . .
H12F H 0.6073 0.3375 0.6529 0.034 Uiso 1 1 calc GR . . . .
C12 C 0.44567(14) 0.10925(8) 0.60587(4) 0.0222(3) Uani 1 1 d . . . . .
H12 H 0.4612 0.0598 0.5974 0.027 Uiso 1 1 calc R . . . .
C49 C 0.42766(16) 0.63183(8) 0.93048(5) 0.0303(4) Uani 1 1 d . . . . .
H49 H 0.4484 0.6776 0.9403 0.036 Uiso 1 1 calc R . . . .
C22 C 0.43453(15) -0.30829(8) 0.63565(5) 0.0284(4) Uani 1 1 d . . . . .
H22 H 0.4021 -0.3462 0.6197 0.034 Uiso 1 1 calc R . . . .
C76 C 0.26520(14) 0.32137(8) 0.78570(4) 0.0245(3) Uani 1 1 d . . . . .
H76A H 0.2943 0.3340 0.7641 0.029 Uiso 1 1 calc R . . . .
H76B H 0.2413 0.3633 0.8022 0.029 Uiso 1 1 calc R . . . .
C60 C 0.35475(15) 0.17595(8) 0.96057(4) 0.0263(3) Uani 1 1 d . . . . .
H60 H 0.3338 0.1802 0.9844 0.032 Uiso 1 1 calc R . . . .
C79 C 0.28803(15) 0.17984(8) 0.76807(4) 0.0273(4) Uani 1 1 d . . . . .
H79A H 0.3126 0.1381 0.7515 0.033 Uiso 1 1 calc R . . . .
H79B H 0.2595 0.1670 0.7896 0.033 Uiso 1 1 calc R . . . .
C107 C 0.07621(14) 0.90887(9) 0.78824(4) 0.0239(3) Uani 1 1 d . . . . .
H107 H 0.0771 0.8707 0.8008 0.029 Uiso 1 1 calc R . . . .
C144 C 0.96281(14) 0.28054(8) 0.66039(4) 0.0232(3) Uani 1 1 d . . . . .
H144 H 0.9751 0.3305 0.6630 0.028 Uiso 1 1 calc R . . . .
C124 C 0.64978(14) 0.56585(8) 0.62527(5) 0.0261(3) Uani 1 1 d . . . . .
H12G H 0.6758 0.6005 0.6454 0.039 Uiso 1 1 calc GR . . . .
H12H H 0.5695 0.5507 0.6294 0.039 Uiso 1 1 calc GR . . . .
H12I H 0.6500 0.5850 0.6043 0.039 Uiso 1 1 calc GR . . . .
C141 C 0.91146(15) 0.15625(8) 0.57387(5) 0.0269(4) Uani 1 1 d . . . . .
H141 H 0.9247 0.1096 0.5643 0.032 Uiso 1 1 calc R . . . .
C154 C 1.35073(14) 0.37867(9) 0.68807(5) 0.0274(4) Uani 1 1 d . . . . .
H15C H 1.3171 0.3328 0.6838 0.041 Uiso 1 1 calc GR . . . .
H15D H 1.3908 0.3887 0.7108 0.041 Uiso 1 1 calc GR . . . .
H15E H 1.4078 0.3817 0.6697 0.041 Uiso 1 1 calc GR . . . .
C38 C 0.53153(15) -0.13945(9) 0.52213(4) 0.0270(4) Uani 1 1 d . . . . .
H38A H 0.4871 -0.1246 0.5033 0.032 Uiso 1 1 calc R . . . .
H38B H 0.4852 -0.1758 0.5293 0.032 Uiso 1 1 calc R . . . .
C100 C -0.06344(15) 1.08534(8) 0.85755(5) 0.0291(4) Uani 1 1 d . . . . .
H100 H -0.0962 1.1242 0.8724 0.035 Uiso 1 1 calc R . . . .
C75 C 0.62610(15) 0.35337(9) 0.77720(4) 0.0294(4) Uani 1 1 d . . . . .
H75A H 0.5621 0.3196 0.7737 0.044 Uiso 1 1 calc GR . . . .
H75B H 0.6729 0.3481 0.7558 0.044 Uiso 1 1 calc GR . . . .
H75C H 0.5922 0.3989 0.7828 0.044 Uiso 1 1 calc GR . . . .
C157 C 0.79433(15) 0.60959(8) 0.73200(5) 0.0285(4) Uani 1 1 d . . . . .
H15F H 0.8180 0.6523 0.7482 0.034 Uiso 1 1 calc R . . . .
H15G H 0.7632 0.6209 0.7103 0.034 Uiso 1 1 calc R . . . .
C142 C 0.85667(15) 0.19603(8) 0.55429(4) 0.0270(4) Uani 1 1 d . . . . .
H142 H 0.8341 0.1766 0.5309 0.032 Uiso 1 1 calc R . . . .
C155 C 1.12771(15) 0.43278(9) 0.72480(4) 0.0274(4) Uani 1 1 d . . . . .
H15H H 1.0655 0.4671 0.7274 0.041 Uiso 1 1 calc GR . . . .
H15I H 1.1737 0.4391 0.7465 0.041 Uiso 1 1 calc GR . . . .
H15J H 1.0916 0.3875 0.7198 0.041 Uiso 1 1 calc GR . . . .
C150 C 1.09749(14) 0.42266(9) 0.57579(4) 0.0277(4) Uani 1 1 d . . . . .
H15K H 1.0274 0.3954 0.5783 0.042 Uiso 1 1 calc GR . . . .
H15L H 1.1301 0.4076 0.5523 0.042 Uiso 1 1 calc GR . . . .
H15M H 1.0753 0.4705 0.5794 0.042 Uiso 1 1 calc GR . . . .
C135 C 0.96626(15) 0.63197(8) 0.64579(5) 0.0267(3) Uani 1 1 d . . . . .
H135 H 0.9303 0.5940 0.6550 0.032 Uiso 1 1 calc R . . . .
C55 C 0.26282(16) 0.48886(9) 0.95900(4) 0.0282(4) Uani 1 1 d . . . . .
H55 H 0.2425 0.4428 0.9449 0.034 Uiso 1 1 calc R . . . .
C27 C 0.47219(15) -0.25484(8) 0.58433(4) 0.0258(3) Uani 1 1 d . . . . .
H27 H 0.5139 -0.2135 0.5802 0.031 Uiso 1 1 calc R . . . .
C72 C 0.59696(14) 0.35522(9) 0.92586(4) 0.0265(3) Uani 1 1 d . . . . .
H72A H 0.5291 0.3848 0.9251 0.040 Uiso 1 1 calc GR . . . .
H72B H 0.6326 0.3661 0.9492 0.040 Uiso 1 1 calc GR . . . .
H72C H 0.5704 0.3078 0.9206 0.040 Uiso 1 1 calc GR . . . .
C130 C 0.95459(15) 0.67449(8) 0.59031(5) 0.0276(4) Uani 1 1 d . . . . .
H130 H 0.9965 0.7136 0.6022 0.033 Uiso 1 1 calc R . . . .
C34 C 0.05757(15) -0.15100(9) 0.57161(5) 0.0315(4) Uani 1 1 d . . . . .
H34A H 0.1042 -0.1923 0.5700 0.047 Uiso 1 1 calc GR . . . .
H34B H 0.0113 -0.1543 0.5501 0.047 Uiso 1 1 calc GR . . . .
H34C H 0.0040 -0.1458 0.5916 0.047 Uiso 1 1 calc GR . . . .
C159 C 0.67025(14) 0.51226(9) 0.72416(4) 0.0263(3) Uani 1 1 d . . . . .
H15N H 0.6367 0.5222 0.7025 0.032 Uiso 1 1 calc R . . . .
H15O H 0.6091 0.4882 0.7350 0.032 Uiso 1 1 calc R . . . .
C61 C 0.40712(15) 0.11664(8) 0.94285(4) 0.0261(3) Uani 1 1 d . . . . .
H61 H 0.4208 0.0804 0.9543 0.031 Uiso 1 1 calc R . . . .
C33 C 0.06105(14) -0.00106(8) 0.57746(5) 0.0270(3) Uani 1 1 d . . . . .
H33A H 0.0152 0.0089 0.5991 0.040 Uiso 1 1 calc GR . . . .
H33B H 0.0069 -0.0118 0.5574 0.040 Uiso 1 1 calc GR . . . .
H33C H 0.1095 0.0385 0.5758 0.040 Uiso 1 1 calc GR . . . .
C102 C -0.00739(15) 1.02687(9) 0.80050(5) 0.0283(4) Uani 1 1 d . . . . .
H102 H -0.0010 1.0257 0.7762 0.034 Uiso 1 1 calc R . . . .
C118 C 0.00705(14) 0.80406(8) 0.97131(4) 0.0249(3) Uani 1 1 d . . . . .
H11A H -0.0492 0.7687 0.9595 0.030 Uiso 1 1 calc R . . . .
H11B H -0.0313 0.8298 0.9927 0.030 Uiso 1 1 calc R . . . .
C119 C 0.11795(15) 0.77099(9) 0.98111(4) 0.0279(4) Uani 1 1 d . . . . .
H11C H 0.0976 0.7392 0.9962 0.033 Uiso 1 1 calc R . . . .
H11D H 0.1566 0.7451 0.9598 0.033 Uiso 1 1 calc R . . . .
C16 C 0.60471(16) 0.05653(9) 0.74413(4) 0.0304(4) Uani 1 1 d . . . . .
H16A H 0.6012 0.1011 0.7600 0.046 Uiso 1 1 calc GR . . . .
H16B H 0.6436 0.0244 0.7560 0.046 Uiso 1 1 calc GR . . . .
H16C H 0.5243 0.0405 0.7373 0.046 Uiso 1 1 calc GR . . . .
C114 C -0.42159(15) 0.80820(9) 0.93699(5) 0.0291(4) Uani 1 1 d . . . . .
H11E H -0.4756 0.7917 0.9174 0.044 Uiso 1 1 calc GR . . . .
H11F H -0.4674 0.8225 0.9585 0.044 Uiso 1 1 calc GR . . . .
H11G H -0.3676 0.7718 0.9396 0.044 Uiso 1 1 calc GR . . . .
C52 C 0.46736(14) 0.50573(8) 0.84417(4) 0.0242(3) Uani 1 1 d . . . . .
H52 H 0.4805 0.4561 0.8422 0.029 Uiso 1 1 calc R . . . .
C5 C 0.75851(14) -0.19086(9) 0.62158(5) 0.0285(4) Uani 1 1 d . . . . .
H5A H 0.7257 -0.2259 0.6327 0.043 Uiso 1 1 calc GR . . . .
H5B H 0.8355 -0.1758 0.6321 0.043 Uiso 1 1 calc GR . . . .
H5C H 0.7684 -0.2094 0.5965 0.043 Uiso 1 1 calc GR . . . .
C77 C 0.15920(14) 0.27445(8) 0.77702(4) 0.0252(3) Uani 1 1 d . . . . .
H77A H 0.1278 0.2633 0.7987 0.030 Uiso 1 1 calc R . . . .
H77B H 0.0960 0.2974 0.7664 0.030 Uiso 1 1 calc R . . . .
C35 C 0.24595(15) -0.08356(9) 0.53591(4) 0.0280(4) Uani 1 1 d . . . . .
H35A H 0.3042 -0.0467 0.5385 0.042 Uiso 1 1 calc GR . . . .
H35B H 0.1917 -0.0810 0.5167 0.042 Uiso 1 1 calc GR . . . .
H35C H 0.2868 -0.1272 0.5308 0.042 Uiso 1 1 calc GR . . . .
C146 C 1.07954(15) 0.25090(10) 0.67004(5) 0.0335(4) Uani 1 1 d . . . . .
H14D H 1.0690 0.2024 0.6692 0.050 Uiso 1 1 calc GR . . . .
H14E H 1.1033 0.2740 0.6937 0.050 Uiso 1 1 calc GR . . . .
H14F H 1.1409 0.2574 0.6534 0.050 Uiso 1 1 calc GR . . . .
C36 C 0.61576(15) -0.03089(9) 0.54132(4) 0.0272(4) Uani 1 1 d . . . . .
H36A H 0.6281 0.0068 0.5618 0.033 Uiso 1 1 calc R . . . .
H36B H 0.5731 -0.0129 0.5232 0.033 Uiso 1 1 calc R . . . .
C85 C 0.26019(14) 0.96913(8) 0.87366(5) 0.0278(4) Uani 1 1 d . . . . .
H85A H 0.2227 1.0060 0.8650 0.042 Uiso 1 1 calc GR . . . .
H85B H 0.3288 0.9528 0.8591 0.042 Uiso 1 1 calc GR . . . .
H85C H 0.2860 0.9857 0.8979 0.042 Uiso 1 1 calc GR . . . .
C158 C 0.77763(14) 0.46756(8) 0.71543(4) 0.0254(3) Uani 1 1 d . . . . .
H15P H 0.8092 0.4560 0.7370 0.030 Uiso 1 1 calc R . . . .
H15Q H 0.7545 0.4249 0.6992 0.030 Uiso 1 1 calc R . . . .
C112 C -0.18602(15) 0.80395(10) 0.81978(4) 0.0301(4) Uani 1 1 d . . . . .
H11H H -0.1114 0.8295 0.8224 0.045 Uiso 1 1 calc GR . . . .
H11I H -0.2148 0.7982 0.7957 0.045 Uiso 1 1 calc GR . . . .
H11J H -0.1731 0.7594 0.8252 0.045 Uiso 1 1 calc GR . . . .
C129 C 0.92161(17) 0.66916(9) 0.55594(5) 0.0316(4) Uani 1 1 d . . . . .
H129 H 0.9388 0.7049 0.5444 0.038 Uiso 1 1 calc R . . . .
C101 C -0.05357(16) 1.08364(9) 0.82231(5) 0.0316(4) Uani 1 1 d . . . . .
H101 H -0.0783 1.1212 0.8131 0.038 Uiso 1 1 calc R . . . .
C147 C 0.7785(2) 0.30638(9) 0.54422(5) 0.0361(4) Uani 1 1 d . . . . .
H147 H 0.7761 0.3546 0.5574 0.043 Uiso 1 1 calc R . . . .
