# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex3
_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H29 Ca Cl N0 O2 Si0'
_chemical_formula_weight         352.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0963(6)
_cell_length_b                   13.5005(9)
_cell_length_c                   17.6543(13)
_cell_angle_alpha                80.412(6)
_cell_angle_beta                 76.114(6)
_cell_angle_gamma                70.938(6)
_cell_volume                     1980.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4297
_cell_measurement_theta_min      2.6000
_cell_measurement_theta_max      72.7300

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_T_max  0.7404
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       /w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13210
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         67.48
_reflns_number_total             7128
_reflns_number_gt                5716
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0474P)²+2.1931P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7128
_refine_ls_number_parameters     425
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1267
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl -0.15873(9) 0.95081(6) -0.00117(5) 0.03218(19) Uani 1 1 d . . .
Ca2 Ca 0.14224(8) 0.84742(5) 0.02338(4) 0.02565(16) Uani 1 1 d . . .
Cl1 Cl 0.34043(9) 0.45185(6) 0.50093(5) 0.03001(18) Uani 1 1 d . . .
Ca1 Ca 0.65991(8) 0.35760(5) 0.46240(4) 0.02599(16) Uani 1 1 d . . .
O1 O 0.6025(3) 0.20206(18) 0.53854(16) 0.0398(6) Uani 1 1 d . A .
O2 O 0.8472(3) 0.29478(19) 0.54824(13) 0.0341(5) Uani 1 1 d . . .
C1 C 0.6319(4) 0.3511(3) 0.31559(19) 0.0343(8) Uani 1 1 d . . .
C2 C 0.7243(4) 0.2481(3) 0.3379(2) 0.0338(8) Uani 1 1 d . . .
C3 C 0.8721(4) 0.2527(3) 0.3456(2) 0.0341(8) Uani 1 1 d . . .
C4 C 0.8716(4) 0.3592(3) 0.3287(2) 0.0355(8) Uani 1 1 d . . .
C5 C 0.7237(4) 0.4193(3) 0.31042(19) 0.0336(8) Uani 1 1 d . . .
C6 C 0.4684(5) 0.3795(4) 0.2986(2) 0.0485(10) Uani 1 1 d . . .
H6A H 0.4701 0.3377 0.2578 0.073 Uiso 1 1 calc R . .
H6B H 0.4335 0.4546 0.2804 0.073 Uiso 1 1 calc R . .
H6C H 0.3947 0.3648 0.3464 0.073 Uiso 1 1 calc R . .
C7 C 0.6750(6) 0.1493(3) 0.3469(3) 0.0516(11) Uani 1 1 d . . .
H7A H 0.7008 0.1219 0.2957 0.077 Uiso 1 1 calc R . .
H7B H 0.5605 0.1658 0.3673 0.077 Uiso 1 1 calc R . .
H7C H 0.7319 0.0961 0.3833 0.077 Uiso 1 1 calc R . .
C8 C 1.0128(5) 0.1603(3) 0.3610(3) 0.0514(11) Uani 1 1 d . . .
H8A H 0.9863 0.0947 0.3649 0.077 Uiso 1 1 calc R . .
H8B H 1.0399 0.1661 0.4103 0.077 Uiso 1 1 calc R . .
H8C H 1.1037 0.1603 0.3179 0.077 Uiso 1 1 calc R . .
C9 C 1.0086(5) 0.4007(4) 0.3259(2) 0.0540(11) Uani 1 1 d . . .
H9A H 1.0543 0.4190 0.2712 0.081 Uiso 1 1 calc R . .
H9B H 1.0899 0.3466 0.3502 0.081 Uiso 1 1 calc R . .
H9C H 0.9704 0.4636 0.3545 0.081 Uiso 1 1 calc R . .
C10 C 0.6754(6) 0.5365(3) 0.2875(2) 0.0522(11) Uani 1 1 d . . .
H10A H 0.6574 0.5738 0.3336 0.078 Uiso 1 1 calc R . .
H10B H 0.5775 0.5573 0.2670 0.078 Uiso 1 1 calc R . .
H10C H 0.7599 0.5545 0.2471 0.078 Uiso 1 1 calc R . .
C11 C 0.7183(5) 0.1012(3) 0.5530(3) 0.0439(9) Uani 1 1 d U . .
C12 C 0.6214(12) 0.0230(7) 0.5769(6) 0.0487(19) Uani 0.50 1 d PU A 1
H12A H 0.6716 -0.0396 0.6102 0.058 Uiso 0.50 1 calc PR A 1
H12B H 0.5992 0.0008 0.5311 0.058 Uiso 0.50 1 calc PR A 1
C13 C 0.4691(18) 0.1004(12) 0.6245(9) 0.062(3) Uani 0.50 1 d PU A 1
H13A H 0.3767 0.0733 0.6347 0.074 Uiso 0.50 1 calc PR A 1
H13B H 0.4885 0.1105 0.6752 0.074 Uiso 0.50 1 calc PR A 1
C12A C 0.6294(13) 0.0427(8) 0.6162(7) 0.062(2) Uani 0.50 1 d PU A 2
H12C H 0.6346 0.0570 0.6685 0.074 Uiso 0.50 1 calc PR A 2
H12D H 0.6729 -0.0340 0.6119 0.074 Uiso 0.50 1 calc PR A 2
C13A C 0.4500(18) 0.0861(12) 0.6023(10) 0.061(3) Uani 0.50 1 d PU A 2
H13C H 0.4338 0.0497 0.5622 0.074 Uiso 0.50 1 calc PR A 2
H13D H 0.3720 0.0807 0.6515 0.074 Uiso 0.50 1 calc PR A 2
C14 C 0.4439(6) 0.1959(4) 0.5746(4) 0.0800(17) Uani 1 1 d U . .
C15 C 1.0020(5) 0.3086(4) 0.5365(2) 0.0463(9) Uani 1 1 d . . .
H15A H 1.0052 0.3752 0.5037 0.056 Uiso 1 1 calc R . .
H15B H 1.0842 0.2495 0.5100 0.056 Uiso 1 1 calc R . .
C16 C 1.0303(4) 0.3112(3) 0.6169(2) 0.0395(8) Uani 1 1 d . . .
H16A H 1.1012 0.3541 0.6150 0.047 Uiso 1 1 calc R . .
H16B H 1.0759 0.2394 0.6413 0.047 Uiso 1 1 calc R . .
C17 C 0.8625(4) 0.3624(3) 0.6604(2) 0.0393(8) Uani 1 1 d . . .
H17A H 0.8531 0.3460 0.7179 0.047 Uiso 1 1 calc R . .
H17B H 0.8301 0.4398 0.6478 0.047 Uiso 1 1 calc R . .
C18 C 0.7662(5) 0.3129(3) 0.6298(2) 0.0402(8) Uani 1 1 d . . .
H18A H 0.7618 0.2455 0.6611 0.048 Uiso 1 1 calc R . .
H18B H 0.6565 0.3604 0.6318 0.048 Uiso 1 1 calc R . .
O3 O 0.3971(3) 0.82174(19) -0.06509(14) 0.0347(5) Uani 1 1 d . . .
O4 O 0.1455(3) 0.73354(18) -0.06951(14) 0.0340(5) Uani 1 1 d . . .
C19 C 0.1285(5) 0.6879(3) 0.1343(2) 0.0359(8) Uani 1 1 d . . .
C20 C 0.2819(4) 0.6963(3) 0.1268(2) 0.0349(8) Uani 1 1 d . . .
C21 C 0.2647(4) 0.7930(3) 0.1543(2) 0.0353(8) Uani 1 1 d . . .
C22 C 0.1016(4) 0.8429(3) 0.17912(19) 0.0335(8) Uani 1 1 d . . .
C23 C 0.0169(4) 0.7784(3) 0.1667(2) 0.0340(8) Uani 1 1 d . . .
C24 C 0.0868(7) 0.5946(4) 0.1203(3) 0.0642(14) Uani 1 1 d . . .
H24A H 0.1841 0.5401 0.1003 0.096 Uiso 1 1 calc R . .
H24B H 0.0178 0.6162 0.0818 0.096 Uiso 1 1 calc R . .
H24C H 0.0313 0.5666 0.1697 0.096 Uiso 1 1 calc R . .
C25 C 0.4366(5) 0.6141(4) 0.1005(3) 0.0599(13) Uani 1 1 d . . .
H25A H 0.4167 0.5472 0.0998 0.090 Uiso 1 1 calc R . .
H25B H 0.5074 0.6050 0.1368 0.090 Uiso 1 1 calc R . .
H25C H 0.4864 0.6367 0.0477 0.090 Uiso 1 1 calc R . .
C26 C 0.3972(6) 0.8323(5) 0.1622(3) 0.0691(15) Uani 1 1 d . . .
H26A H 0.4099 0.8881 0.1201 0.104 Uiso 1 1 calc R . .
H26B H 0.4962 0.7741 0.1584 0.104 Uiso 1 1 calc R . .
H26C H 0.3715 0.8604 0.2131 0.104 Uiso 1 1 calc R . .
C27 C 0.0326(7) 0.9444(3) 0.2174(2) 0.0600(13) Uani 1 1 d . . .
H27A H 0.0564 0.9326 0.2700 0.090 Uiso 1 1 calc R . .
H27B H -0.0827 0.9689 0.2213 0.090 Uiso 1 1 calc R . .
H27C H 0.0791 0.9977 0.1859 0.090 Uiso 1 1 calc R . .
C28 C -0.1601(5) 0.7973(4) 0.1894(3) 0.0591(12) Uani 1 1 d . . .
H28A H -0.1992 0.7869 0.1451 0.089 Uiso 1 1 calc R . .
H28B H -0.2122 0.8696 0.2035 0.089 Uiso 1 1 calc R . .
H28C H -0.1840 0.7478 0.2343 0.089 Uiso 1 1 calc R . .
C29 C 0.5359(5) 0.8421(4) -0.0533(3) 0.0505(10) Uani 1 1 d . . .
H29A H 0.5983 0.7817 -0.0225 0.061 Uiso 1 1 calc R . .
H29B H 0.5057 0.9060 -0.0256 0.061 Uiso 1 1 calc R . .
C30 C 0.6301(5) 0.8580(4) -0.1361(3) 0.0623(13) Uani 1 1 d . . .
H30A H 0.6992 0.9021 -0.1378 0.075 Uiso 1 1 calc R . .
H30B H 0.6960 0.7898 -0.1562 0.075 Uiso 1 1 calc R . .
C31 C 0.5032(6) 0.9123(4) -0.1809(3) 0.0589(12) Uani 1 1 d . . .
H31A H 0.5416 0.9022 -0.2373 0.071 Uiso 1 1 calc R . .
H31B H 0.4637 0.9887 -0.1748 0.071 Uiso 1 1 calc R . .
C32 C 0.3753(5) 0.8601(3) -0.1449(2) 0.0439(9) Uani 1 1 d . . .
H32A H 0.2687 0.9113 -0.1449 0.053 Uiso 1 1 calc R . .
H32B H 0.3867 0.8010 -0.1746 0.053 Uiso 1 1 calc R . .
C33 C 0.2546(4) 0.6295(3) -0.0787(2) 0.0384(8) Uani 1 1 d . . .
H33A H 0.3011 0.6010 -0.0314 0.046 Uiso 1 1 calc R . .
H33B H 0.3416 0.6306 -0.1246 0.046 Uiso 1 1 calc R . .
C34 C 0.1566(5) 0.5629(3) -0.0907(2) 0.0432(9) Uani 1 1 d . . .
H34A H 0.2137 0.5182 -0.1341 0.052 Uiso 1 1 calc R . .
H34B H 0.1323 0.5173 -0.0424 0.052 Uiso 1 1 calc R . .
C35 C 0.0058(5) 0.6428(3) -0.1105(3) 0.0478(10) Uani 1 1 d . . .
H35A H -0.0175 0.6274 -0.1585 0.057 Uiso 1 1 calc R . .
H35B H -0.0859 0.6433 -0.0668 0.057 Uiso 1 1 calc R . .
C36 C 0.0420(5) 0.7467(3) -0.1233(2) 0.0427(9) Uani 1 1 d . . .
H36A H 0.0958 0.7600 -0.1781 0.051 Uiso 1 1 calc R . .
H36B H -0.0562 0.8058 -0.1109 0.051 Uiso 1 1 calc R . .


_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
Cl2 Ca2 2.7348(10) 2_575 ?
Cl2 Ca2 2.7391(10) . ?
Ca2 O4 2.417(2) . ?
Ca2 O3 2.419(2) . ?
Ca2 C23 2.663(3) . ?
Ca2 C19 2.672(3) . ?
Ca2 C22 2.678(3) . ?
Ca2 C21 2.694(3) . ?
Ca2 C20 2.699(3) . ?
Ca2 Cl2 2.7348(10) 2_575 ?
Ca2 C32 3.224(4) . ?
Ca2 Ca2 4.1569(12) 2_575 ?
Cl1 Ca1 2.7297(10) . ?
Cl1 Ca1 2.7541(10) 2_666 ?
Ca1 O2 2.405(2) . ?
Ca1 O1 2.435(2) . ?
Ca1 C5 2.656(3) . ?
Ca1 C4 2.667(3) . ?
Ca1 C1 2.683(3) . ?
Ca1 C3 2.694(3) . ?
Ca1 C2 2.694(3) . ?
Ca1 Cl1 2.7541(10) 2_666 ?
Ca1 C18 3.229(4) . ?
Ca1 Ca1 4.1892(12) 2_666 ?
O1 C11 1.451(4) . ?
O1 C14 1.454(5) . ?
O2 C15 1.442(4) . ?
O2 C18 1.471(4) . ?
C1 C5 1.412(5) . ?
C1 C2 1.417(5) . ?
C1 C6 1.501(5) . ?
C2 C3 1.405(5) . ?
C2 C7 1.514(5) . ?
C3 C4 1.418(5) . ?
C3 C8 1.510(5) . ?
C4 C5 1.407(5) . ?
C4 C9 1.513(5) . ?
C5 C10 1.509(5) . ?
C11 C12A 1.487(11) . ?
C11 C12 1.533(10) . ?
C12 C13 1.584(19) . ?
C13 C14 1.420(17) . ?
C12A C13A 1.61(2) . ?
C13A C14 1.468(16) . ?
C15 C16 1.511(5) . ?
C16 C17 1.524(5) . ?
C17 C18 1.496(5) . ?
O3 C29 1.444(5) . ?
O3 C32 1.455(4) . ?
O4 C33 1.440(4) . ?
O4 C36 1.443(4) . ?
C19 C20 1.409(5) . ?
C19 C23 1.412(5) . ?
C19 C24 1.501(5) . ?
C20 C21 1.416(5) . ?
C20 C25 1.505(5) . ?
C21 C22 1.407(5) . ?
C21 C26 1.509(5) . ?
C22 C23 1.409(5) . ?
C22 C27 1.507(5) . ?
C23 C28 1.508(5) . ?
C29 C30 1.527(6) . ?
C30 C31 1.479(6) . ?
C31 C32 1.512(5) . ?
C33 C34 1.524(5) . ?
C34 C35 1.518(6) . ?
C35 C36 1.512(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ca2 Cl2 Ca2 98.82(3) 2_575 . ?
O4 Ca2 O3 74.44(8) . . ?
O4 Ca2 C23 109.17(10) . . ?
O3 Ca2 C23 139.75(10) . . ?
O4 Ca2 C19 87.45(9) . . ?
O3 Ca2 C19 114.05(11) . . ?