C39 C 0.64982(16) -0.16695(9) 0.50833(5) 0.0321(4) Uani 1 1 d . . . . .
H39A H 0.6936 -0.1834 0.5268 0.039 Uiso 1 1 calc R . . . .
H39B H 0.6380 -0.2056 0.4883 0.039 Uiso 1 1 calc R . . . .
C93 C 0.11925(16) 0.72107(9) 0.75793(5) 0.0307(4) Uani 1 1 d . . . . .
H93A H 0.1143 0.6762 0.7424 0.046 Uiso 1 1 calc GR . . . .
H93B H 0.1608 0.7523 0.7460 0.046 Uiso 1 1 calc GR . . . .
H93C H 0.0393 0.7379 0.7641 0.046 Uiso 1 1 calc GR . . . .
C109 C -0.00472(17) 0.88811(10) 0.75640(5) 0.0328(4) Uani 1 1 d . . . . .
H10A H -0.0855 0.8815 0.7641 0.049 Uiso 1 1 calc GR . . . .
H10B H 0.0237 0.8457 0.7417 0.049 Uiso 1 1 calc GR . . . .
H10C H -0.0042 0.9238 0.7429 0.049 Uiso 1 1 calc GR . . . .
C37 C 0.73441(15) -0.05780(10) 0.52728(4) 0.0309(4) Uani 1 1 d . . . . .
H37A H 0.7805 -0.0212 0.5202 0.037 Uiso 1 1 calc R . . . .
H37B H 0.7794 -0.0734 0.5458 0.037 Uiso 1 1 calc R . . . .
C21 C 0.43691(16) -0.30867(9) 0.67079(5) 0.0325(4) Uani 1 1 d . . . . .
H21 H 0.4075 -0.3467 0.6788 0.039 Uiso 1 1 calc R . . . .
C50 C 0.36236(16) 0.59477(9) 0.94955(5) 0.0303(4) Uani 1 1 d . . . . .
H50 H 0.3389 0.6154 0.9726 0.036 Uiso 1 1 calc R . . . .
C73 C 0.85107(15) 0.40193(9) 0.81477(5) 0.0308(4) Uani 1 1 d . . . . .
H73A H 0.8211 0.4484 0.8197 0.046 Uiso 1 1 calc GR . . . .
H73B H 0.8901 0.3923 0.7920 0.046 Uiso 1 1 calc GR . . . .
H73C H 0.9080 0.3968 0.8329 0.046 Uiso 1 1 calc GR . . . .
C71 C 0.76093(17) 0.45893(9) 0.90689(5) 0.0334(4) Uani 1 1 d . . . . .
H71A H 0.8167 0.4697 0.8897 0.050 Uiso 1 1 calc GR . . . .
H71B H 0.8001 0.4652 0.9297 0.050 Uiso 1 1 calc GR . . . .
H71C H 0.6926 0.4891 0.9087 0.050 Uiso 1 1 calc GR . . . .
C17 C 0.80231(15) 0.08512(10) 0.72220(5) 0.0315(4) Uani 1 1 d . . . . .
H17A H 0.8470 0.0898 0.7014 0.047 Uiso 1 1 calc GR . . . .
H17B H 0.8404 0.0514 0.7331 0.047 Uiso 1 1 calc GR . . . .
H17C H 0.8006 0.1289 0.7388 0.047 Uiso 1 1 calc GR . . . .
C128 C 0.86326(17) 0.61134(9) 0.53838(5) 0.0314(4) Uani 1 1 d . . . . .
H128 H 0.8415 0.6077 0.5146 0.038 Uiso 1 1 calc R . . . .
C74 C 0.79274(17) 0.25477(9) 0.79965(5) 0.0349(4) Uani 1 1 d . . . . .
H74A H 0.8496 0.2472 0.8173 0.052 Uiso 1 1 calc GR . . . .
H74B H 0.8336 0.2525 0.7774 0.052 Uiso 1 1 calc GR . . . .
H74C H 0.7307 0.2199 0.7966 0.052 Uiso 1 1 calc GR . . . .
C32 C 0.32257(15) -0.01905(10) 0.68523(4) 0.0301(4) Uani 1 1 d . . . . .
H32A H 0.3979 -0.0431 0.6808 0.045 Uiso 1 1 calc GR . . . .
H32B H 0.2979 -0.0178 0.7093 0.045 Uiso 1 1 calc GR . . . .
H32C H 0.3323 0.0273 0.6818 0.045 Uiso 1 1 calc GR . . . .
C65 C 0.40854(16) 0.08726(8) 0.82976(4) 0.0271(4) Uani 1 1 d . . . . .
H65A H 0.4446 0.0486 0.8372 0.041 Uiso 1 1 calc GR . . . .
H65B H 0.4291 0.0861 0.8054 0.041 Uiso 1 1 calc GR . . . .
H65C H 0.3223 0.0848 0.8319 0.041 Uiso 1 1 calc GR . . . .
C117 C 0.22780(15) 0.86921(9) 0.97677(4) 0.0300(4) Uani 1 1 d . . . . .
H11K H 0.2695 0.8440 0.9559 0.036 Uiso 1 1 calc R . . . .
H11L H 0.2815 0.9053 0.9893 0.036 Uiso 1 1 calc R . . . .
C53 C 0.58223(16) 0.53555(10) 0.83329(5) 0.0341(4) Uani 1 1 d . . . . .
H53A H 0.5710 0.5837 0.8334 0.051 Uiso 1 1 calc GR . . . .
H53B H 0.6039 0.5114 0.8097 0.051 Uiso 1 1 calc GR . . . .
H53C H 0.6455 0.5307 0.8497 0.051 Uiso 1 1 calc GR . . . .
C31 C 0.06486(14) -0.01699(10) 0.66711(5) 0.0301(4) Uani 1 1 d . . . . .
H31A H 0.0717 0.0288 0.6626 0.045 Uiso 1 1 calc GR . . . .
H31B H 0.0505 -0.0140 0.6920 0.045 Uiso 1 1 calc GR . . . .
H31C H -0.0012 -0.0410 0.6535 0.045 Uiso 1 1 calc GR . . . .
C95 C -0.05983(15) 0.67154(8) 0.89381(4) 0.0257(4) Uani 1 1 d . . . . .
H95 H -0.0348 0.7195 0.9034 0.031 Uiso 1 1 calc R . . . .
C116 C 0.11697(15) 0.90078(9) 0.96561(4) 0.0286(4) Uani 1 1 d . . . . .
H11M H 0.0789 0.9291 0.9864 0.034 Uiso 1 1 calc R . . . .
H11N H 0.1385 0.9305 0.9495 0.034 Uiso 1 1 calc R . . . .
C115 C -0.24144(15) 0.91466(9) 0.96888(4) 0.0297(4) Uani 1 1 d . . . . .
H11O H -0.1983 0.8769 0.9751 0.045 Uiso 1 1 calc GR . . . .
H11P H -0.2932 0.9352 0.9882 0.045 Uiso 1 1 calc GR . . . .
H11Q H -0.1849 0.9487 0.9643 0.045 Uiso 1 1 calc GR . . . .
C80 C 0.09132(17) 0.16676(10) 0.74413(5) 0.0359(4) Uani 1 1 d . . . . .
H80A H 0.1147 0.1262 0.7270 0.054 Uiso 1 1 calc GR . . . .
H80B H 0.0279 0.1900 0.7343 0.054 Uiso 1 1 calc GR . . . .
H80C H 0.0631 0.1535 0.7653 0.054 Uiso 1 1 calc GR . . . .
C132 C 0.77670(18) 0.49409(9) 0.53362(5) 0.0332(4) Uani 1 1 d . . . . .
H132 H 0.7981 0.4563 0.5453 0.040 Uiso 1 1 calc R . . . .
C136 C 0.92416(16) 0.69867(8) 0.66890(5) 0.0297(4) Uani 1 1 d . . . . .
H13D H 0.9616 0.7369 0.6612 0.045 Uiso 1 1 calc GR . . . .
H13E H 0.9460 0.6999 0.6933 0.045 Uiso 1 1 calc GR . . . .
H13F H 0.8380 0.7018 0.6670 0.045 Uiso 1 1 calc GR . . . .
C111 C -0.32619(18) 0.93373(10) 0.83668(5) 0.0362(4) Uani 1 1 d . . . . .
H11R H -0.3862 0.9599 0.8517 0.054 Uiso 1 1 calc GR . . . .
H11S H -0.3539 0.9242 0.8124 0.054 Uiso 1 1 calc GR . . . .
H11T H -0.2523 0.9599 0.8386 0.054 Uiso 1 1 calc GR . . . .
C67 C 0.28174(18) 0.29547(9) 0.96536(4) 0.0316(4) Uani 1 1 d . . . . .
H67 H 0.3097 0.3329 0.9543 0.038 Uiso 1 1 calc R . . . .
C104 C -0.04053(18) 1.03574(8) 0.91073(5) 0.0316(4) Uani 1 1 d . . . . .
H104 H -0.0267 0.9895 0.9152 0.038 Uiso 1 1 calc R . . . .
C28 C 0.34336(16) -0.25128(9) 0.57284(5) 0.0330(4) Uani 1 1 d . . . . .
H28A H 0.3005 -0.2917 0.5762 0.049 Uiso 1 1 calc GR . . . .
H28B H 0.3406 -0.2492 0.5481 0.049 Uiso 1 1 calc GR . . . .
H28C H 0.3064 -0.2107 0.5868 0.049 Uiso 1 1 calc GR . . . .
C160 C 0.59931(17) 0.61889(10) 0.75657(5) 0.0382(4) Uani 1 1 d . . . . .
H16D H 0.6221 0.6602 0.7734 0.057 Uiso 1 1 calc GR . . . .
H16E H 0.5377 0.5948 0.7667 0.057 Uiso 1 1 calc GR . . . .
H16F H 0.5689 0.6309 0.7352 0.057 Uiso 1 1 calc GR . . . .
C94 C 0.31404(15) 0.69302(9) 0.78194(5) 0.0298(4) Uani 1 1 d . . . . .
H94A H 0.3568 0.6896 0.8033 0.045 Uiso 1 1 calc GR . . . .
H94B H 0.3540 0.7260 0.7708 0.045 Uiso 1 1 calc GR . . . .
H94C H 0.3126 0.6487 0.7658 0.045 Uiso 1 1 calc GR . . . .
C66 C 0.58995(16) 0.15673(10) 0.85074(5) 0.0359(4) Uani 1 1 d . . . . .
H66A H 0.6181 0.2011 0.8636 0.054 Uiso 1 1 calc GR . . . .
H66B H 0.6137 0.1501 0.8262 0.054 Uiso 1 1 calc GR . . . .
H66C H 0.6245 0.1211 0.8610 0.054 Uiso 1 1 calc GR . . . .
C54 C 0.36743(16) 0.51289(10) 0.81896(5) 0.0350(4) Uani 1 1 d . . . . .
H54A H 0.2957 0.4909 0.8253 0.052 Uiso 1 1 calc GR . . . .
H54B H 0.3904 0.4913 0.7951 0.052 Uiso 1 1 calc GR . . . .
H54C H 0.3520 0.5610 0.8203 0.052 Uiso 1 1 calc GR . . . .
C96 C -0.01729(17) 0.62923(8) 0.91933(4) 0.0300(4) Uani 1 1 d . . . . .
H96A H -0.0445 0.5823 0.9114 0.045 Uiso 1 1 calc GR . . . .
H96B H -0.0494 0.6478 0.9426 0.045 Uiso 1 1 calc GR . . . .
H96C H 0.0694 0.6304 0.9204 0.045 Uiso 1 1 calc GR . . . .
C152 C 1.26104(17) 0.32129(9) 0.59603(5) 0.0340(4) Uani 1 1 d . . . . .
H15R H 1.3196 0.3118 0.6128 0.051 Uiso 1 1 calc GR . . . .
H15S H 1.2964 0.3135 0.5727 0.051 Uiso 1 1 calc GR . . . .
H15T H 1.1924 0.2913 0.5956 0.051 Uiso 1 1 calc GR . . . .
C153 C 1.30345(17) 0.52687(9) 0.70195(5) 0.0342(4) Uani 1 1 d . . . . .
H15U H 1.3617 0.5328 0.6844 0.051 Uiso 1 1 calc GR . . . .
H15V H 1.3435 0.5292 0.7244 0.051 Uiso 1 1 calc GR . . . .
H15W H 1.2442 0.5628 0.7044 0.051 Uiso 1 1 calc GR . . . .
C13 C 0.31182(16) 0.11901(10) 0.60565(5) 0.0357(4) Uani 1 1 d . . . . .
H13A H 0.2745 0.0921 0.6207 0.054 Uiso 1 1 calc GR . . . .
H13B H 0.2815 0.1042 0.5818 0.054 Uiso 1 1 calc GR . . . .
H13C H 0.2935 0.1670 0.6143 0.054 Uiso 1 1 calc GR . . . .
C29 C 0.53349(19) -0.31681(10) 0.56214(5) 0.0376(4) Uani 1 1 d . . . . .
H29A H 0.6161 -0.3178 0.5697 0.056 Uiso 1 1 calc GR . . . .
H29B H 0.5307 -0.3140 0.5375 0.056 Uiso 1 1 calc GR . . . .
H29C H 0.4928 -0.3582 0.5651 0.056 Uiso 1 1 calc GR . . . .
C30 C 0.18533(17) -0.15095(9) 0.66380(5) 0.0342(4) Uani 1 1 d . . . . .
H30A H 0.1245 -0.1759 0.6482 0.051 Uiso 1 1 calc GR . . . .
H30B H 0.1604 -0.1463 0.6881 0.051 Uiso 1 1 calc GR . . . .
H30C H 0.2601 -0.1757 0.6602 0.051 Uiso 1 1 calc GR . . . .
C113 C -0.44804(15) 0.94942(9) 0.92761(5) 0.0326(4) Uani 1 1 d . . . . .
H11U H -0.4083 0.9925 0.9272 0.049 Uiso 1 1 calc GR . . . .
H11V H -0.4975 0.9548 0.9485 0.049 Uiso 1 1 calc GR . . . .
H11W H -0.4978 0.9359 0.9067 0.049 Uiso 1 1 calc GR . . . .