C23 Ca2 C19 30.69(11) . . ?
O4 Ca2 C22 137.41(10) . . ?
O3 Ca2 C22 123.86(10) . . ?
C23 Ca2 C22 30.59(11) . . ?
C19 Ca2 C22 50.40(10) . . ?
O4 Ca2 C21 127.99(10) . . ?
O3 Ca2 C21 94.66(10) . . ?
C23 Ca2 C21 50.42(11) . . ?
C19 Ca2 C21 50.28(11) . . ?
C22 Ca2 C21 30.37(11) . . ?
O4 Ca2 C20 97.70(10) . . ?
O3 Ca2 C20 89.32(10) . . ?
C23 Ca2 C20 50.51(11) . . ?
C19 Ca2 C20 30.41(11) . . ?
C22 Ca2 C20 50.30(10) . . ?
C21 Ca2 C20 30.45(11) . . ?
O4 Ca2 Cl2 130.53(7) . 2_575 ?
O3 Ca2 Cl2 80.42(6) . 2_575 ?
C23 Ca2 Cl2 117.42(8) . 2_575 ?
C19 Ca2 Cl2 141.98(8) . 2_575 ?
C22 Ca2 Cl2 91.91(8) . 2_575 ?
C21 Ca2 Cl2 95.53(8) . 2_575 ?
C20 Ca2 Cl2 124.15(9) . 2_575 ?
O4 Ca2 Cl2 84.15(6) . . ?
O3 Ca2 Cl2 130.92(6) . . ?
C23 Ca2 Cl2 88.82(8) . . ?
C19 Ca2 Cl2 108.38(9) . . ?
C22 Ca2 Cl2 101.83(8) . . ?
C21 Ca2 Cl2 132.19(9) . . ?
C20 Ca2 Cl2 137.75(8) . . ?
Cl2 Ca2 Cl2 81.18(3) 2_575 . ?
O4 Ca2 C32 63.56(9) . . ?
O3 Ca2 C32 25.06(9) . . ?
C23 Ca2 C32 162.04(11) . . ?
C19 Ca2 C32 131.79(11) . . ?
C22 Ca2 C32 147.16(11) . . ?
C21 Ca2 C32 119.42(11) . . ?
C20 Ca2 C32 112.53(11) . . ?
Cl2 Ca2 C32 75.71(8) 2_575 . ?
Cl2 Ca2 C32 106.01(8) . . ?
O4 Ca2 Ca2 111.12(6) . 2_575 ?
O3 Ca2 Ca2 108.79(6) . 2_575 ?
C23 Ca2 Ca2 106.83(8) . 2_575 ?
C19 Ca2 Ca2 136.55(9) . 2_575 ?
C22 Ca2 Ca2 99.03(8) . 2_575 ?
C21 Ca2 Ca2 120.39(8) . 2_575 ?
C20 Ca2 Ca2 148.99(8) . 2_575 ?
Cl2 Ca2 Ca2 40.63(2) 2_575 2_575 ?
Cl2 Ca2 Ca2 40.55(2) . 2_575 ?
C32 Ca2 Ca2 91.11(8) . 2_575 ?
Ca1 Cl1 Ca1 99.62(3) . 2_666 ?
O2 Ca1 O1 74.71(9) . . ?
O2 Ca1 C5 126.26(10) . . ?
O1 Ca1 C5 134.72(10) . . ?
O2 Ca1 C4 96.84(10) . . ?
O1 Ca1 C4 125.84(10) . . ?
C5 Ca1 C4 30.65(11) . . ?
O2 Ca1 C1 141.84(10) . . ?
O1 Ca1 C1 106.42(10) . . ?
C5 Ca1 C1 30.66(11) . . ?
C4 Ca1 C1 50.60(11) . . ?
O2 Ca1 C3 91.46(10) . . ?
O1 Ca1 C3 95.27(10) . . ?
C5 Ca1 C3 50.56(11) . . ?
C4 Ca1 C3 30.68(11) . . ?
C1 Ca1 C3 50.42(11) . . ?
O2 Ca1 C2 115.71(10) . . ?
O1 Ca1 C2 84.77(10) . . ?
C5 Ca1 C2 50.45(10) . . ?
C4 Ca1 C2 50.35(11) . . ?
C1 Ca1 C2 30.57(11) . . ?
C3 Ca1 C2 30.24(11) . . ?
O2 Ca1 Cl1 127.97(6) . . ?
O1 Ca1 Cl1 85.16(6) . . ?
C5 Ca1 Cl1 102.02(8) . . ?
C4 Ca1 Cl1 132.65(9) . . ?
C1 Ca1 Cl1 89.61(8) . . ?
C3 Ca1 Cl1 138.54(8) . . ?
C2 Ca1 Cl1 109.35(8) . . ?
O2 Ca1 Cl1 80.91(6) . 2_666 ?
O1 Ca1 Cl1 134.49(7) . 2_666 ?
C5 Ca1 Cl1 90.60(8) . 2_666 ?
C4 Ca1 Cl1 94.44(8) . 2_666 ?
C1 Ca1 Cl1 116.31(8) . 2_666 ?
C3 Ca1 Cl1 123.50(8) . 2_666 ?
C2 Ca1 Cl1 140.72(8) . 2_666 ?
Cl1 Ca1 Cl1 80.38(3) . 2_666 ?
O2 Ca1 C18 25.27(9) . . ?
O1 Ca1 C18 67.98(10) . . ?
C5 Ca1 C18 147.75(11) . . ?
C4 Ca1 C18 121.01(11) . . ?
C1 Ca1 C18 165.69(10) . . ?
C3 Ca1 C18 115.89(10) . . ?
C2 Ca1 C18 135.63(11) . . ?
Cl1 Ca1 C18 102.70(7) . . ?
Cl1 Ca1 C18 73.55(7) 2_666 . ?
O2 Ca1 Ca1 107.28(6) . 2_666 ?
O1 Ca1 Ca1 113.94(7) . 2_666 ?
C5 Ca1 Ca1 98.20(8) . 2_666 ?
C4 Ca1 Ca1 119.49(8) . 2_666 ?
C1 Ca1 Ca1 106.68(8) . 2_666 ?
C3 Ca1 Ca1 148.35(8) . 2_666 ?
C2 Ca1 Ca1 136.45(8) . 2_666 ?
Cl1 Ca1 Ca1 40.405(19) . 2_666 ?
Cl1 Ca1 Ca1 39.97(2) 2_666 2_666 ?
C18 Ca1 Ca1 87.54(7) . 2_666 ?
C11 O1 C14 109.5(3) . . ?
C11 O1 Ca1 126.0(2) . . ?
C14 O1 Ca1 124.4(2) . . ?
C15 O2 C18 108.2(3) . . ?
C15 O2 Ca1 128.2(2) . . ?
C18 O2 Ca1 110.5(2) . . ?
C5 C1 C2 107.4(3) . . ?
C5 C1 C6 127.3(3) . . ?
C2 C1 C6 125.3(3) . . ?
C5 C1 Ca1 73.61(19) . . ?
C2 C1 Ca1 75.14(19) . . ?
C6 C1 Ca1 118.4(2) . . ?
C3 C2 C1 108.5(3) . . ?
C3 C2 C7 126.0(4) . . ?
C1 C2 C7 125.4(4) . . ?
C3 C2 Ca1 74.88(19) . . ?
C1 C2 Ca1 74.29(18) . . ?
C7 C2 Ca1 119.9(2) . . ?
C2 C3 C4 107.7(3) . . ?
C2 C3 C8 126.5(4) . . ?
C4 C3 C8 125.5(4) . . ?
C2 C3 Ca1 74.88(19) . . ?
C4 C3 Ca1 73.61(19) . . ?
C8 C3 Ca1 122.0(2) . . ?
C5 C4 C3 108.0(3) . . ?
C5 C4 C9 125.6(4) . . ?
C3 C4 C9 126.3(4) . . ?
C5 C4 Ca1 74.25(19) . . ?
C3 C4 Ca1 75.72(19) . . ?
C9 C4 Ca1 118.7(2) . . ?
C4 C5 C1 108.4(3) . . ?
C4 C5 C10 125.0(4) . . ?
C1 C5 C10 126.6(4) . . ?
C4 C5 Ca1 75.1(2) . . ?
C1 C5 Ca1 75.73(19) . . ?
C10 C5 Ca1 116.5(2) . . ?
O1 C11 C12A 104.5(5) . . ?
O1 C11 C12 104.5(4) . . ?
C12A C11 C12 31.1(5) . . ?
C11 C12 C13 96.1(8) . . ?
C14 C13 C12 103.8(11) . . ?
C11 C12A C13A 104.6(9) . . ?
C14 C13A C12A 98.9(9) . . ?
C13 C14 O1 104.6(7) . . ?
C13 C14 C13A 21.8(9) . . ?
O1 C14 C13A 109.9(7) . . ?
O2 C15 C16 106.4(3) . . ?
C15 C16 C17 101.5(3) . . ?
C18 C17 C16 102.2(3) . . ?
O2 C18 C17 105.7(3) . . ?
O2 C18 Ca1 44.26(14) . . ?
C17 C18 Ca1 130.0(2) . . ?
C29 O3 C32 109.2(3) . . ?
C29 O3 Ca2 127.6(2) . . ?
C32 O3 Ca2 110.2(2) . . ?
C33 O4 C36 104.3(3) . . ?
C33 O4 Ca2 124.6(2) . . ?
C36 O4 Ca2 131.0(2) . . ?
C20 C19 C23 108.4(3) . . ?
C20 C19 C24 127.1(4) . . ?
C23 C19 C24 124.2(4) . . ?
C20 C19 Ca2 75.85(19) . . ?
C23 C19 Ca2 74.29(19) . . ?
C24 C19 Ca2 121.6(2) . . ?
C19 C20 C21 107.6(3) . . ?
C19 C20 C25 126.5(4) . . ?
C21 C20 C25 125.8(4) . . ?
C19 C20 Ca2 73.74(19) . . ?
C21 C20 Ca2 74.57(19) . . ?
C25 C20 Ca2 121.1(2) . . ?
C22 C21 C20 108.1(3) . . ?
C22 C21 C26 125.4(4) . . ?
C20 C21 C26 126.4(4) . . ?
C22 C21 Ca2 74.2(2) . . ?
C20 C21 Ca2 74.97(19) . . ?
C26 C21 Ca2 120.6(3) . . ?
C21 C22 C23 108.3(3) . . ?
C21 C22 C27 125.1(4) . . ?
C23 C22 C27 126.6(4) . . ?
C21 C22 Ca2 75.4(2) . . ?
C23 C22 Ca2 74.12(19) . . ?
C27 C22 Ca2 119.7(2) . . ?
C22 C23 C19 107.7(3) . . ?
C22 C23 C28 126.6(4) . . ?
C19 C23 C28 125.5(4) . . ?
C22 C23 Ca2 75.3(2) . . ?
C19 C23 Ca2 75.0(2) . . ?
C28 C23 Ca2 119.3(2) . . ?
O3 C29 C30 104.2(3) . . ?
C31 C30 C29 102.4(4) . . ?
C30 C31 C32 103.6(4) . . ?
O3 C32 C31 105.8(3) . . ?
O3 C32 Ca2 44.78(15) . . ?
C31 C32 Ca2 136.0(3) . . ?
O4 C33 C34 105.5(3) . . ?
C35 C34 C33 104.4(3) . . ?
C36 C35 C34 103.9(3) . . ?
O4 C36 C35 103.5(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 1021899'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex6

_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H66 Ca N2 O Si'
_chemical_formula_weight         719.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   10.74110(10)
_cell_length_b                   14.40170(10)
_cell_length_c                   27.9573(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4324.72(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    23026
_cell_measurement_theta_min      3.0710
_cell_measurement_theta_max      73.7040

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5186
_exptl_absorpt_correction_T_max  0.8167
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       /w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27936
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         67.48
_reflns_number_total             7792
_reflns_number_gt                7695
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0570P)²+0.8603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_number_reflns         7792
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.21957(3) 0.48930(2) 0.228884(10) 0.02140(8) Uani 1 1 d . . .
Si1 Si 0.23413(4) 0.48716(3) 0.345825(14) 0.02138(10) Uani 1 1 d . . .
N1 N 0.29922(12) 0.59872(9) 0.36848(5) 0.0237(3) Uani 1 1 d . . .
N2 N 0.13225(13) 0.53523(9) 0.39473(5) 0.0247(3) Uani 1 1 d . . .
O1 O 0.32465(11) 0.41666(8) 0.37933(4) 0.0280(3) Uani 1 1 d . . .
C1 C 0.20524(15) 0.60970(10) 0.39915(5) 0.0230(3) Uani 1 1 d . . .
C2 C 0.18872(16) 0.68925(11) 0.43265(6) 0.0262(3) Uani 1 1 d . . .
C3 C 0.2679(2) 0.69506(13) 0.47173(7) 0.0382(4) Uani 1 1 d . . .
H3 H 0.3292 0.6487 0.4770 0.046 Uiso 1 1 calc R . .
C4 C 0.2565(2) 0.76939(15) 0.50298(7) 0.0491(5) Uani 1 1 d . . .
H4 H 0.3099 0.7736 0.5300 0.059 Uiso 1 1 calc R . .
C5 C 0.1678(2) 0.83735(14) 0.49508(7) 0.0464(5) Uani 1 1 d . . .
H5 H 0.1607 0.8882 0.5166 0.056 Uiso 1 1 calc R . .
C6 C 0.0900(2) 0.83139(13) 0.45605(7) 0.0390(4) Uani 1 1 d . . .
H6 H 0.0294 0.8783 0.4506 0.047 Uiso 1 1 calc R . .
C7 C 0.09980(16) 0.75706(11) 0.42466(6) 0.0295(4) Uani 1 1 d . . .
H7 H 0.0458 0.7528 0.3978 0.035 Uiso 1 1 calc R . .
C8 C 0.02526(16) 0.50415(12) 0.42442(6) 0.0312(4) Uani 1 1 d . . .
C9 C -0.00209(19) 0.40491(13) 0.40975(8) 0.0420(5) Uani 1 1 d . . .
H9A H -0.0179 0.4025 0.3753 0.063 Uiso 1 1 calc R . .
H9B H -0.0756 0.3825 0.4270 0.063 Uiso 1 1 calc R . .
H9C H 0.0696 0.3656 0.4175 0.063 Uiso 1 1 calc R . .
C10 C 0.0539(3) 0.5086(2) 0.47724(8) 0.0708(8) Uani 1 1 d . . .
H10A H 0.1287 0.4720 0.4840 0.106 Uiso 1 1 calc R . .
H10B H -0.0165 0.4835 0.4954 0.106 Uiso 1 1 calc R . .
H10C H 0.0681 0.5733 0.4866 0.106 Uiso 1 1 calc R . .
C11 C -0.0912(2) 0.56252(15) 0.41237(10) 0.0541(6) Uani 1 1 d . . .
H11A H -0.0766 0.6274 0.4213 0.081 Uiso 1 1 calc R . .
H11B H -0.1629 0.5384 0.4301 0.081 Uiso 1 1 calc R . .
H11C H -0.1081 0.5588 0.3780 0.081 Uiso 1 1 calc R . .
C12 C 0.39805(15) 0.66301(11) 0.35182(7) 0.0302(4) Uani 1 1 d . . .
C13 C 0.41687(19) 0.64232(13) 0.29867(7) 0.0408(5) Uani 1 1 d . . .
H13A H 0.4365 0.5764 0.2945 0.061 Uiso 1 1 calc R . .