C110 C -0.43973(15) 0.79998(10) 0.84114(5) 0.0320(4) Uani 1 1 d . . . . .
H11X H -0.4285 0.7559 0.8473 0.048 Uiso 1 1 calc GR . . . .
H11Y H -0.4589 0.7932 0.8162 0.048 Uiso 1 1 calc GR . . . .
H H -0.5047 0.8239 0.8549 0.048 Uiso 1 1 calc GR . . . .
C14 C 0.50514(18) 0.14648(9) 0.58031(4) 0.0329(4) Uani 1 1 d . . . . .
H14A H 0.4895 0.1951 0.5875 0.049 Uiso 1 1 calc GR . . . .
H14B H 0.4733 0.1293 0.5568 0.049 Uiso 1 1 calc GR . . . .
H14C H 0.5907 0.1389 0.5803 0.049 Uiso 1 1 calc GR . . . .
C137 C 1.10080(17) 0.62672(11) 0.64870(6) 0.0423(5) Uani 1 1 d . . . . .
H13G H 1.1267 0.5826 0.6352 0.063 Uiso 1 1 calc GR . . . .
H13H H 1.1232 0.6312 0.6733 0.063 Uiso 1 1 calc GR . . . .
H13I H 1.1386 0.6630 0.6395 0.063 Uiso 1 1 calc GR . . . .
C151 C 1.34299(15) 0.46595(10) 0.60211(5) 0.0356(4) Uani 1 1 d . . . . .
H15X H 1.3203 0.5138 0.6074 0.053 Uiso 1 1 calc GR . . . .
H15Y H 1.3683 0.4528 0.5777 0.053 Uiso 1 1 calc GR . . . .
HA H 1.4083 0.4592 0.6175 0.053 Uiso 1 1 calc GR . . . .
C145 C 0.86598(16) 0.27048(10) 0.68586(5) 0.0352(4) Uani 1 1 d . . . . .
H14G H 0.7929 0.2918 0.6802 0.053 Uiso 1 1 calc GR . . . .
H14H H 0.8909 0.2913 0.7097 0.053 Uiso 1 1 calc GR . . . .
H14I H 0.8520 0.2219 0.6840 0.053 Uiso 1 1 calc GR . . . .
C149 C 0.8550(2) 0.30345(11) 0.51204(5) 0.0483(6) Uani 1 1 d . . . . .
H14J H 0.9348 0.3200 0.5193 0.072 Uiso 1 1 calc GR . . . .
H14K H 0.8202 0.3319 0.4974 0.072 Uiso 1 1 calc GR . . . .
H14L H 0.8591 0.2565 0.4988 0.072 Uiso 1 1 calc GR . . . .
C25 C 0.49864(19) -0.12025(11) 0.74267(5) 0.0394(5) Uani 1 1 d . . . . .
H25A H 0.4152 -0.1176 0.7363 0.059 Uiso 1 1 calc GR . . . .
H25B H 0.5240 -0.0768 0.7573 0.059 Uiso 1 1 calc GR . . . .
H25C H 0.5085 -0.1562 0.7557 0.059 Uiso 1 1 calc GR . . . .
C57 C 0.34089(19) 0.48015(10) 0.98962(5) 0.0377(4) Uani 1 1 d . . . . .
H57A H 0.4104 0.4532 0.9807 0.057 Uiso 1 1 calc GR . . . .
H57B H 0.2958 0.4569 1.0049 0.057 Uiso 1 1 calc GR . . . .
H57C H 0.3665 0.5248 1.0028 0.057 Uiso 1 1 calc GR . . . .
C120 C 0.30360(17) 0.79417(11) 1.01174(5) 0.0408(5) Uani 1 1 d . . . . .
H12A H 0.2804 0.7633 1.0268 0.061 Uiso 1 1 calc GR . . . .
H12B H 0.3537 0.8305 1.0250 0.061 Uiso 1 1 calc GR . . . .
H12C H 0.3476 0.7690 0.9916 0.061 Uiso 1 1 calc GR . . . .
C70 C 0.83939(15) 0.31378(10) 0.89870(5) 0.0366(4) Uani 1 1 d . . . . .
H70A H 0.8155 0.2660 0.8926 0.055 Uiso 1 1 calc GR . . . .
H70B H 0.8657 0.3253 0.9231 0.055 Uiso 1 1 calc GR . . . .
H70C H 0.9044 0.3216 0.8835 0.055 Uiso 1 1 calc GR . . . .
C97 C -0.19478(17) 0.67023(10) 0.89154(6) 0.0397(5) Uani 1 1 d . . . . .
H97A H -0.2210 0.7000 0.8763 0.059 Uiso 1 1 calc GR . . . .
H97B H -0.2279 0.6860 0.9149 0.059 Uiso 1 1 calc GR . . . .
H97C H -0.2221 0.6238 0.8819 0.059 Uiso 1 1 calc GR . . . .
C56 C 0.14730(19) 0.52393(11) 0.97313(6) 0.0459(5) Uani 1 1 d . . . . .
H56A H 0.1657 0.5682 0.9882 0.069 Uiso 1 1 calc GR . . . .
H56B H 0.1050 0.4958 0.9867 0.069 Uiso 1 1 calc GR . . . .
H56C H 0.0975 0.5302 0.9536 0.069 Uiso 1 1 calc GR . . . .
C148 C 0.6516(2) 0.28375(12) 0.53351(5) 0.0453(5) Uani 1 1 d . . . . .
H14M H 0.6517 0.2365 0.5206 0.068 Uiso 1 1 calc GR . . . .
H14N H 0.6191 0.3126 0.5186 0.068 Uiso 1 1 calc GR . . . .
H14O H 0.6027 0.2877 0.5544 0.068 Uiso 1 1 calc GR . . . .
C106 C -0.16511(19) 1.05660(11) 0.92298(5) 0.0447(5) Uani 1 1 d . . . . .
H10D H -0.1792 1.1033 0.9207 0.067 Uiso 1 1 calc GR . . . .
H10E H -0.1737 1.0537 0.9475 0.067 Uiso 1 1 calc GR . . . .
H10F H -0.2227 1.0262 0.9087 0.067 Uiso 1 1 calc GR . . . .
C108 C 0.20272(17) 0.91973(12) 0.77691(6) 0.0481(6) Uani 1 1 d . . . . .
H10G H 0.2050 0.9583 0.7654 0.072 Uiso 1 1 calc GR . . . .
H10H H 0.2296 0.8789 0.7606 0.072 Uiso 1 1 calc GR . . . .
H10I H 0.2548 0.9290 0.7975 0.072 Uiso 1 1 calc GR . . . .
C105 C 0.0508(2) 1.08348(13) 0.93204(5) 0.0513(6) Uani 1 1 d . . . . .
H10J H 0.1302 1.0708 0.9231 0.077 Uiso 1 1 calc GR . . . .
H10K H 0.0464 1.0802 0.9566 0.077 Uiso 1 1 calc GR . . . .
H10L H 0.0345 1.1301 0.9301 0.077 Uiso 1 1 calc GR . . . .
C40 C 0.83152(17) -0.13997(14) 0.48261(5) 0.0489(6) Uani 1 1 d . . . . .
H40A H 0.8765 -0.1575 0.5001 0.073 Uiso 1 1 calc GR . . . .
H40B H 0.8765 -0.1033 0.4758 0.073 Uiso 1 1 calc GR . . . .
H40C H 0.8177 -0.1765 0.4621 0.073 Uiso 1 1 calc GR . . . .
C26 C 0.70317(18) -0.14475(13) 0.71862(7) 0.0515(6) Uani 1 1 d . . . . .
H26A H 0.7112 -0.1846 0.7289 0.077 Uiso 1 1 calc GR . . . .
H26B H 0.7310 -0.1044 0.7353 0.077 Uiso 1 1 calc GR . . . .
H26C H 0.7506 -0.1509 0.6973 0.077 Uiso 1 1 calc GR . . . .
C69 C 0.1463(2) 0.29609(12) 0.96504(7) 0.0604(7) Uani 1 1 d . . . . .
H69A H 0.1179 0.2937 0.9412 0.091 Uiso 1 1 calc GR . . . .
H69B H 0.1182 0.3380 0.9802 0.091 Uiso 1 1 calc GR . . . .
H69C H 0.1161 0.2570 0.9735 0.091 Uiso 1 1 calc GR . . . .
C134 C 0.8215(3) 0.47485(13) 0.49656(7) 0.0673(8) Uani 1 1 d . . . . .
H13J H 0.7971 0.5091 0.4837 0.101 Uiso 1 1 calc GR . . . .
H13K H 0.7884 0.4307 0.4852 0.101 Uiso 1 1 calc GR . . . .
H13L H 0.9080 0.4723 0.4968 0.101 Uiso 1 1 calc GR . . . .
C68 C 0.3265(4) 0.31064(13) 1.00265(6) 0.0841(12) Uani 1 1 d . . . . .
H68A H 0.2997 0.2750 1.0144 0.126 Uiso 1 1 calc GR . . . .
H68B H 0.2957 0.3544 1.0150 0.126 Uiso 1 1 calc GR . . . .
H68C H 0.4132 0.3123 1.0027 0.126 Uiso 1 1 calc GR . . . .
C133 C 0.6446(2) 0.49758(17) 0.53322(9) 0.0885(12) Uani 1 1 d . . . . .
H13M H 0.6152 0.5080 0.5573 0.133 Uiso 1 1 calc GR . . . .
H13N H 0.6120 0.4539 0.5209 0.133 Uiso 1 1 calc GR . . . .
H13O H 0.6199 0.5331 0.5212 0.133 Uiso 1 1 calc GR . . . .
H82 H 0.2975(18) 0.8611(10) 0.8921(5) 0.026(5) Uiso 1 1 d . . . . .
H2 H 0.8040(18) -0.0781(10) 0.6114(5) 0.029(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
Ca1 O1 2.4332(11) . ?
Ca1 N1 2.3273(12) . ?
Ca1 N2 2.3299(13) . ?
Ca1 N3 2.2927(12) . ?
Ca2 O2 2.4230(11) . ?
Ca2 N5 2.3324(12) . ?
Ca2 N6 2.3441(12) . ?
Ca2 N7 2.3054(12) . ?
Ca3 O3 2.4187(12) . ?
Ca3 N9 2.3334(12) . ?
Ca3 N10 2.3371(12) . ?
Ca3 N11 2.2948(12) . ?
Ca4 O4 2.4235(10) . ?
Ca4 N14 2.3299(12) . ?
Ca4 N13 2.3530(13) . ?
Ca4 N15 2.3080(12) . ?
Si8 N15 1.6938(14) . ?
Si8 C154 1.8886(17) . ?
Si8 C155 1.8847(17) . ?
Si8 C153 1.8840(17) . ?
Si2 N3 1.6889(14) . ?
Si2 C34 1.8816(17) . ?
Si2 C33 1.8786(17) . ?
Si2 C35 1.8816(17) . ?
Si4 N7 1.6940(13) . ?
Si4 C75 1.8832(19) . ?
Si4 C73 1.8839(16) . ?
Si4 C74 1.8841(18) . ?
Si1 N3 1.7004(13) . ?
Si1 C32 1.8857(17) . ?
Si1 C31 1.8854(16) . ?
Si1 C30 1.8792(19) . ?
Si6 N11 1.6924(13) . ?
Si6 C114 1.8797(17) . ?
Si6 C115 1.8899(18) . ?
Si6 C113 1.8840(18) . ?
Si5 N11 1.6988(14) . ?
Si5 C112 1.8913(17) . ?
Si5 C111 1.879(2) . ?
Si5 C110 1.8845(17) . ?
Si7 N15 1.6958(13) . ?
Si7 C150 1.8896(18) . ?
Si7 C152 1.8844(18) . ?
Si7 C151 1.8832(18) . ?
Si3 N7 1.6977(14) . ?
Si3 C72 1.8855(17) . ?
Si3 C71 1.8812(17) . ?
Si3 C70 1.8828(19) . ?
O4 C156 1.4454(18) . ?
O4 C158 1.4453(19) . ?
O1 C38 1.4417(19) . ?
O1 C36 1.444(2) . ?
O2 C78 1.4456(18) . ?
O2 C76 1.449(2) . ?
O3 C118 1.443(2) . ?
O3 C116 1.4462(19) . ?
N9 C81 1.3335(19) . ?
N9 C86 1.4275(17) . ?
N14 C123 1.3247(19) . ?
N14 C138 1.4303(18) . ?
N1 C6 1.4289(18) . ?
N1 C1 1.3316(18) . ?
N5 C43 1.328(2) . ?
N5 C58 1.427(2) . ?
N2 C18 1.432(2) . ?
N2 C3 1.3266(19) . ?
N10 C83 1.322(2) . ?
N10 C98 1.429(2) . ?
N6 C41 1.3248(19) . ?
N6 C46 1.4352(18) . ?
N13 C121 1.3305(19) . ?
N13 C126 1.432(2) . ?
N12 C119 1.455(2) . ?
N12 C117 1.457(2) . ?
N12 C120 1.455(2) . ?
N8 C79 1.454(2) . ?
N8 C77 1.459(2) . ?
N8 C80 1.462(2) . ?
N16 C157 1.462(2) . ?
N16 C159 1.456(2) . ?
N16 C160 1.460(2) . ?
N4 C39 1.451(2) . ?
N4 C37 1.458(2) . ?
N4 C40 1.467(2) . ?
C6 C11 1.417(2) . ?
C6 C7 1.405(2) . ?
C123 C122 1.422(2) . ?
C123 C125 1.5174(19) . ?
C81 C82 1.411(2) . ?
C81 C84 1.518(2) . ?
C43 C42 1.412(2) . ?
C43 C45 1.5176(19) . ?
C18 C19 1.404(2) . ?
C18 C23 1.412(2) . ?
C87 C86 1.416(2) . ?
C87 C88 1.396(2) . ?
C87 C92 1.523(2) . ?
C138 C143 1.410(2) . ?
C138 C139 1.408(2) . ?
C1 C2 1.412(2) . ?
C1 C4 1.516(2) . ?
C122 H122 0.9500 . ?
C122 C121 1.411(2) . ?
C90 H90 0.9500 . ?
C90 C91 1.396(2) . ?
C90 C89 1.381(2) . ?
C3 C2 1.413(2) . ?