H13B H 0.4857 0.6801 0.2864 0.061 Uiso 1 1 calc R . .
H13C H 0.3405 0.6573 0.2811 0.061 Uiso 1 1 calc R . .
C14 C 0.5173(2) 0.64134(18) 0.37865(11) 0.0607(7) Uani 1 1 d . . .
H14A H 0.5050 0.6530 0.4129 0.091 Uiso 1 1 calc R . .
H14B H 0.5846 0.6810 0.3667 0.091 Uiso 1 1 calc R . .
H14C H 0.5394 0.5760 0.3738 0.091 Uiso 1 1 calc R . .
C15 C 0.36564(18) 0.76594(12) 0.35692(7) 0.0355(4) Uani 1 1 d . . .
H15A H 0.2846 0.7779 0.3420 0.053 Uiso 1 1 calc R . .
H15B H 0.4296 0.8035 0.3411 0.053 Uiso 1 1 calc R . .
H15C H 0.3620 0.7824 0.3909 0.053 Uiso 1 1 calc R . .
C16 C 0.45487(15) 0.45297(12) 0.20026(6) 0.0272(3) Uani 1 1 d . . .
C17 C 0.37966(15) 0.43944(12) 0.15954(6) 0.0277(3) Uani 1 1 d . . .
C18 C 0.30176(14) 0.36185(12) 0.16804(6) 0.0266(3) Uani 1 1 d . . .
C19 C 0.32891(14) 0.32704(11) 0.21438(6) 0.0244(3) Uani 1 1 d . . .
C20 C 0.42466(14) 0.38312(11) 0.23424(6) 0.0245(3) Uani 1 1 d . . .
C21 C 0.56124(16) 0.52074(14) 0.20338(7) 0.0378(4) Uani 1 1 d . . .
H21A H 0.5902 0.5247 0.2366 0.057 Uiso 1 1 calc R . .
H21B H 0.5331 0.5821 0.1927 0.057 Uiso 1 1 calc R . .
H21C H 0.6296 0.4996 0.1829 0.057 Uiso 1 1 calc R . .
C22 C 0.39785(18) 0.48846(15) 0.11256(7) 0.0411(4) Uani 1 1 d . . .
H22A H 0.4759 0.4677 0.0979 0.062 Uiso 1 1 calc R . .
H22B H 0.4014 0.5556 0.1180 0.062 Uiso 1 1 calc R . .
H22C H 0.3281 0.4740 0.0912 0.062 Uiso 1 1 calc R . .
C23 C 0.21378(18) 0.31804(14) 0.13280(7) 0.0375(4) Uani 1 1 d . . .
H23A H 0.1730 0.3667 0.1139 0.056 Uiso 1 1 calc R . .
H23B H 0.1507 0.2821 0.1501 0.056 Uiso 1 1 calc R . .
H23C H 0.2603 0.2768 0.1114 0.056 Uiso 1 1 calc R . .
C24 C 0.27093(17) 0.24230(12) 0.23691(7) 0.0343(4) Uani 1 1 d . . .
H24A H 0.1875 0.2578 0.2486 0.052 Uiso 1 1 calc R . .
H24B H 0.3227 0.2214 0.2637 0.052 Uiso 1 1 calc R . .
H24C H 0.2650 0.1926 0.2131 0.052 Uiso 1 1 calc R . .
C25 C 0.49637(16) 0.36424(13) 0.27947(6) 0.0331(4) Uani 1 1 d . . .
H25A H 0.5772 0.3368 0.2714 0.050 Uiso 1 1 calc R . .
H25B H 0.4492 0.3211 0.2996 0.050 Uiso 1 1 calc R . .
H25C H 0.5094 0.4226 0.2968 0.050 Uiso 1 1 calc R . .
C26 C 0.11369(16) 0.64617(12) 0.19859(7) 0.0336(4) Uani 1 1 d . . .
C27 C 0.07520(16) 0.57860(13) 0.16502(6) 0.0310(4) Uani 1 1 d . . .
C28 C -0.00464(14) 0.51571(11) 0.18884(6) 0.0258(3) Uani 1 1 d . . .
C29 C -0.01626(15) 0.54526(11) 0.23682(6) 0.0265(3) Uani 1 1 d . . .
C30 C 0.05649(15) 0.62589(12) 0.24271(6) 0.0293(4) Uani 1 1 d . . .
C31 C 0.1925(2) 0.73029(17) 0.18777(11) 0.0664(8) Uani 1 1 d . . .
H31A H 0.1441 0.7745 0.1686 0.100 Uiso 1 1 calc R . .
H31B H 0.2666 0.7112 0.1698 0.100 Uiso 1 1 calc R . .
H31C H 0.2179 0.7598 0.2178 0.100 Uiso 1 1 calc R . .
C32 C 0.0977(2) 0.5828(2) 0.11206(7) 0.0588(7) Uani 1 1 d . . .
H32A H 0.0282 0.6149 0.0965 0.088 Uiso 1 1 calc R . .
H32B H 0.1045 0.5196 0.0993 0.088 Uiso 1 1 calc R . .
H32C H 0.1752 0.6166 0.1058 0.088 Uiso 1 1 calc R . .
C33 C -0.07838(19) 0.43981(14) 0.16572(9) 0.0449(5) Uani 1 1 d . . .
H33A H -0.0288 0.4111 0.1403 0.067 Uiso 1 1 calc R . .
H33B H -0.1548 0.4658 0.1520 0.067 Uiso 1 1 calc R . .
H33C H -0.0998 0.3928 0.1897 0.067 Uiso 1 1 calc R . .
C34 C -0.09796(17) 0.49991(17) 0.27353(7) 0.0468(5) Uani 1 1 d . . .
H34A H -0.1450 0.4493 0.2586 0.070 Uiso 1 1 calc R . .
H34B H -0.1560 0.5459 0.2866 0.070 Uiso 1 1 calc R . .
H34C H -0.0463 0.4749 0.2994 0.070 Uiso 1 1 calc R . .
C35 C 0.0604(2) 0.68434(16) 0.28746(9) 0.0549(6) Uani 1 1 d . . .
H35A H 0.1455 0.7067 0.2927 0.082 Uiso 1 1 calc R . .
H35B H 0.0341 0.6468 0.3149 0.082 Uiso 1 1 calc R . .
H35C H 0.0042 0.7375 0.2839 0.082 Uiso 1 1 calc R . .
C36 C 0.31677(15) 0.32301(11) 0.38770(6) 0.0254(3) Uani 1 1 d . . .
C37 C 0.23268(16) 0.26913(12) 0.36230(6) 0.0301(4) Uani 1 1 d . . .
H37 H 0.1815 0.2975 0.3388 0.036 Uiso 1 1 calc R . .
C38 C 0.22199(18) 0.17474(12) 0.37067(7) 0.0367(4) Uani 1 1 d . . .
H38 H 0.1648 0.1383 0.3528 0.044 Uiso 1 1 calc R . .
C39 C 0.2953(2) 0.13454(13) 0.40522(8) 0.0433(5) Uani 1 1 d . . .
H39 H 0.2876 0.0701 0.4120 0.052 Uiso 1 1 calc R . .
C40 C 0.3805(2) 0.18801(13) 0.43017(7) 0.0415(4) Uani 1 1 d . . .
H40 H 0.4315 0.1586 0.4534 0.050 Uiso 1 1 calc R . .
C41 C 0.39482(17) 0.28347(12) 0.42263(6) 0.0309(4) Uani 1 1 d . . .
C42 C 0.49211(19) 0.34049(13) 0.45013(7) 0.0398(4) Uani 1 1 d . . .
C43 C 0.5892(2) 0.37831(16) 0.41481(9) 0.0496(5) Uani 1 1 d . . .
H43A H 0.6271 0.3266 0.3973 0.074 Uiso 1 1 calc R . .
H43B H 0.6539 0.4120 0.4324 0.074 Uiso 1 1 calc R . .
H43C H 0.5487 0.4205 0.3922 0.074 Uiso 1 1 calc R . .
C44 C 0.5612(3) 0.28158(18) 0.48773(10) 0.0682(8) Uani 1 1 d . . .
H44A H 0.5015 0.2582 0.5113 0.102 Uiso 1 1 calc R . .
H44B H 0.6238 0.3200 0.5039 0.102 Uiso 1 1 calc R . .
H44C H 0.6023 0.2292 0.4719 0.102 Uiso 1 1 calc R . .
C45 C 0.4302(3) 0.42127(16) 0.47698(7) 0.0517(6) Uani 1 1 d . . .
H45A H 0.3901 0.4630 0.4539 0.078 Uiso 1 1 calc R . .
H45B H 0.4934 0.4556 0.4950 0.078 Uiso 1 1 calc R . .
H45C H 0.3674 0.3968 0.4991 0.078 Uiso 1 1 calc R . .


_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 C19 2.6466(15) . ?
Ca1 C18 2.6538(15) . ?
Ca1 C30 2.6621(16) . ?
Ca1 C29 2.6674(16) . ?
Ca1 C26 2.6673(17) . ?
Ca1 C28 2.6828(15) . ?
Ca1 C20 2.6859(15) . ?
Ca1 C17 2.6889(16) . ?
Ca1 C27 2.6920(16) . ?
Ca1 C16 2.7022(16) . ?
Ca1 Si1 3.2732(5) . ?
Si1 O1 1.6893(12) . ?
Si1 N1 1.8632(13) . ?
Si1 N2 1.8831(14) . ?
Si1 C1 2.3310(16) . ?
N1 C1 1.334(2) . ?
N1 C12 1.484(2) . ?
N2 C1 1.334(2) . ?
N2 C8 1.487(2) . ?
O1 C36 1.3715(19) . ?
C1 C2 1.490(2) . ?
C2 C7 1.384(2) . ?
C2 C3 1.387(2) . ?
C3 C4 1.387(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.378(3) . ?
C6 C7 1.388(2) . ?
C8 C10 1.510(3) . ?
C8 C9 1.516(2) . ?
C8 C11 1.545(3) . ?
C12 C14 1.517(3) . ?
C12 C13 1.529(3) . ?
C12 C15 1.529(2) . ?
C16 C17 1.409(2) . ?
C16 C20 1.421(2) . ?
C16 C21 1.505(2) . ?
C17 C18 1.416(2) . ?
C17 C22 1.504(3) . ?
C18 C19 1.420(2) . ?
C18 C23 1.504(2) . ?
C19 C20 1.421(2) . ?
C19 C24 1.508(2) . ?
C20 C25 1.505(2) . ?
C26 C30 1.409(3) . ?
C26 C27 1.414(3) . ?
C26 C31 1.508(3) . ?
C27 C28 1.414(2) . ?
C27 C32 1.501(3) . ?
C28 C29 1.413(2) . ?
C28 C33 1.497(2) . ?
C29 C30 1.409(2) . ?
C29 C34 1.500(3) . ?
C30 C35 1.508(3) . ?
C36 C37 1.387(2) . ?
C36 C41 1.407(2) . ?
C37 C38 1.384(2) . ?
C38 C39 1.374(3) . ?
C39 C40 1.384(3) . ?
C40 C41 1.399(2) . ?
C41 C42 1.535(3) . ?
C42 C45 1.536(3) . ?
C42 C43 1.536(3) . ?
C42 C44 1.542(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Ca1 C18 31.07(5) . . ?
C19 Ca1 C30 165.16(5) . . ?
C18 Ca1 C30 145.39(5) . . ?
C19 Ca1 C29 134.50(5) . . ?
C18 Ca1 C29 125.32(5) . . ?
C30 Ca1 C29 30.67(5) . . ?
C19 Ca1 C26 152.67(6) . . ?
C18 Ca1 C26 121.61(6) . . ?
C30 Ca1 C26 30.66(6) . . ?
C29 Ca1 C26 50.63(5) . . ?
C19 Ca1 C28 117.36(5) . . ?
C18 Ca1 C28 97.42(5) . . ?
C30 Ca1 C28 50.60(5) . . ?
C29 Ca1 C28 30.62(5) . . ?
C26 Ca1 C28 50.56(5) . . ?
C19 Ca1 C20 30.89(5) . . ?
C18 Ca1 C20 50.88(5) . . ?
C30 Ca1 C20 162.23(5) . . ?
C29 Ca1 C20 161.13(5) . . ?
C26 Ca1 C20 148.17(5) . . ?
C28 Ca1 C20 147.17(5) . . ?
C19 Ca1 C17 50.95(5) . . ?
C18 Ca1 C17 30.73(5) . . ?
C30 Ca1 C17 136.29(5) . . ?
C29 Ca1 C17 138.41(5) . . ?
C26 Ca1 C17 105.66(6) . . ?
C28 Ca1 C17 108.12(5) . . ?
C20 Ca1 C17 50.48(5) . . ?
C19 Ca1 C27 125.16(5) . . ?
C18 Ca1 C27 95.56(5) . . ?
C30 Ca1 C27 50.53(5) . . ?
C29 Ca1 C27 50.49(5) . . ?
C26 Ca1 C27 30.59(6) . . ?
C28 Ca1 C27 30.51(5) . . ?
C20 Ca1 C27 141.39(5) . . ?
C17 Ca1 C27 91.02(5) . . ?
C19 Ca1 C16 50.85(5) . . ?
C18 Ca1 C16 50.59(5) . . ?
C30 Ca1 C16 143.28(6) . . ?
C29 Ca1 C16 166.25(5) . . ?
C26 Ca1 C16 117.96(6) . . ?
C28 Ca1 C16 138.03(5) . . ?
C20 Ca1 C16 30.58(5) . . ?
C17 Ca1 C16 30.31(5) . . ?
C27 Ca1 C16 115.78(5) . . ?
C19 Ca1 Si1 97.09(4) . . ?
C18 Ca1 Si1 128.16(4) . . ?
C30 Ca1 Si1 83.88(4) . . ?
C29 Ca1 Si1 88.01(4) . . ?
C26 Ca1 Si1 110.22(4) . . ?
C28 Ca1 Si1 117.45(4) . . ?
C20 Ca1 Si1 84.25(4) . . ?
C17 Ca1 Si1 133.39(4) . . ?
C27 Ca1 Si1 133.99(4) . . ?
C16 Ca1 Si1 104.43(4) . . ?
O1 Si1 N1 96.54(6) . . ?
O1 Si1 N2 98.79(6) . . ?
N1 Si1 N2 69.77(6) . . ?
O1 Si1 C1 100.20(6) . . ?
N1 Si1 C1 34.88(6) . . ?
N2 Si1 C1 34.91(6) . . ?
O1 Si1 Ca1 125.94(4) . . ?
N1 Si1 Ca1 110.44(4) . . ?
N2 Si1 Ca1 133.95(5) . . ?
C1 Si1 Ca1 128.71(4) . . ?
C1 N1 C12 132.02(14) . . ?
C1 N1 Si1 92.11(9) . . ?
C12 N1 Si1 134.42(11) . . ?
C1 N2 C8 130.13(14) . . ?
C1 N2 Si1 91.22(10) . . ?
C8 N2 Si1 138.06(11) . . ?
C36 O1 Si1 130.56(11) . . ?
N2 C1 N1 106.85(13) . . ?
N2 C1 C2 127.31(15) . . ?
N1 C1 C2 125.82(14) . . ?
N2 C1 Si1 53.87(8) . . ?
N1 C1 Si1 53.01(8) . . ?
C2 C1 Si1 178.78(12) . . ?
C7 C2 C3 120.50(16) . . ?
C7 C2 C1 121.54(15) . . ?