C3 C5 1.515(2) . ?
C41 C42 1.423(2) . ?
C41 C44 1.515(2) . ?
C143 C142 1.397(2) . ?
C143 C147 1.519(3) . ?
C58 C63 1.409(2) . ?
C58 C59 1.410(2) . ?
C83 C82 1.422(2) . ?
C83 C85 1.513(2) . ?
C11 C10 1.395(2) . ?
C11 C15 1.520(2) . ?
C9 H9 0.9500 . ?
C9 C8 1.382(2) . ?
C9 C10 1.383(2) . ?
C63 C64 1.520(2) . ?
C63 C62 1.392(2) . ?
C121 C124 1.519(2) . ?
C86 C91 1.405(2) . ?
C103 C98 1.407(2) . ?
C103 C107 1.522(2) . ?
C103 C102 1.393(3) . ?
C2 H2 0.97(2) . ?
C82 H82 0.96(2) . ?
C7 C8 1.399(2) . ?
C7 C12 1.517(2) . ?
C126 C131 1.410(2) . ?
C126 C127 1.413(2) . ?
C139 C140 1.399(2) . ?
C139 C144 1.519(2) . ?
C51 C46 1.412(2) . ?
C51 C55 1.522(2) . ?
C51 C50 1.399(2) . ?
C8 H8 0.9500 . ?
C88 H88 0.9500 . ?
C88 C89 1.382(2) . ?
C19 C24 1.522(2) . ?
C19 C20 1.398(2) . ?
C98 C99 1.409(2) . ?
C46 C47 1.409(2) . ?
C91 C95 1.518(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C140 H140 0.9500 . ?
C140 C141 1.379(3) . ?
C89 H89 0.9500 . ?
C10 H10 0.9500 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C64 H64 1.0000 . ?
C64 C65 1.535(2) . ?
C64 C66 1.532(2) . ?
C42 H42 0.9500 . ?
C131 C135 1.516(2) . ?
C131 C130 1.394(2) . ?
C23 C22 1.396(2) . ?
C23 C27 1.513(2) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C99 C100 1.392(3) . ?
C99 C104 1.519(2) . ?
C62 H62 0.9500 . ?
C62 C61 1.382(2) . ?
C15 H15 1.0000 . ?
C15 C16 1.534(2) . ?
C15 C17 1.535(2) . ?
C92 H92 1.0000 . ?
C92 C93 1.530(3) . ?
C92 C94 1.533(2) . ?
C78 H78A 0.9900 . ?
C78 H78B 0.9900 . ?
C78 C79 1.510(2) . ?
C156 H15A 0.9900 . ?
C156 H15B 0.9900 . ?
C156 C157 1.510(2) . ?
C47 C48 1.397(2) . ?
C47 C52 1.520(2) . ?
C24 H24 1.0000 . ?
C24 C25 1.523(2) . ?
C24 C26 1.526(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(3) . ?
C127 C128 1.390(3) . ?
C127 C132 1.530(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.380(3) . ?
C59 C60 1.390(2) . ?
C59 C67 1.528(2) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C125 H12D 0.9800 . ?
C125 H12E 0.9800 . ?
C125 H12F 0.9800 . ?
C12 H12 1.0000 . ?
C12 C13 1.527(2) . ?
C12 C14 1.530(2) . ?
C49 H49 0.9500 . ?
C49 C50 1.379(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.379(3) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C76 C77 1.515(2) . ?
C60 H60 0.9500 . ?
C60 C61 1.387(2) . ?
C79 H79A 0.9900 . ?
C79 H79B 0.9900 . ?
C107 H107 1.0000 . ?
C107 C109 1.528(2) . ?
C107 C108 1.527(2) . ?
C144 H144 1.0000 . ?
C144 C146 1.531(2) . ?
C144 C145 1.525(2) . ?
C124 H12G 0.9800 . ?
C124 H12H 0.9800 . ?
C124 H12I 0.9800 . ?
C141 H141 0.9500 . ?
C141 C142 1.373(3) . ?
C154 H15C 0.9800 . ?
C154 H15D 0.9800 . ?
C154 H15E 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.508(2) . ?
C100 H100 0.9500 . ?
C100 C101 1.379(3) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C157 H15F 0.9900 . ?
C157 H15G 0.9900 . ?
C142 H142 0.9500 . ?
C155 H15H 0.9800 . ?
C155 H15I 0.9800 . ?
C155 H15J 0.9800 . ?
C150 H15K 0.9800 . ?
C150 H15L 0.9800 . ?
C150 H15M 0.9800 . ?
C135 H135 1.0000 . ?
C135 C136 1.533(2) . ?
C135 C137 1.530(3) . ?
C55 H55 1.0000 . ?
C55 C57 1.528(3) . ?
C55 C56 1.537(3) . ?
C27 H27 1.0000 . ?
C27 C28 1.529(2) . ?
C27 C29 1.534(2) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C130 H130 0.9500 . ?
C130 C129 1.378(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C159 H15N 0.9900 . ?
C159 H15O 0.9900 . ?
C159 C158 1.513(2) . ?
C61 H61 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C102 H102 0.9500 . ?
C102 C101 1.382(3) . ?
C118 H11A 0.9900 . ?
C118 H11B 0.9900 . ?
C118 C119 1.510(2) . ?
C119 H11C 0.9900 . ?
C119 H11D 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C114 H11E 0.9800 . ?
C114 H11F 0.9800 . ?
C114 H11G 0.9800 . ?
C52 H52 1.0000 . ?
C52 C53 1.528(2) . ?
C52 C54 1.526(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C146 H14D 0.9800 . ?
C146 H14E 0.9800 . ?
C146 H14F 0.9800 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.511(2) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C158 H15P 0.9900 . ?
C158 H15Q 0.9900 . ?
C112 H11H 0.9800 . ?
C112 H11I 0.9800 . ?
C112 H11J 0.9800 . ?
C129 H129 0.9500 . ?
C129 C128 1.385(3) . ?
C101 H101 0.9500 . ?
C147 H147 1.0000 . ?
C147 C149 1.522(3) . ?
C147 C148 1.533(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C109 H10A 0.9800 . ?
C109 H10B 0.9800 . ?
C109 H10C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C21 H21 0.9500 . ?
C50 H50 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C128 H128 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C117 H11K 0.9900 . ?
C117 H11L 0.9900 . ?
C117 C116 1.514(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C95 H95 1.0000 . ?
C95 C96 1.526(3) . ?
C95 C97 1.527(3) . ?
C116 H11M 0.9900 . ?
C116 H11N 0.9900 . ?
C115 H11O 0.9800 . ?
C115 H11P 0.9800 . ?
C115 H11Q 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C132 H132 1.0000 . ?
C132 C134 1.511(3) . ?
C132 C133 1.495(3) . ?
C136 H13D 0.9800 . ?
C136 H13E 0.9800 . ?
C136 H13F 0.9800 . ?
C111 H11R 0.9800 . ?
C111 H11S 0.9800 . ?
C111 H11T 0.9800 . ?
C67 H67 1.0000 . ?
C67 C69 1.531(3) . ?
C67 C68 1.512(3) . ?
C104 H104 1.0000 . ?
C104 C106 1.521(3) . ?
C104 C105 1.527(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C160 H16D 0.9800 . ?
C160 H16E 0.9800 . ?
C160 H16F 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C152 H15R 0.9800 . ?
C152 H15S 0.9800 . ?
C152 H15T 0.9800 . ?
C153 H15U 0.9800 . ?
C153 H15V 0.9800 . ?
C153 H15W 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C113 H11U 0.9800 . ?
C113 H11V 0.9800 . ?
C113 H11W 0.9800 . ?
C110 H11X 0.9800 . ?
C110 H11Y 0.9800 . ?
C110 H 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C137 H13G 0.9800 . ?
C137 H13H 0.9800 . ?
C137 H13I 0.9800 . ?
C151 H15X 0.9800 . ?
C151 H15Y 0.9800 . ?
C151 HA 0.9800 . ?
C145 H14G 0.9800 . ?
C145 H14H 0.9800 . ?
C145 H14I 0.9800 . ?
C149 H14J 0.9800 . ?
C149 H14K 0.9800 . ?
C149 H14L 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C120 H12A 0.9800 . ?
C120 H12B 0.9800 . ?
C120 H12C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C148 H14M 0.9800 . ?
C148 H14N 0.9800 . ?
C148 H14O 0.9800 . ?
C106 H10D 0.9800 . ?
C106 H10E 0.9800 . ?
C106 H10F 0.9800 . ?
C108 H10G 0.9800 . ?
C108 H10H 0.9800 . ?
C108 H10I 0.9800 . ?
C105 H10J 0.9800 . ?
C105 H10K 0.9800 . ?
C105 H10L 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C134 H13J 0.9800 . ?
C134 H13K 0.9800 . ?
C134 H13L 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C133 H13M 0.9800 . ?
C133 H13N 0.9800 . ?
C133 H13O 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ca1 O1 100.58(4) . . ?
N1 Ca1 N2 83.23(4) . . ?
N2 Ca1 O1 102.21(4) . . ?
N3 Ca1 O1 118.77(4) . . ?
N3 Ca1 N1 125.82(4) . . ?
N3 Ca1 N2 119.06(5) . . ?
N5 Ca2 O2 99.44(4) . . ?
N5 Ca2 N6 83.49(4) . . ?
N6 Ca2 O2 109.84(4) . . ?
N7 Ca2 O2 110.04(4) . . ?
N7 Ca2 N5 132.18(5) . . ?
N7 Ca2 N6 118.23(4) . . ?
N9 Ca3 O3 97.39(4) . . ?
N9 Ca3 N10 83.31(4) . . ?
N10 Ca3 O3 109.77(4) . . ?
N11 Ca3 O3 112.17(4) . . ?
N11 Ca3 N9 135.10(4) . . ?
N11 Ca3 N10 114.88(5) . . ?
N14 Ca4 O4 107.00(4) . . ?
N14 Ca4 N13 83.50(4) . . ?
N13 Ca4 O4 100.44(4) . . ?
N15 Ca4 O4 109.70(4) . . ?
N15 Ca4 N14 115.40(4) . . ?
N15 Ca4 N13 136.26(5) . . ?
N15 Si8 C154 115.78(7) . . ?
N15 Si8 C155 111.45(7) . . ?
N15 Si8 C153 113.20(8) . . ?
C155 Si8 C154 105.35(8) . . ?
C153 Si8 C154 104.26(8) . . ?
C153 Si8 C155 105.96(8) . . ?
N3 Si2 C34 114.03(8) . . ?
N3 Si2 C33 115.28(7) . . ?
N3 Si2 C35 111.08(7) . . ?
C34 Si2 C35 106.95(8) . . ?
C33 Si2 C34 105.27(8) . . ?
C33 Si2 C35 103.34(8) . . ?
N7 Si4 C75 111.73(7) . . ?
N7 Si4 C73 115.61(7) . . ?
N7 Si4 C74 113.34(8) . . ?
C75 Si4 C73 104.91(9) . . ?
C75 Si4 C74 106.16(9) . . ?
C73 Si4 C74 104.23(8) . . ?
N3 Si1 C32 108.95(7) . . ?
N3 Si1 C31 115.37(8) . . ?
N3 Si1 C30 112.94(7) . . ?
C31 Si1 C32 105.31(8) . . ?
C30 Si1 C32 107.30(9) . . ?
C30 Si1 C31 106.43(8) . . ?
N11 Si6 C114 113.26(7) . . ?
N11 Si6 C115 111.29(7) . . ?
N11 Si6 C113 115.26(8) . . ?
C114 Si6 C115 106.42(8) . . ?
C114 Si6 C113 104.22(8) . . ?
C113 Si6 C115 105.64(9) . . ?
N11 Si5 C112 109.08(7) . . ?
N11 Si5 C111 113.53(8) . . ?
N11 Si5 C110 115.16(8) . . ?
C111 Si5 C112 106.57(9) . . ?
C111 Si5 C110 106.87(9) . . ?
C110 Si5 C112 104.96(8) . . ?
N15 Si7 C150 109.19(7) . . ?
N15 Si7 C152 114.63(8) . . ?
N15 Si7 C151 114.56(8) . . ?
C152 Si7 C150 105.04(9) . . ?
C151 Si7 C150 106.11(9) . . ?
C151 Si7 C152 106.59(9) . . ?
N7 Si3 C72 109.48(7) . . ?
N7 Si3 C71 114.14(8) . . ?
N7 Si3 C70 114.62(8) . . ?
C71 Si3 C72 105.63(8) . . ?
C71 Si3 C70 106.69(9) . . ?
C70 Si3 C72 105.57(9) . . ?
C156 O4 Ca4 127.56(9) . . ?
C158 O4 Ca4 123.66(9) . . ?
C158 O4 C156 108.71(11) . . ?
C38 O1 Ca1 128.97(9) . . ?
C38 O1 C36 109.39(12) . . ?
C36 O1 Ca1 121.41(9) . . ?
C78 O2 Ca2 127.55(10) . . ?
C78 O2 C76 108.54(12) . . ?
C76 O2 Ca2 123.86(9) . . ?
C118 O3 Ca3 126.86(9) . . ?
C118 O3 C116 109.55(12) . . ?
C116 O3 Ca3 123.56(10) . . ?
C81 N9 Ca3 102.37(8) . . ?
C81 N9 C86 117.87(12) . . ?
C86 N9 Ca3 135.03(9) . . ?
C123 N14 Ca4 105.27(9) . . ?
C123 N14 C138 119.19(11) . . ?
C138 N14 Ca4 134.10(9) . . ?
C6 N1 Ca1 134.04(9) . . ?
C1 N1 Ca1 104.63(8) . . ?
C1 N1 C6 117.58(11) . . ?
C43 N5 Ca2 100.93(10) . . ?
C43 N5 C58 118.65(12) . . ?
C58 N5 Ca2 134.48(9) . . ?
C18 N2 Ca1 129.13(9) . . ?
C3 N2 Ca1 106.20(10) . . ?
C3 N2 C18 120.14(13) . . ?
C83 N10 Ca3 105.95(10) . . ?
C83 N10 C98 120.32(12) . . ?
C98 N10 Ca3 130.56(9) . . ?
C41 N6 Ca2 104.13(9) . . ?