C3 C2 C1 117.93(16) . . ?
C2 C3 C4 119.26(19) . . ?
C5 C4 C3 120.40(19) . . ?
C6 C5 C4 120.03(18) . . ?
C5 C6 C7 120.17(19) . . ?
C2 C7 C6 119.64(17) . . ?
N2 C8 C10 112.07(16) . . ?
N2 C8 C9 106.42(13) . . ?
C10 C8 C9 110.14(18) . . ?
N2 C8 C11 109.92(15) . . ?
C10 C8 C11 110.8(2) . . ?
C9 C8 C11 107.29(16) . . ?
N1 C12 C14 108.71(14) . . ?
N1 C12 C13 106.15(14) . . ?
C14 C12 C13 109.19(18) . . ?
N1 C12 C15 114.38(14) . . ?
C14 C12 C15 110.21(17) . . ?
C13 C12 C15 108.03(15) . . ?
C17 C16 C20 108.13(15) . . ?
C17 C16 C21 124.85(16) . . ?
C20 C16 C21 126.42(16) . . ?
C17 C16 Ca1 74.32(9) . . ?
C20 C16 Ca1 74.07(9) . . ?
C21 C16 Ca1 124.55(11) . . ?
C16 C17 C18 108.20(15) . . ?
C16 C17 C22 124.48(16) . . ?
C18 C17 C22 126.41(16) . . ?
C16 C17 Ca1 75.37(9) . . ?
C18 C17 Ca1 73.26(9) . . ?
C22 C17 Ca1 125.97(12) . . ?
C17 C18 C19 108.08(14) . . ?
C17 C18 C23 126.34(16) . . ?
C19 C18 C23 125.37(16) . . ?
C17 C18 Ca1 76.01(9) . . ?
C19 C18 Ca1 74.19(9) . . ?
C23 C18 Ca1 120.07(11) . . ?
C18 C19 C20 107.74(14) . . ?
C18 C19 C24 125.60(15) . . ?
C20 C19 C24 126.58(15) . . ?
C18 C19 Ca1 74.74(9) . . ?
C20 C19 Ca1 76.08(8) . . ?
C24 C19 Ca1 117.86(10) . . ?
C19 C20 C16 107.85(14) . . ?
C19 C20 C25 126.58(16) . . ?
C16 C20 C25 124.93(15) . . ?
C19 C20 Ca1 73.03(8) . . ?
C16 C20 Ca1 75.34(9) . . ?
C25 C20 Ca1 124.71(10) . . ?
C30 C26 C27 108.13(15) . . ?
C30 C26 C31 125.9(2) . . ?
C27 C26 C31 125.7(2) . . ?
C30 C26 Ca1 74.47(9) . . ?
C27 C26 Ca1 75.67(10) . . ?
C31 C26 Ca1 120.31(13) . . ?
C28 C27 C26 107.78(15) . . ?
C28 C27 C32 126.03(19) . . ?
C26 C27 C32 125.4(2) . . ?
C28 C27 Ca1 74.39(9) . . ?
C26 C27 Ca1 73.74(9) . . ?
C32 C27 Ca1 125.48(13) . . ?
C29 C28 C27 107.93(15) . . ?
C29 C28 C33 125.69(17) . . ?
C27 C28 C33 125.82(17) . . ?
C29 C28 Ca1 74.09(9) . . ?
C27 C28 Ca1 75.10(9) . . ?
C33 C28 Ca1 123.49(11) . . ?
C30 C29 C28 108.08(15) . . ?
C30 C29 C34 127.09(17) . . ?
C28 C29 C34 124.76(16) . . ?
C30 C29 Ca1 74.46(9) . . ?
C28 C29 Ca1 75.30(9) . . ?
C34 C29 Ca1 118.74(11) . . ?
C26 C30 C29 108.07(15) . . ?
C26 C30 C35 126.75(19) . . ?
C29 C30 C35 124.92(19) . . ?
C26 C30 Ca1 74.87(10) . . ?
C29 C30 Ca1 74.87(9) . . ?
C35 C30 Ca1 120.96(11) . . ?
O1 C36 C37 120.21(15) . . ?
O1 C36 C41 118.66(15) . . ?
C37 C36 C41 121.13(15) . . ?
C38 C37 C36 121.14(17) . . ?
C39 C38 C37 119.02(18) . . ?
C38 C39 C40 119.91(17) . . ?
C39 C40 C41 122.91(19) . . ?
C40 C41 C36 115.88(17) . . ?
C40 C41 C42 121.66(17) . . ?
C36 C41 C42 122.44(15) . . ?
C45 C42 C41 110.79(17) . . ?
C45 C42 C43 109.86(18) . . ?
C41 C42 C43 109.27(16) . . ?
C45 C42 C44 106.99(19) . . ?
C41 C42 C44 112.02(17) . . ?
C43 C42 C44 107.8(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.039
_database_code_depnum_ccdc_archive 'CCDC 1021900'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex10

_audit_creation_method           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36.50 H44 Ca O'
_chemical_formula_weight         538.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.91840(10)
_cell_length_b                   14.12280(10)
_cell_length_c                   23.6163(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9090(10)
_cell_angle_gamma                90.00
_cell_volume                     3236.87(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15141
_cell_measurement_theta_min      3.6570
_cell_measurement_theta_max      73.5520

_exptl_crystal_description       rod
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1164
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5334
_exptl_absorpt_correction_T_max  0.8230
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21947
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         67.48
_reflns_number_total             5811
_reflns_number_gt                5684
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0406P)²+5.5300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00116(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5811
_refine_ls_number_parameters     390
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1445
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.24837(5) 0.01252(4) 0.29989(2) 0.02402(16) Uani 1 1 d . . .
O1 O 0.2204(2) 0.00399(16) 0.20121(8) 0.0387(5) Uani 1 1 d . . .
C1 C 0.5195(3) 0.0308(2) 0.31894(12) 0.0299(6) Uani 1 1 d . . .
C2 C 0.4837(3) 0.0381(2) 0.37352(11) 0.0284(6) Uani 1 1 d . . .
C3 C 0.4088(3) 0.1230(2) 0.37478(11) 0.0292(6) Uani 1 1 d . . .
C4 C 0.3977(3) 0.1685(2) 0.32053(12) 0.0308(6) Uani 1 1 d . . .
C5 C 0.4682(3) 0.1120(2) 0.28635(11) 0.0311(6) Uani 1 1 d . . .
C6 C 0.0104(3) -0.00142(19) 0.33534(12) 0.0284(6) Uani 1 1 d . . .
C7 C 0.1047(3) -0.0555(2) 0.37539(12) 0.0309(6) Uani 1 1 d . . .
C8 C 0.1441(3) -0.1348(2) 0.34572(13) 0.0322(6) Uani 1 1 d . . .
C9 C 0.0724(3) -0.12945(19) 0.28752(12) 0.0298(6) Uani 1 1 d . . .
C10 C -0.0094(3) -0.0473(2) 0.28088(11) 0.0279(6) Uani 1 1 d . . .
C11 C 0.5978(3) -0.0498(2) 0.29917(15) 0.0444(8) Uani 1 1 d . . .
H11A H 0.6961 -0.0433 0.3164 0.067 Uiso 1 1 calc R . .
H11B H 0.5846 -0.0486 0.2569 0.067 Uiso 1 1 calc R . .
H11C H 0.5637 -0.1100 0.3114 0.067 Uiso 1 1 calc R . .
C12 C 0.5281(3) -0.0302(2) 0.42311(13) 0.0403(7) Uani 1 1 d . . .
H12A H 0.6175 -0.0105 0.4461 0.060 Uiso 1 1 calc R . .
H12B H 0.5360 -0.0940 0.4078 0.060 Uiso 1 1 calc R . .
H12C H 0.4594 -0.0305 0.4476 0.060 Uiso 1 1 calc R . .