C41 N6 C46 119.48(12) . . ?
C46 N6 Ca2 134.04(9) . . ?
Si6 N11 Ca3 126.71(7) . . ?
Si6 N11 Si5 124.41(8) . . ?
Si5 N11 Ca3 108.88(6) . . ?
C121 N13 Ca4 101.04(10) . . ?
C121 N13 C126 118.68(13) . . ?
C126 N13 Ca4 133.24(10) . . ?
Si2 N3 Ca1 123.97(7) . . ?
Si2 N3 Si1 124.71(7) . . ?
Si1 N3 Ca1 111.21(7) . . ?
Si4 N7 Ca2 126.50(7) . . ?
Si4 N7 Si3 124.84(7) . . ?
Si3 N7 Ca2 108.64(6) . . ?
Si8 N15 Ca4 127.03(6) . . ?
Si8 N15 Si7 125.28(7) . . ?
Si7 N15 Ca4 107.59(6) . . ?
C119 N12 C117 109.04(14) . . ?
C119 N12 C120 111.61(15) . . ?
C120 N12 C117 111.66(15) . . ?
C79 N8 C77 109.30(13) . . ?
C79 N8 C80 110.84(15) . . ?
C77 N8 C80 110.47(14) . . ?
C159 N16 C157 108.86(12) . . ?
C159 N16 C160 110.72(14) . . ?
C160 N16 C157 110.47(15) . . ?
C39 N4 C37 108.81(13) . . ?
C39 N4 C40 110.74(17) . . ?
C37 N4 C40 111.10(15) . . ?
C11 C6 N1 119.24(14) . . ?
C7 C6 N1 120.55(13) . . ?
C7 C6 C11 120.18(13) . . ?
N14 C123 C122 124.03(13) . . ?
N14 C123 C125 121.43(13) . . ?
C122 C123 C125 114.49(12) . . ?
N9 C81 C82 124.41(14) . . ?
N9 C81 C84 119.99(13) . . ?
C82 C81 C84 115.59(13) . . ?
N5 C43 C42 124.19(13) . . ?
N5 C43 C45 120.09(14) . . ?
C42 C43 C45 115.69(13) . . ?
C19 C18 N2 118.92(14) . . ?
C19 C18 C23 120.51(15) . . ?
C23 C18 N2 120.39(14) . . ?
C86 C87 C92 122.38(13) . . ?
C88 C87 C86 118.33(14) . . ?
C88 C87 C92 119.22(13) . . ?
C143 C138 N14 118.64(14) . . ?
C139 C138 N14 120.93(13) . . ?
C139 C138 C143 120.35(13) . . ?
N1 C1 C2 124.73(13) . . ?
N1 C1 C4 120.21(13) . . ?
C2 C1 C4 115.03(12) . . ?
C123 C122 H122 114.1 . . ?
C121 C122 C123 131.85(13) . . ?
C121 C122 H122 114.1 . . ?
C91 C90 H90 119.4 . . ?
C89 C90 H90 119.4 . . ?
C89 C90 C91 121.18(14) . . ?
N2 C3 C2 124.00(14) . . ?
N2 C3 C5 120.94(14) . . ?
C2 C3 C5 115.03(13) . . ?
N6 C41 C42 124.19(14) . . ?
N6 C41 C44 121.59(13) . . ?
C42 C41 C44 114.21(13) . . ?
C138 C143 C147 122.76(14) . . ?
C142 C143 C138 118.43(16) . . ?
C142 C143 C147 118.78(15) . . ?
C63 C58 N5 121.36(14) . . ?
C63 C58 C59 119.78(15) . . ?
C59 C58 N5 118.78(13) . . ?
N10 C83 C82 124.22(13) . . ?
N10 C83 C85 121.63(14) . . ?
C82 C83 C85 114.13(13) . . ?
C6 C11 C15 122.48(13) . . ?
C10 C11 C6 118.22(15) . . ?
C10 C11 C15 119.27(14) . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.28(14) . . ?
C10 C9 H9 120.4 . . ?
C58 C63 C64 121.94(15) . . ?
C62 C63 C58 119.14(15) . . ?
C62 C63 C64 118.90(14) . . ?
N13 C121 C122 124.46(13) . . ?
N13 C121 C124 120.34(14) . . ?
C122 C121 C124 115.18(13) . . ?
C87 C86 N9 119.49(13) . . ?
C91 C86 N9 120.52(12) . . ?
C91 C86 C87 119.94(13) . . ?
C98 C103 C107 121.59(15) . . ?
C102 C103 C98 118.89(14) . . ?
C102 C103 C107 119.52(15) . . ?
C1 C2 C3 131.64(13) . . ?
C1 C2 H2 116.4(12) . . ?
C3 C2 H2 110.9(12) . . ?
C81 C82 C83 131.12(14) . . ?
C81 C82 H82 114.7(12) . . ?
C83 C82 H82 113.1(12) . . ?
C6 C7 C12 122.80(13) . . ?
C8 C7 C6 119.07(14) . . ?
C8 C7 C12 118.08(14) . . ?
C131 C126 N13 120.29(15) . . ?
C131 C126 C127 119.88(15) . . ?
C127 C126 N13 119.71(13) . . ?
C138 C139 C144 121.91(13) . . ?
C140 C139 C138 118.43(15) . . ?
C140 C139 C144 119.63(15) . . ?
C46 C51 C55 123.30(14) . . ?
C50 C51 C46 118.36(15) . . ?
C50 C51 C55 118.30(15) . . ?
C9 C8 C7 121.23(15) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C87 C88 H88 119.1 . . ?
C89 C88 C87 121.90(14) . . ?
C89 C88 H88 119.1 . . ?
C18 C19 C24 121.36(15) . . ?
C20 C19 C18 118.62(15) . . ?
C20 C19 C24 120.02(15) . . ?
C103 C98 N10 119.53(13) . . ?
C103 C98 C99 119.99(16) . . ?
C99 C98 N10 120.36(14) . . ?
C51 C46 N6 119.81(14) . . ?
C47 C46 N6 119.57(13) . . ?
C47 C46 C51 120.50(14) . . ?
C90 C91 C86 119.31(13) . . ?
C90 C91 C95 118.40(14) . . ?
C86 C91 C95 122.25(13) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C139 C140 H140 119.3 . . ?
C141 C140 C139 121.39(16) . . ?
C141 C140 H140 119.3 . . ?
C90 C89 C88 119.27(13) . . ?
C90 C89 H89 120.4 . . ?
C88 C89 H89 120.4 . . ?
C11 C10 H10 119.0 . . ?
C9 C10 C11 121.94(15) . . ?
C9 C10 H10 119.0 . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C63 C64 H64 107.9 . . ?
C63 C64 C65 112.65(13) . . ?
C63 C64 C66 110.41(15) . . ?
C65 C64 H64 107.9 . . ?
C66 C64 H64 107.9 . . ?
C66 C64 C65 110.00(13) . . ?
C43 C42 C41 131.57(14) . . ?
C43 C42 H42 114.2 . . ?
C41 C42 H42 114.2 . . ?
C126 C131 C135 122.06(15) . . ?
C130 C131 C126 119.15(16) . . ?
C130 C131 C135 118.78(14) . . ?
C18 C23 C27 121.99(15) . . ?
C22 C23 C18 118.50(16) . . ?
C22 C23 C27 119.49(15) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C98 C99 C104 121.99(16) . . ?
C100 C99 C98 118.83(16) . . ?
C100 C99 C104 119.18(14) . . ?
C63 C62 H62 119.3 . . ?
C61 C62 C63 121.37(15) . . ?
C61 C62 H62 119.3 . . ?
C11 C15 H15 108.2 . . ?
C11 C15 C16 110.02(13) . . ?
C11 C15 C17 112.88(14) . . ?
C16 C15 H15 108.2 . . ?
C16 C15 C17 109.34(14) . . ?
C17 C15 H15 108.2 . . ?
C87 C92 H92 108.1 . . ?
C87 C92 C93 109.51(13) . . ?
C87 C92 C94 113.00(14) . . ?
C93 C92 H92 108.1 . . ?
C93 C92 C94 109.81(13) . . ?
C94 C92 H92 108.1 . . ?
O2 C78 H78A 109.5 . . ?
O2 C78 H78B 109.5 . . ?
O2 C78 C79 110.85(12) . . ?
H78A C78 H78B 108.1 . . ?
C79 C78 H78A 109.5 . . ?
C79 C78 H78B 109.5 . . ?
O4 C156 H15A 109.5 . . ?
O4 C156 H15B 109.5 . . ?
O4 C156 C157 110.73(13) . . ?
H15A C156 H15B 108.1 . . ?
C157 C156 H15A 109.5 . . ?
C157 C156 H15B 109.5 . . ?
C46 C47 C52 121.63(13) . . ?
C48 C47 C46 118.54(15) . . ?
C48 C47 C52 119.74(15) . . ?
C19 C24 H24 107.2 . . ?
C19 C24 C25 112.37(14) . . ?
C19 C24 C26 111.65(15) . . ?
C25 C24 H24 107.2 . . ?
C25 C24 C26 110.92(16) . . ?
C26 C24 H24 107.2 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.32(17) . . ?
C21 C20 H20 119.3 . . ?
C126 C127 C132 121.63(15) . . ?
C128 C127 C126 118.58(15) . . ?
C128 C127 C132 119.77(16) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 C47 121.38(16) . . ?
C49 C48 H48 119.3 . . ?
C58 C59 C67 121.29(15) . . ?
C60 C59 C58 118.93(14) . . ?
C60 C59 C67 119.76(15) . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C123 C125 H12D 109.5 . . ?
C123 C125 H12E 109.5 . . ?
C123 C125 H12F 109.5 . . ?
H12D C125 H12E 109.5 . . ?
H12D C125 H12F 109.5 . . ?
H12E C125 H12F 109.5 . . ?
C7 C12 H12 107.5 . . ?
C7 C12 C13 112.35(14) . . ?
C7 C12 C14 111.43(13) . . ?
C13 C12 H12 107.5 . . ?
C13 C12 C14 110.42(15) . . ?
C14 C12 H12 107.5 . . ?
C48 C49 H49 120.1 . . ?
C50 C49 C48 119.74(15) . . ?
C50 C49 H49 120.1 . . ?
C23 C22 H22 119.3 . . ?
C21 C22 C23 121.43(16) . . ?
C21 C22 H22 119.3 . . ?
O2 C76 H76A 109.5 . . ?
O2 C76 H76B 109.5 . . ?
O2 C76 C77 110.68(14) . . ?
H76A C76 H76B 108.1 . . ?
C77 C76 H76A 109.5 . . ?
C77 C76 H76B 109.5 . . ?
C59 C60 H60 119.3 . . ?
C61 C60 C59 121.49(15) . . ?
C61 C60 H60 119.3 . . ?
N8 C79 C78 109.93(14) . . ?
N8 C79 H79A 109.7 . . ?
N8 C79 H79B 109.7 . . ?
C78 C79 H79A 109.7 . . ?
C78 C79 H79B 109.7 . . ?
H79A C79 H79B 108.2 . . ?
C103 C107 H107 107.7 . . ?
C103 C107 C109 111.45(14) . . ?
C103 C107 C108 111.46(14) . . ?
C109 C107 H107 107.7 . . ?
C108 C107 H107 107.7 . . ?
C108 C107 C109 110.51(15) . . ?
C139 C144 H144 107.4 . . ?
C139 C144 C146 113.03(14) . . ?
C139 C144 C145 111.15(13) . . ?
C146 C144 H144 107.4 . . ?
C145 C144 H144 107.4 . . ?
C145 C144 C146 110.16(15) . . ?
C121 C124 H12G 109.5 . . ?
C121 C124 H12H 109.5 . . ?
C121 C124 H12I 109.5 . . ?
H12G C124 H12H 109.5 . . ?
H12G C124 H12I 109.5 . . ?
H12H C124 H12I 109.5 . . ?
C140 C141 H141 120.2 . . ?
C142 C141 C140 119.68(14) . . ?
C142 C141 H141 120.2 . . ?
Si8 C154 H15C 109.5 . . ?
Si8 C154 H15D 109.5 . . ?
Si8 C154 H15E 109.5 . . ?
H15C C154 H15D 109.5 . . ?
H15C C154 H15E 109.5 . . ?
H15D C154 H15E 109.5 . . ?
O1 C38 H38A 109.3 . . ?
O1 C38 H38B 109.3 . . ?
O1 C38 C39 111.55(13) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.3 . . ?
C39 C38 H38B 109.3 . . ?
C99 C100 H100 119.3 . . ?
C101 C100 C99 121.44(15) . . ?
C101 C100 H100 119.3 . . ?
Si4 C75 H75A 109.5 . . ?
Si4 C75 H75B 109.5 . . ?
Si4 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N16 C157 C156 109.69(14) . . ?
N16 C157 H15F 109.7 . . ?
N16 C157 H15G 109.7 . . ?
C156 C157 H15F 109.7 . . ?
C156 C157 H15G 109.7 . . ?
H15F C157 H15G 108.2 . . ?
C143 C142 H142 119.2 . . ?
C141 C142 C143 121.57(16) . . ?
C141 C142 H142 119.2 . . ?
Si8 C155 H15H 109.5 . . ?
Si8 C155 H15I 109.5 . . ?
Si8 C155 H15J 109.5 . . ?
H15H C155 H15I 109.5 . . ?
H15H C155 H15J 109.5 . . ?
H15I C155 H15J 109.5 . . ?
Si7 C150 H15K 109.5 . . ?
Si7 C150 H15L 109.5 . . ?
Si7 C150 H15M 109.5 . . ?
H15K C150 H15L 109.5 . . ?
H15K C150 H15M 109.5 . . ?
H15L C150 H15M 109.5 . . ?
C131 C135 H135 107.6 . . ?
C131 C135 C136 112.89(14) . . ?
C131 C135 C137 111.15(15) . . ?
C136 C135 H135 107.6 . . ?
C137 C135 H135 107.6 . . ?
C137 C135 C136 109.73(14) . . ?
C51 C55 H55 108.2 . . ?
C51 C55 C57 110.16(15) . . ?
C51 C55 C56 112.62(16) . . ?
C57 C55 H55 108.2 . . ?
C57 C55 C56 109.25(16) . . ?
C56 C55 H55 108.2 . . ?
C23 C27 H27 107.7 . . ?
C23 C27 C28 110.24(14) . . ?
C23 C27 C29 112.71(15) . . ?
C28 C27 H27 107.7 . . ?
C28 C27 C29 110.70(15) . . ?
C29 C27 H27 107.7 . . ?
Si3 C72 H72A 109.5 . . ?
Si3 C72 H72B 109.5 . . ?
Si3 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C131 C130 H130 119.4 . . ?
C129 C130 C131 121.12(16) . . ?
C129 C130 H130 119.4 . . ?
Si2 C34 H34A 109.5 . . ?
Si2 C34 H34B 109.5 . . ?
Si2 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N16 C159 H15N 109.6 . . ?
N16 C159 H15O 109.6 . . ?
N16 C159 C158 110.40(13) . . ?
H15N C159 H15O 108.1 . . ?
C158 C159 H15N 109.6 . . ?
C158 C159 H15O 109.6 . . ?
C62 C61 C60 119.18(16) . . ?
C62 C61 H61 120.4 . . ?
C60 C61 H61 120.4 . . ?
Si2 C33 H33A 109.5 . . ?
Si2 C33 H33B 109.5 . . ?
Si2 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C103 C102 H102 119.3 . . ?
C101 C102 C103 121.33(16) . . ?
C101 C102 H102 119.3 . . ?
O3 C118 H11A 109.5 . . ?
O3 C118 H11B 109.5 . . ?
O3 C118 C119 110.78(13) . . ?
H11A C118 H11B 108.1 . . ?
C119 C118 H11A 109.5 . . ?
C119 C118 H11B 109.5 . . ?
N12 C119 C118 109.04(14) . . ?
N12 C119 H11C 109.9 . . ?
N12 C119 H11D 109.9 . . ?
C118 C119 H11C 109.9 . . ?
C118 C119 H11D 109.9 . . ?
H11C C119 H11D 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si6 C114 H11E 109.5 . . ?
Si6 C114 H11F 109.5 . . ?
Si6 C114 H11G 109.5 . . ?
H11E C114 H11F 109.5 . . ?
H11E C114 H11G 109.5 . . ?
H11F C114 H11G 109.5 . . ?
C47 C52 H52 107.2 . . ?
C47 C52 C53 113.49(14) . . ?
C47 C52 C54 111.06(14) . . ?
C53 C52 H52 107.2 . . ?
C54 C52 H52 107.2 . . ?
C54 C52 C53 110.35(15) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N8 C77 C76 110.10(13) . . ?
N8 C77 H77A 109.6 . . ?
N8 C77 H77B 109.6 . . ?
C76 C77 H77A 109.6 . . ?
C76 C77 H77B 109.6 . . ?
H77A C77 H77B 108.2 . . ?
Si2 C35 H35A 109.5 . . ?
Si2 C35 H35B 109.5 . . ?
Si2 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C144 C146 H14D 109.5 . . ?
C144 C146 H14E 109.5 . . ?
C144 C146 H14F 109.5 . . ?
H14D C146 H14E 109.5 . . ?
H14D C146 H14F 109.5 . . ?
H14E C146 H14F 109.5 . . ?
O1 C36 H36A 109.4 . . ?
O1 C36 H36B 109.4 . . ?
O1 C36 C37 111.38(14) . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 H36A 109.4 . . ?
C37 C36 H36B 109.4 . . ?
C83 C85 H85A 109.5 . . ?
C83 C85 H85B 109.5 . . ?
C83 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O4 C158 C159 110.58(13) . . ?
O4 C158 H15P 109.5 . . ?
O4 C158 H15Q 109.5 . . ?
C159 C158 H15P 109.5 . . ?
C159 C158 H15Q 109.5 . . ?
H15P C158 H15Q 108.1 . . ?
Si5 C112 H11H 109.5 . . ?
Si5 C112 H11I 109.5 . . ?
Si5 C112 H11J 109.5 . . ?
H11H C112 H11I 109.5 . . ?
H11H C112 H11J 109.5 . . ?
H11I C112 H11J 109.5 . . ?
C130 C129 H129 120.3 . . ?
C130 C129 C128 119.49(17) . . ?
C128 C129 H129 120.3 . . ?
C100 C101 C102 119.44(17) . . ?
C100 C101 H101 120.3 . . ?
C102 C101 H101 120.3 . . ?
C143 C147 H147 108.0 . . ?
C143 C147 C149 110.25(18) . . ?
C143 C147 C148 112.11(16) . . ?
C149 C147 H147 108.0 . . ?
C149 C147 C148 110.42(16) . . ?
C148 C147 H147 108.0 . . ?
N4 C39 C38 109.52(15) . . ?
N4 C39 H39A 109.8 . . ?
N4 C39 H39B 109.8 . . ?
C38 C39 H39A 109.8 . . ?
C38 C39 H39B 109.8 . . ?
H39A C39 H39B 108.2 . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C107 C109 H10A 109.5 . . ?
C107 C109 H10B 109.5 . . ?
C107 C109 H10C 109.5 . . ?
H10A C109 H10B 109.5 . . ?
H10A C109 H10C 109.5 . . ?
H10B C109 H10C 109.5 . . ?
N4 C37 C36 109.93(13) . . ?
N4 C37 H37A 109.7 . . ?
N4 C37 H37B 109.7 . . ?
C36 C37 H37A 109.7 . . ?
C36 C37 H37B 109.7 . . ?
H37A C37 H37B 108.2 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.62(16) . . ?
C22 C21 H21 120.2 . . ?
C51 C50 H50 119.3 . . ?
C49 C50 C51 121.45(16) . . ?
C49 C50 H50 119.3 . . ?
Si4 C73 H73A 109.5 . . ?
Si4 C73 H73B 109.5 . . ?
Si4 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
Si3 C71 H71A 109.5 . . ?
Si3 C71 H71B 109.5 . . ?
Si3 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C127 C128 H128 119.1 . . ?
C129 C128 C127 121.71(17) . . ?
C129 C128 H128 119.1 . . ?
Si4 C74 H74A 109.5 . . ?
Si4 C74 H74B 109.5 . . ?
Si4 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
Si1 C32 H32A 109.5 . . ?
Si1 C32 H32B 109.5 . . ?
Si1 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N12 C117 H11K 109.5 . . ?
N12 C117 H11L 109.5 . . ?
N12 C117 C116 110.56(14) . . ?
H11K C117 H11L 108.1 . . ?
C116 C117 H11K 109.5 . . ?
C116 C117 H11L 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
Si1 C31 H31A 109.5 . . ?
Si1 C31 H31B 109.5 . . ?
Si1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C91 C95 H95 107.5 . . ?
C91 C95 C96 111.68(13) . . ?
C91 C95 C97 112.08(15) . . ?
C96 C95 H95 107.5 . . ?
C96 C95 C97 110.41(15) . . ?
C97 C95 H95 107.5 . . ?
O3 C116 C117 111.04(14) . . ?
O3 C116 H11M 109.4 . . ?
O3 C116 H11N 109.4 . . ?
C117 C116 H11M 109.4 . . ?
C117 C116 H11N 109.4 . . ?
H11M C116 H11N 108.0 . . ?
Si6 C115 H11O 109.5 . . ?
Si6 C115 H11P 109.5 . . ?
Si6 C115 H11Q 109.5 . . ?
H11O C115 H11P 109.5 . . ?
H11O C115 H11Q 109.5 . . ?
H11P C115 H11Q 109.5 . . ?
N8 C80 H80A 109.5 . . ?
N8 C80 H80B 109.5 . . ?
N8 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C127 C132 H132 107.0 . . ?
C134 C132 C127 112.68(17) . . ?
C134 C132 H132 107.0 . . ?
C133 C132 C127 113.43(17) . . ?
C133 C132 H132 107.0 . . ?
C133 C132 C134 109.4(2) . . ?
C135 C136 H13D 109.5 . . ?
C135 C136 H13E 109.5 . . ?
C135 C136 H13F 109.5 . . ?
H13D C136 H13E 109.5 . . ?
H13D C136 H13F 109.5 . . ?
H13E C136 H13F 109.5 . . ?
Si5 C111 H11R 109.5 . . ?
Si5 C111 H11S 109.5 . . ?
Si5 C111 H11T 109.5 . . ?
H11R C111 H11S 109.5 . . ?
H11R C111 H11T 109.5 . . ?
H11S C111 H11T 109.5 . . ?
C59 C67 H67 107.5 . . ?
C59 C67 C69 112.55(16) . . ?
C69 C67 H67 107.5 . . ?
C68 C67 C59 111.74(17) . . ?
C68 C67 H67 107.5 . . ?
C68 C67 C69 109.8(2) . . ?
C99 C104 H104 107.5 . . ?
C99 C104 C106 111.73(17) . . ?
C99 C104 C105 111.76(15) . . ?
C106 C104 H104 107.5 . . ?
C106 C104 C105 110.49(15) . . ?
C105 C104 H104 107.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N16 C160 H16D 109.5 . . ?
N16 C160 H16E 109.5 . . ?
N16 C160 H16F 109.5 . . ?
H16D C160 H16E 109.5 . . ?
H16D C160 H16F 109.5 . . ?
H16E C160 H16F 109.5 . . ?
C92 C94 H94A 109.5 . . ?
C92 C94 H94B 109.5 . . ?
C92 C94 H94C 109.5 . . ?
H94A C94 H94B 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
Si7 C152 H15R 109.5 . . ?
Si7 C152 H15S 109.5 . . ?
Si7 C152 H15T 109.5 . . ?
H15R C152 H15S 109.5 . . ?
H15R C152 H15T 109.5 . . ?
H15S C152 H15T 109.5 . . ?
Si8 C153 H15U 109.5 . . ?
Si8 C153 H15V 109.5 . . ?
Si8 C153 H15W 109.5 . . ?
H15U C153 H15V 109.5 . . ?
H15U C153 H15W 109.5 . . ?
H15V C153 H15W 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C30 H30A 109.5 . . ?
Si1 C30 H30B 109.5 . . ?
Si1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si6 C113 H11U 109.5 . . ?
Si6 C113 H11V 109.5 . . ?
Si6 C113 H11W 109.5 . . ?
H11U C113 H11V 109.5 . . ?
H11U C113 H11W 109.5 . . ?
H11V C113 H11W 109.5 . . ?
Si5 C110 H11X 109.5 . . ?
Si5 C110 H11Y 109.5 . . ?
Si5 C110 H 109.5 . . ?
H11X C110 H11Y 109.5 . . ?
H11X C110 H 109.5 . . ?
H11Y C110 H 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C135 C137 H13G 109.5 . . ?
C135 C137 H13H 109.5 . . ?
C135 C137 H13I 109.5 . . ?
H13G C137 H13H 109.5 . . ?
H13G C137 H13I 109.5 . . ?
H13H C137 H13I 109.5 . . ?
Si7 C151 H15X 109.5 . . ?
Si7 C151 H15Y 109.5 . . ?
Si7 C151 HA 109.5 . . ?
H15X C151 H15Y 109.5 . . ?
H15X C151 HA 109.5 . . ?
H15Y C151 HA 109.5 . . ?
C144 C145 H14G 109.5 . . ?
C144 C145 H14H 109.5 . . ?
C144 C145 H14I 109.5 . . ?
H14G C145 H14H 109.5 . . ?
H14G C145 H14I 109.5 . . ?
H14H C145 H14I 109.5 . . ?
C147 C149 H14J 109.5 . . ?
C147 C149 H14K 109.5 . . ?
C147 C149 H14L 109.5 . . ?
H14J C149 H14K 109.5 . . ?
H14J C149 H14L 109.5 . . ?
H14K C149 H14L 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N12 C120 H12A 109.5 . . ?
N12 C120 H12B 109.5 . . ?
N12 C120 H12C 109.5 . . ?
H12A C120 H12B 109.5 . . ?
H12A C120 H12C 109.5 . . ?
H12B C120 H12C 109.5 . . ?
Si3 C70 H70A 109.5 . . ?
Si3 C70 H70B 109.5 . . ?
Si3 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C95 C97 H97A 109.5 . . ?
C95 C97 H97B 109.5 . . ?
C95 C97 H97C 109.5 . . ?
H97A C97 H97B 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C147 C148 H14M 109.5 . . ?
C147 C148 H14N 109.5 . . ?
C147 C148 H14O 109.5 . . ?
H14M C148 H14N 109.5 . . ?
H14M C148 H14O 109.5 . . ?
H14N C148 H14O 109.5 . . ?
C104 C106 H10D 109.5 . . ?
C104 C106 H10E 109.5 . . ?
C104 C106 H10F 109.5 . . ?
H10D C106 H10E 109.5 . . ?
H10D C106 H10F 109.5 . . ?
H10E C106 H10F 109.5 . . ?
C107 C108 H10G 109.5 . . ?
C107 C108 H10H 109.5 . . ?
C107 C108 H10I 109.5 . . ?
H10G C108 H10H 109.5 . . ?
H10G C108 H10I 109.5 . . ?
H10H C108 H10I 109.5 . . ?
C104 C105 H10J 109.5 . . ?
C104 C105 H10K 109.5 . . ?
C104 C105 H10L 109.5 . . ?
H10J C105 H10K 109.5 . . ?
H10J C105 H10L 109.5 . . ?
H10K C105 H10L 109.5 . . ?
N4 C40 H40A 109.5 . . ?
N4 C40 H40B 109.5 . . ?
N4 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C132 C134 H13J 109.5 . . ?
C132 C134 H13K 109.5 . . ?
C132 C134 H13L 109.5 . . ?
H13J C134 H13K 109.5 . . ?
H13J C134 H13L 109.5 . . ?
H13K C134 H13L 109.5 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C132 C133 H13M 109.5 . . ?
C132 C133 H13N 109.5 . . ?
C132 C133 H13O 109.5 . . ?
H13M C133 H13N 109.5 . . ?
H13M C133 H13O 109.5 . . ?
H13N C133 H13O 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C38 C39 -128.45(13) . . . . ?
Ca1 O1 C36 C37 128.68(12) . . . . ?
Ca1 N1 C6 C11 135.67(12) . . . . ?
Ca1 N1 C6 C7 -42.73(19) . . . . ?
Ca1 N1 C1 C2 -35.21(17) . . . . ?
Ca1 N1 C1 C4 142.71(12) . . . . ?
Ca1 N2 C18 C19 -114.50(14) . . . . ?
Ca1 N2 C18 C23 60.67(17) . . . . ?
Ca1 N2 C3 C2 31.55(17) . . . . ?
Ca1 N2 C3 C5 -146.31(13) . . . . ?
Ca2 O2 C78 C79 123.03(13) . . . . ?
Ca2 O2 C76 C77 -123.42(11) . . . . ?
Ca2 N5 C43 C42 -39.56(15) . . . . ?
Ca2 N5 C43 C45 138.33(12) . . . . ?
Ca2 N5 C58 C63 -47.73(19) . . . . ?
Ca2 N5 C58 C59 128.91(13) . . . . ?
Ca2 N6 C41 C42 27.07(17) . . . . ?
Ca2 N6 C41 C44 -151.30(12) . . . . ?
Ca2 N6 C46 C51 -129.85(13) . . . . ?
Ca2 N6 C46 C47 46.1(2) . . . . ?
Ca3 O3 C118 C119 123.36(12) . . . . ?
Ca3 O3 C116 C117 -125.65(13) . . . . ?
Ca3 N9 C81 C82 -38.69(16) . . . . ?
Ca3 N9 C81 C84 140.29(11) . . . . ?
Ca3 N9 C86 C87 138.42(12) . . . . ?
Ca3 N9 C86 C91 -38.9(2) . . . . ?
Ca3 N10 C83 C82 26.19(16) . . . . ?
Ca3 N10 C83 C85 -151.96(12) . . . . ?
Ca3 N10 C98 C103 -115.16(13) . . . . ?
Ca3 N10 C98 C99 60.88(18) . . . . ?
Ca4 O4 C156 C157 123.34(12) . . . . ?
Ca4 O4 C158 C159 -124.03(12) . . . . ?
Ca4 N14 C123 C122 27.20(17) . . . . ?
Ca4 N14 C123 C125 -150.09(12) . . . . ?
Ca4 N14 C138 C143 -122.58(14) . . . . ?
Ca4 N14 C138 C139 54.06(19) . . . . ?
Ca4 N13 C121 C122 -39.64(16) . . . . ?
Ca4 N13 C121 C124 138.56(13) . . . . ?
Ca4 N13 C126 C131 -44.29(19) . . . . ?
Ca4 N13 C126 C127 131.76(13) . . . . ?
O4 C156 C157 N16 60.25(18) . . . . ?
O1 C38 C39 N4 -59.61(19) . . . . ?
O1 C36 C37 N4 58.37(19) . . . . ?
O2 C78 C79 N8 59.96(18) . . . . ?
O2 C76 C77 N8 -59.09(18) . . . . ?
O3 C118 C119 N12 61.14(16) . . . . ?
N9 C81 C82 C83 -16.9(2) . . . . ?
N9 C86 C91 C90 177.76(14) . . . . ?
N9 C86 C91 C95 -4.5(2) . . . . ?
N14 C123 C122 C121 24.9(3) . . . . ?
N14 C138 C143 C142 -179.24(13) . . . . ?
N14 C138 C143 C147 2.5(2) . . . . ?
N14 C138 C139 C140 -179.94(13) . . . . ?
N14 C138 C139 C144 2.0(2) . . . . ?
N1 C6 C11 C10 178.41(12) . . . . ?
N1 C6 C11 C15 -3.5(2) . . . . ?
N1 C6 C7 C8 -179.90(12) . . . . ?
N1 C6 C7 C12 -2.7(2) . . . . ?
N1 C1 C2 C3 -16.8(3) . . . . ?
N5 C43 C42 C41 -16.9(2) . . . . ?
N5 C58 C63 C64 0.5(2) . . . . ?
N5 C58 C63 C62 178.79(13) . . . . ?
N5 C58 C59 C60 179.72(14) . . . . ?
N5 C58 C59 C67 -2.2(2) . . . . ?
N2 C18 C19 C24 -3.4(2) . . . . ?
N2 C18 C19 C20 176.04(13) . . . . ?
N2 C18 C23 C22 -175.23(13) . . . . ?
N2 C18 C23 C27 2.9(2) . . . . ?
N2 C3 C2 C1 19.4(3) . . . . ?
N10 C83 C82 C81 25.8(2) . . . . ?
N10 C98 C99 C100 -178.90(14) . . . . ?
N10 C98 C99 C104 1.2(2) . . . . ?
N6 C41 C42 C43 25.8(3) . . . . ?
N6 C46 C47 C48 -177.22(14) . . . . ?
N6 C46 C47 C52 6.1(2) . . . . ?
N13 C126 C131 C135 -1.7(2) . . . . ?
N13 C126 C131 C130 177.60(13) . . . . ?
N13 C126 C127 C128 -178.59(14) . . . . ?
N13 C126 C127 C132 -0.2(2) . . . . ?
N12 C117 C116 O3 -57.00(17) . . . . ?
N16 C159 C158 O4 -59.23(18) . . . . ?
C6 N1 C1 C2 163.54(14) . . . . ?
C6 N1 C1 C4 -18.5(2) . . . . ?
C6 C11 C10 C9 2.2(2) . . . . ?
C6 C11 C15 C16 -114.36(15) . . . . ?
C6 C11 C15 C17 123.20(15) . . . . ?
C6 C7 C8 C9 0.9(2) . . . . ?
C6 C7 C12 C13 122.18(16) . . . . ?
C6 C7 C12 C14 -113.31(16) . . . . ?
C123 N14 C138 C143 73.35(18) . . . . ?
C123 N14 C138 C139 -110.00(16) . . . . ?
C123 C122 C121 N13 -15.4(3) . . . . ?
C123 C122 C121 C124 166.29(16) . . . . ?
C81 N9 C86 C87 -70.88(19) . . . . ?
C81 N9 C86 C91 111.79(16) . . . . ?
C43 N5 C58 C63 99.34(16) . . . . ?
C43 N5 C58 C59 -84.02(17) . . . . ?
C18 N2 C3 C2 -170.23(14) . . . . ?
C18 N2 C3 C5 11.9(2) . . . . ?
C18 C19 C24 C25 139.77(17) . . . . ?
C18 C19 C24 C26 -94.9(2) . . . . ?
C18 C19 C20 C21 -0.7(2) . . . . ?
C18 C23 C22 C21 -0.8(2) . . . . ?
C18 C23 C27 C28 -110.58(17) . . . . ?
C18 C23 C27 C29 125.18(17) . . . . ?
C87 C86 C91 C90 0.4(2) . . . . ?
C87 C86 C91 C95 178.14(15) . . . . ?
C87 C88 C89 C90 -0.7(2) . . . . ?
C138 N14 C123 C122 -164.59(14) . . . . ?
C138 N14 C123 C125 18.1(2) . . . . ?
C138 C143 C142 C141 -1.6(2) . . . . ?
C138 C143 C147 C149 121.91(16) . . . . ?
C138 C143 C147 C148 -114.63(17) . . . . ?
C138 C139 C140 C141 0.1(2) . . . . ?
C138 C139 C144 C146 -146.06(15) . . . . ?
C138 C139 C144 C145 89.47(18) . . . . ?
C1 N1 C6 C11 -69.97(18) . . . . ?
C1 N1 C6 C7 111.64(15) . . . . ?
C90 C91 C95 C96 57.3(2) . . . . ?
C90 C91 C95 C97 -67.2(2) . . . . ?
C3 N2 C18 C19 92.84(17) . . . . ?
C3 N2 C18 C23 -91.99(18) . . . . ?
C41 N6 C46 C51 70.6(2) . . . . ?
C41 N6 C46 C47 -113.42(16) . . . . ?
C143 C138 C139 C140 -3.4(2) . . . . ?
C143 C138 C139 C144 178.56(13) . . . . ?
C58 N5 C43 C42 163.71(13) . . . . ?
C58 N5 C43 C45 -18.40(19) . . . . ?
C58 C63 C64 C65 -127.90(16) . . . . ?
C58 C63 C64 C66 108.69(17) . . . . ?
C58 C63 C62 C61 0.9(2) . . . . ?
C58 C59 C60 C61 2.0(2) . . . . ?
C58 C59 C67 C69 91.4(2) . . . . ?
C58 C59 C67 C68 -144.6(2) . . . . ?
C83 N10 C98 C103 87.97(17) . . . . ?
C83 N10 C98 C99 -95.98(17) . . . . ?
C11 C6 C7 C8 1.7(2) . . . . ?
C11 C6 C7 C12 178.92(13) . . . . ?
C63 C58 C59 C60 -3.6(2) . . . . ?
C63 C58 C59 C67 174.48(15) . . . . ?
C63 C62 C61 C60 -2.4(2) . . . . ?
C121 N13 C126 C131 100.20(17) . . . . ?
C121 N13 C126 C127 -83.75(17) . . . . ?
C86 N9 C81 C82 162.04(14) . . . . ?
C86 N9 C81 C84 -19.0(2) . . . . ?
C86 C87 C88 C89 2.7(2) . . . . ?
C86 C87 C92 C93 -112.65(16) . . . . ?
C86 C87 C92 C94 124.59(15) . . . . ?
C86 C91 C95 C96 -120.42(16) . . . . ?
C86 C91 C95 C97 115.08(17) . . . . ?
C103 C98 C99 C100 -2.9(2) . . . . ?
C103 C98 C99 C104 177.27(15) . . . . ?
C103 C102 C101 C100 -0.3(3) . . . . ?
C7 C6 C11 C10 -3.2(2) . . . . ?
C7 C6 C11 C15 174.92(13) . . . . ?
C126 N13 C121 C122 165.90(14) . . . . ?
C126 N13 C121 C124 -15.9(2) . . . . ?
C126 C131 C135 C136 -126.76(16) . . . . ?
C126 C131 C135 C137 109.44(17) . . . . ?
C126 C131 C130 C129 0.6(2) . . . . ?
C126 C127 C128 C129 1.4(3) . . . . ?
C126 C127 C132 C134 -141.6(2) . . . . ?
C126 C127 C132 C133 93.4(3) . . . . ?
C139 C138 C143 C142 4.1(2) . . . . ?
C139 C138 C143 C147 -174.13(15) . . . . ?
C139 C140 C141 C142 2.4(2) . . . . ?
C51 C46 C47 C48 -1.3(2) . . . . ?
C51 C46 C47 C52 -177.93(15) . . . . ?
C8 C9 C10 C11 0.3(2) . . . . ?
C8 C7 C12 C13 -60.60(18) . . . . ?
C8 C7 C12 C14 63.91(18) . . . . ?
C88 C87 C86 N9 -179.88(14) . . . . ?
C88 C87 C86 C91 -2.5(2) . . . . ?
C88 C87 C92 C93 64.35(19) . . . . ?
C88 C87 C92 C94 -58.41(19) . . . . ?
C19 C18 C23 C22 -0.1(2) . . . . ?
C19 C18 C23 C27 178.00(14) . . . . ?
C19 C20 C21 C22 -0.1(3) . . . . ?
C98 N10 C83 C82 -171.90(13) . . . . ?
C98 N10 C83 C85 10.0(2) . . . . ?
C98 C103 C107 C109 133.15(16) . . . . ?
C98 C103 C107 C108 -102.87(19) . . . . ?
C98 C103 C102 C101 -1.8(2) . . . . ?
C98 C99 C100 C101 0.7(2) . . . . ?
C98 C99 C104 C106 -130.39(17) . . . . ?
C98 C99 C104 C105 105.22(19) . . . . ?
C46 N6 C41 C42 -167.96(14) . . . . ?
C46 N6 C41 C44 13.7(2) . . . . ?
C46 C51 C55 C57 112.83(17) . . . . ?
C46 C51 C55 C56 -124.92(18) . . . . ?
C46 C51 C50 C49 -0.8(3) . . . . ?
C46 C47 C48 C49 0.1(2) . . . . ?
C46 C47 C52 C53 -152.48(16) . . . . ?
C46 C47 C52 C54 82.51(19) . . . . ?
C91 C90 C89 C88 -1.5(2) . . . . ?
C4 C1 C2 C3 165.19(16) . . . . ?
C140 C139 C144 C146 35.9(2) . . . . ?
C140 C139 C144 C145 -88.59(18) . . . . ?
C140 C141 C142 C143 -1.6(2) . . . . ?
C89 C90 C91 C86 1.6(2) . . . . ?
C89 C90 C91 C95 -176.17(15) . . . . ?
C10 C11 C15 C16 63.73(18) . . . . ?
C10 C11 C15 C17 -58.70(18) . . . . ?
C10 C9 C8 C7 -1.9(2) . . . . ?
C84 C81 C82 C83 164.10(15) . . . . ?
C64 C63 C62 C61 179.20(14) . . . . ?
C131 C126 C127 C128 -2.5(2) . . . . ?
C131 C126 C127 C132 175.83(15) . . . . ?
C131 C130 C129 C128 -1.7(3) . . . . ?
C23 C18 C19 C24 -178.56(14) . . . . ?
C23 C18 C19 C20 0.9(2) . . . . ?
C23 C22 C21 C20 0.9(3) . . . . ?
C45 C43 C42 C41 165.17(15) . . . . ?
C99 C100 C101 C102 0.8(3) . . . . ?
C62 C63 C64 C65 53.8(2) . . . . ?
C62 C63 C64 C66 -69.61(18) . . . . ?
C15 C11 C10 C9 -176.00(14) . . . . ?
C92 C87 C86 N9 -2.9(2) . . . . ?
C92 C87 C86 C91 174.50(14) . . . . ?
C92 C87 C88 C89 -174.43(15) . . . . ?
C78 O2 C76 C77 58.99(16) . . . . ?
C156 O4 C158 C159 58.84(17) . . . . ?
C47 C48 C49 C50 0.7(3) . . . . ?
C24 C19 C20 C21 178.70(15) . . . . ?
C20 C19 C24 C25 -39.7(2) . . . . ?
C20 C19 C24 C26 85.7(2) . . . . ?
C127 C126 C131 C135 -177.73(14) . . . . ?
C127 C126 C131 C130 1.6(2) . . . . ?
C48 C47 C52 C53 30.9(2) . . . . ?
C48 C47 C52 C54 -94.09(18) . . . . ?
C48 C49 C50 C51 -0.3(3) . . . . ?
C59 C58 C63 C64 -176.11(14) . . . . ?
C59 C58 C63 C62 2.2(2) . . . . ?
C59 C60 C61 C62 1.0(3) . . . . ?
C44 C41 C42 C43 -155.75(15) . . . . ?
C125 C123 C122 C121 -157.67(16) . . . . ?
C12 C7 C8 C9 -176.47(14) . . . . ?
C22 C23 C27 C28 67.55(19) . . . . ?
C22 C23 C27 C29 -56.7(2) . . . . ?
C76 O2 C78 C79 -59.49(17) . . . . ?
C60 C59 C67 C69 -90.6(2) . . . . ?
C60 C59 C67 C68 33.4(3) . . . . ?
C79 N8 C77 C76 57.90(18) . . . . ?
C107 C103 C98 N10 -0.2(2) . . . . ?
C107 C103 C98 C99 -176.25(14) . . . . ?
C107 C103 C102 C101 177.84(15) . . . . ?
C144 C139 C140 C141 178.22(14) . . . . ?
C154 Si8 N15 Ca4 146.24(8) . . . . ?
C154 Si8 N15 Si7 -37.83(12) . . . . ?
C38 O1 C36 C37 -56.36(17) . . . . ?
C100 C99 C104 C106 49.8(2) . . . . ?
C100 C99 C104 C105 -74.6(2) . . . . ?
C75 Si4 N7 Ca2 23.72(11) . . . . ?
C75 Si4 N7 Si3 -158.18(9) . . . . ?
C157 N16 C159 C158 58.19(18) . . . . ?
C142 C143 C147 C149 -56.3(2) . . . . ?
C142 C143 C147 C148 67.2(2) . . . . ?
C155 Si8 N15 Ca4 25.87(11) . . . . ?
C155 Si8 N15 Si7 -158.19(9) . . . . ?
C150 Si7 N15 Ca4 5.22(9) . . . . ?
C150 Si7 N15 Si8 -171.38(9) . . . . ?
C135 C131 C130 C129 179.88(15) . . . . ?
C55 C51 C46 N6 -0.3(2) . . . . ?
C55 C51 C46 C47 -176.22(15) . . . . ?
C55 C51 C50 C49 177.15(17) . . . . ?
C27 C23 C22 C21 -178.96(16) . . . . ?
C72 Si3 N7 Ca2 9.97(9) . . . . ?
C72 Si3 N7 Si4 -168.41(9) . . . . ?
C130 C131 C135 C136 53.9(2) . . . . ?
C130 C131 C135 C137 -69.9(2) . . . . ?
C130 C129 C128 C127 0.7(3) . . . . ?
C34 Si2 N3 Ca1 121.29(9) . . . . ?
C34 Si2 N3 Si1 -54.45(11) . . . . ?
C159 N16 C157 C156 -58.49(18) . . . . ?
C33 Si2 N3 Ca1 -116.73(8) . . . . ?
C33 Si2 N3 Si1 67.52(11) . . . . ?
C102 C103 C98 N10 179.46(13) . . . . ?
C102 C103 C98 C99 3.4(2) . . . . ?
C102 C103 C107 C109 -46.5(2) . . . . ?
C102 C103 C107 C108 77.5(2) . . . . ?
C118 O3 C116 C117 56.48(17) . . . . ?
C119 N12 C117 C116 58.40(17) . . . . ?
C114 Si6 N11 Ca3 -103.04(10) . . . . ?
C114 Si6 N11 Si5 77.06(11) . . . . ?
C52 C47 C48 C49 176.84(16) . . . . ?
C5 C3 C2 C1 -162.65(16) . . . . ?
C77 N8 C79 C78 -58.18(17) . . . . ?
C35 Si2 N3 Ca1 0.36(11) . . . . ?
C35 Si2 N3 Si1 -175.39(9) . . . . ?
C36 O1 C38 C39 57.09(19) . . . . ?
C85 C83 C82 C81 -155.89(15) . . . . ?
C158 O4 C156 C157 -59.68(18) . . . . ?
C112 Si5 N11 Ca3 17.91(9) . . . . ?
C112 Si5 N11 Si6 -162.18(9) . . . . ?
C147 C143 C142 C141 176.69(16) . . . . ?
C39 N4 C37 C36 -59.32(19) . . . . ?
C37 N4 C39 C38 59.68(18) . . . . ?
C50 C51 C46 N6 177.53(15) . . . . ?
C50 C51 C46 C47 1.6(2) . . . . ?
C50 C51 C55 C57 -65.0(2) . . . . ?
C50 C51 C55 C56 57.2(2) . . . . ?
C73 Si4 N7 Ca2 143.59(9) . . . . ?
C73 Si4 N7 Si3 -38.31(13) . . . . ?
C71 Si3 N7 Ca2 -108.17(8) . . . . ?
C71 Si3 N7 Si4 73.44(11) . . . . ?
C128 C127 C132 C134 36.8(3) . . . . ?
C128 C127 C132 C133 -88.2(3) . . . . ?
C74 Si4 N7 Ca2 -96.16(10) . . . . ?
C74 Si4 N7 Si3 81.93(11) . . . . ?
C32 Si1 N3 Ca1 27.93(9) . . . . ?
C32 Si1 N3 Si2 -155.85(9) . . . . ?
C117 N12 C119 C118 -59.98(17) . . . . ?
C31 Si1 N3 Ca1 146.08(7) . . . . ?
C31 Si1 N3 Si2 -37.71(12) . . . . ?
C116 O3 C118 C119 -58.85(16) . . . . ?
C115 Si6 N11 Ca3 16.80(11) . . . . ?
C115 Si6 N11 Si5 -163.10(9) . . . . ?
C80 N8 C79 C78 179.84(13) . . . . ?
C80 N8 C77 C76 -179.89(15) . . . . ?
C132 C127 C128 C129 -176.96(17) . . . . ?
C111 Si5 N11 Ca3 -100.77(9) . . . . ?
C111 Si5 N11 Si6 79.15(11) . . . . ?
C67 C59 C60 C61 -176.06(16) . . . . ?
C104 C99 C100 C101 -179.40(16) . . . . ?
C160 N16 C157 C156 179.73(15) . . . . ?
C160 N16 C159 C158 179.81(15) . . . . ?
C152 Si7 N15 Ca4 -112.28(8) . . . . ?
C152 Si7 N15 Si8 71.12(11) . . . . ?
C153 Si8 N15 Ca4 -93.45(10) . . . . ?
C153 Si8 N15 Si7 82.48(11) . . . . ?
C30 Si1 N3 Ca1 -91.20(9) . . . . ?
C30 Si1 N3 Si2 85.02(11) . . . . ?
C113 Si6 N11 Ca3 137.05(9) . . . . ?
C113 Si6 N11 Si5 -42.85(12) . . . . ?
C110 Si5 N11 Ca3 135.57(8) . . . . ?
C110 Si5 N11 Si6 -44.51(12) . . . . ?
C151 Si7 N15 Ca4 124.03(8) . . . . ?
C151 Si7 N15 Si8 -52.57(12) . . . . ?
C120 N12 C119 C118 176.19(14) . . . . ?
C120 N12 C117 C116 -177.81(14) . . . . ?
C70 Si3 N7 Ca2 128.35(8) . . . . ?
C70 Si3 N7 Si4 -50.04(12) . . . . ?
C40 N4 C39 C38 -177.94(15) . . . . ?
C40 N4 C37 C36 178.52(17) . . . . ?

_shelx_SHELXL_version_number     2014/7

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5 -7 -9 0.1363 4.9907 -7.0001 -9.0021 -0.1594 -0.9608 -0.1463
2 2 -24 0.1355 2.0044 1.9843 -24.0097 -0.1381 -0.6570 0.7180
-4 9 -16 0.0877 -3.9850 8.9836 -16.0078 0.1386 0.3500 0.9301
-5 9 -1 0.0776 -4.9870 8.9927 -1.0022 0.1394 0.8085 0.5149
1 -10 20 0.1721 0.9866 -9.9813 20.0102 0.2085 -0.0837 -0.9769
-1 -12 16 0.1473 -1.0120 -11.9831 16.0097 0.5503 -0.1483 -0.8530
-3 -12 8 0.1221 -3.0082 -11.9886 8.0072 0.8283 -0.2106 -0.5408
-5 -9 -4 0.1003 -5.0011 -8.9984 -3.9976 0.9963 -0.2178 -0.0064
-5 -2 -17 0.1101 -4.9927 -2.0107 -17.0045 0.7661 -0.1838 0.6223
-3 5 -22 0.1125 -2.9881 4.9825 -22.0089 0.2579 -0.0875 0.9388
-7 -2 -9 0.0728 -6.9922 -2.0062 -9.0012 0.9278 0.1663 0.4533
-7 -4 -3 0.0729 -6.9950 -4.0012 -2.9984 0.9769 0.2155 0.2050
-6 -7 5 0.0974 -6.0002 -6.9942 5.0052 0.9480 0.1916 -0.1733
-4 -10 14 0.1229 -4.0067 -9.9863 14.0090 0.8018 0.1215 -0.6175
-1 -10 20 0.1564 -1.0112 -9.9818 20.0105 0.4284 0.0602 -0.9053
6 -2 16 0.1610 5.9885 -1.9873 16.0052 -0.6832 -0.1248 -0.7639
7 4 3 0.1001 6.9950 4.0012 2.9984 -0.9769 -0.2155 -0.2050
6 7 -4 0.0872 6.0000 6.9948 -4.0048 -0.9553 -0.1658 0.1432
5 9 -11 0.0897 5.0042 8.9890 -11.0078 -0.8872 -0.1688 0.4575
-7 2 -4 0.0621 -6.9899 1.9945 -4.0007 0.7058 0.5061 0.4389
-7 -2 6 0.0856 -6.9952 -1.9968 6.0042 0.8187 0.5529 0.0023
-4 -7 19 0.1272 -4.0053 -6.9850 19.0098 0.6263 0.4085 -0.6659
7 2 -8 0.0995 6.9957 1.9956 -8.0049 -0.8041 -0.6045 0.0578
6 5 -15 0.1022 6.0006 4.9892 -15.0082 -0.7824 -0.5547 0.4060
-6 3 12 0.1077 -5.9935 3.0042 12.0046 0.4331 0.8992 -0.0440
-2 -5 24 0.1480 -2.0069 -4.9825 24.0106 0.2772 0.4989 -0.8199
6 -7 1 0.1344 5.9875 -6.9937 1.0014 -0.3421 -0.7750 -0.4828
4 -9 18 0.1773 3.9846 -8.9824 18.0085 -0.1531 -0.2984 -0.9902
-4 9 11 0.1055 -3.9905 9.0004 11.0019 -0.0579 1.0458 0.1183
-4 11 -1 0.0791 -3.9864 10.9918 -1.0030 -0.0633 0.8420 0.5470
-3 10 -15 0.0866 -2.9854 9.9839 -15.0079 -0.0250 0.3565 0.8982
-1 -2 25 0.1562 -1.0057 -1.9835 25.0098 0.0208 0.6108 -0.7838
4 -11 7 0.1510 3.9852 -10.9880 7.0052 0.0197 -0.6873 -0.7274
4 -11 -1 0.1469 3.9868 -10.9930 -0.9977 0.0779 -0.8935 -0.4869
2 -2 -23 0.1494 2.0009 -2.0126 -23.0081 0.0403 -0.8421 0.5520
-2 0 -24 0.1351 -1.9929 -0.0155 -24.0083 0.3945 -0.4746 0.7933
1 2 23 0.1453 0.9958 2.0134 23.0075 -0.3700 0.6263 -0.6594
0 10 11 0.0985 0.0059 10.0009 11.0008 -0.5440 0.8107 0.0090
-1 13 0 0.0724 -0.9882 12.9919 -0.0039 -0.4932 0.7573 0.4775
-1 13 -10 0.0736 -0.9862 12.9857 -10.0075 -0.4205 0.4996 0.7782
2 13 -9 0.0732 2.0103 12.9871 -9.0077 -0.7575 0.3095 0.6407
3 11 3 0.0767 3.0051 10.9960 2.9970 -0.8620 0.4414 0.1761
4 9 10 0.0973 4.0010 9.0019 10.0000 -0.9300 0.4444 -0.1382
4 6 15 0.1155 3.9975 6.0068 15.0027 -0.8272 0.4151 -0.3904
6 4 12 0.1206 5.9943 4.0066 12.0019 -0.9325 0.0884 -0.4398
6 6 8 0.0971 5.9967 6.0029 7.9998 -0.9962 0.0907 -0.2516
5 9 0 0.0790 5.0019 8.9959 -0.0038 -0.9672 0.1147 0.1267
7 1 1 0.1015 6.9930 1.0018 0.9987 -0.8232 -0.4252 -0.2468
7 4 -8 0.0895 6.9973 3.9944 -8.0055 -0.8969 -0.4990 0.1258
7 -3 -5 0.1119 6.9909 -2.9995 -5.0023 -0.5940 -0.7907 -0.2023
6 0 -13 0.1182 5.9961 -0.0066 -13.0059 -0.5650 -0.7668 0.1760
4 4 -21 0.1203 4.0032 3.9855 -21.0096 -0.4725 -0.6182 0.6241
2 -12 10 0.1485 1.9859 -11.9861 10.0070 0.2641 -0.5188 -0.7800
2 -12 -1 0.1403 1.9882 -11.9929 -0.9970 0.3442 -0.8023 -0.4492
0 -2 -24 0.1455 0.0033 -2.0138 -24.0080 0.2674 -0.7240 0.6537
-1 -13 0 0.1278 -1.0096 -12.9925 0.0043 0.7131 -0.6134 -0.4059
-7 -1 -4 0.0603 -6.9924 -1.0037 -3.9997 0.8450 0.3479 0.3370
-6 -6 8 0.0987 -6.0000 -5.9929 8.0060 0.8798 0.3216 -0.2295
5 0 19 0.1562 4.9907 0.0131 19.0059 -0.6879 0.1299 -0.7503

_olex2_date_sample_data_collection 2016-11-28
_olex2_submission_original_sample_id hasj161128a
_olex2_submission_special_instructions 'No special instructions were received'