C13 C 0.3626(4) 0.1638(2) 0.42670(13) 0.0416(7) Uani 1 1 d . . .
H13A H 0.4305 0.2103 0.4457 0.062 Uiso 1 1 calc R . .
H13B H 0.3543 0.1129 0.4539 0.062 Uiso 1 1 calc R . .
H13C H 0.2731 0.1949 0.4141 0.062 Uiso 1 1 calc R . .
C14 C 0.3318(3) 0.2633(2) 0.30479(15) 0.0439(8) Uani 1 1 d . . .
H14A H 0.3982 0.3136 0.3191 0.066 Uiso 1 1 calc R . .
H14B H 0.2510 0.2700 0.3224 0.066 Uiso 1 1 calc R . .
H14C H 0.3032 0.2682 0.2626 0.066 Uiso 1 1 calc R . .
C15 C 0.4958(3) 0.1383(3) 0.22778(13) 0.0482(9) Uani 1 1 d . . .
H15A H 0.5862 0.1688 0.2327 0.072 Uiso 1 1 calc R . .
H15B H 0.4243 0.1821 0.2084 0.072 Uiso 1 1 calc R . .
H15C H 0.4947 0.0810 0.2043 0.072 Uiso 1 1 calc R . .
C16 C 0.0765(4) -0.2037(2) 0.24202(15) 0.0471(8) Uani 1 1 d . . .
H16A H 0.0101 -0.2539 0.2451 0.071 Uiso 1 1 calc R . .
H16B H 0.1693 -0.2309 0.2479 0.071 Uiso 1 1 calc R . .
H16C H 0.0528 -0.1748 0.2035 0.071 Uiso 1 1 calc R . .
C17 C 0.2334(4) -0.2157(2) 0.37302(17) 0.0507(9) Uani 1 1 d . . .
H17A H 0.1751 -0.2659 0.3838 0.076 Uiso 1 1 calc R . .
H17B H 0.2974 -0.1932 0.4077 0.076 Uiso 1 1 calc R . .
H17C H 0.2857 -0.2407 0.3454 0.076 Uiso 1 1 calc R . .
C18 C 0.1391(4) -0.0393(3) 0.43978(13) 0.0494(9) Uani 1 1 d . . .
H18A H 0.0731 -0.0735 0.4579 0.074 Uiso 1 1 calc R . .
H18B H 0.1340 0.0286 0.4478 0.074 Uiso 1 1 calc R . .
H18C H 0.2324 -0.0623 0.4556 0.074 Uiso 1 1 calc R . .
C19 C -0.0640(4) 0.0854(2) 0.35011(16) 0.0452(8) Uani 1 1 d . . .
H19A H -0.1159 0.0694 0.3799 0.068 Uiso 1 1 calc R . .
H19B H -0.1276 0.1080 0.3154 0.068 Uiso 1 1 calc R . .
H19C H 0.0032 0.1351 0.3647 0.068 Uiso 1 1 calc R . .
C20 C -0.1032(3) -0.0147(3) 0.22556(13) 0.0419(7) Uani 1 1 d . . .
H20A H -0.1935 -0.0449 0.2218 0.063 Uiso 1 1 calc R . .
H20B H -0.0629 -0.0322 0.1925 0.063 Uiso 1 1 calc R . .
H20C H -0.1139 0.0542 0.2265 0.063 Uiso 1 1 calc R . .
C21 C 0.1934(3) 0.1012(2) 0.11886(11) 0.0294(6) Uani 1 1 d . . .
C22 C 0.1379(3) 0.1775(2) 0.14340(14) 0.0390(7) Uani 1 1 d . . .
H22A H 0.1002 0.1679 0.1768 0.047 Uiso 1 1 calc R . .
C23 C 0.1367(3) 0.2668(2) 0.12008(16) 0.0466(8) Uani 1 1 d . . .
H23A H 0.0981 0.3183 0.1372 0.056 Uiso 1 1 calc R . .
C24 C 0.1918(3) 0.2812(2) 0.07177(17) 0.0484(8) Uani 1 1 d . . .
H24A H 0.1915 0.3429 0.0556 0.058 Uiso 1 1 calc R . .
C25 C 0.2478(4) 0.2060(2) 0.04661(16) 0.0472(8) Uani 1 1 d . . .
H25A H 0.2862 0.2163 0.0135 0.057 Uiso 1 1 calc R . .
C26 C 0.2475(3) 0.1160(2) 0.06972(13) 0.0359(7) Uani 1 1 d . . .
H26A H 0.2843 0.0643 0.0521 0.043 Uiso 1 1 calc R . .
C27 C 0.2088(3) -0.0806(2) 0.11477(11) 0.0280(6) Uani 1 1 d . . .
C28 C 0.2894(3) -0.1571(2) 0.13936(13) 0.0353(7) Uani 1 1 d . . .
H28A H 0.3457 -0.1508 0.1769 0.042 Uiso 1 1 calc R . .
C29 C 0.2886(3) -0.2412(2) 0.11019(15) 0.0417(7) Uani 1 1 d . . .
H29A H 0.3451 -0.2923 0.1271 0.050 Uiso 1 1 calc R . .
C30 C 0.2048(4) -0.2507(2) 0.05603(16) 0.0483(8) Uani 1 1 d . . .
H30A H 0.2037 -0.3088 0.0357 0.058 Uiso 1 1 calc R . .
C31 C 0.1228(4) -0.1768(2) 0.03113(14) 0.0477(8) Uani 1 1 d . . .
H31A H 0.0643 -0.1846 -0.0059 0.057 Uiso 1 1 calc R . .
C32 C 0.1257(3) -0.0912(2) 0.06012(13) 0.0374(7) Uani 1 1 d . . .
H32A H 0.0708 -0.0398 0.0426 0.045 Uiso 1 1 calc R . .
C33 C 0.2071(3) 0.0079(2) 0.14798(11) 0.0297(6) Uani 1 1 d . . .
C34 C 0.5574(8) 0.0085(5) 0.0321(3) 0.0498(12) Uani 0.50 1 d PDU A -1
C35 C 0.4912(10) -0.0780(7) 0.0250(4) 0.0512(15) Uani 0.50 1 d PDU A -1
H35A H 0.5075 -0.1234 0.0553 0.061 Uiso 0.50 1 calc PR A -1
C36 C 0.4027(8) -0.0974(5) -0.0257(3) 0.0625(14) Uani 0.50 1 d PDU A -1
H36A H 0.3561 -0.1565 -0.0297 0.075 Uiso 0.50 1 calc PR A -1
C37 C 0.3782(12) -0.0373(7) -0.0700(5) 0.0725(17) Uani 0.50 1 d PDU A -1
H37A H 0.3201 -0.0551 -0.1056 0.087 Uiso 0.50 1 calc PR A -1
C38 C 0.4385(9) 0.0518(6) -0.0634(3) 0.0673(15) Uani 0.50 1 d PDU A -1
H38A H 0.4177 0.0973 -0.0936 0.081 Uiso 0.50 1 calc PR A -1
C39 C 0.5302(11) 0.0731(8) -0.0120(4) 0.0531(15) Uani 0.50 1 d PDU A -1
H39A H 0.5743 0.1332 -0.0075 0.064 Uiso 0.50 1 calc PR A -1
C40 C 0.6568(14) 0.0259(9) 0.0879(5) 0.088(3) Uani 0.50 1 d PDU A -1
H40A H 0.6591 -0.0294 0.1131 0.132 Uiso 0.50 1 calc PR A -1
H40B H 0.6276 0.0817 0.1069 0.132 Uiso 0.50 1 calc PR A -1
H40C H 0.7489 0.0369 0.0802 0.132 Uiso 0.50 1 calc PR A -1


_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 2.2925(19) . ?
Ca1 C2 2.632(3) . ?
Ca1 C3 2.633(3) . ?
Ca1 C9 2.634(3) . ?
Ca1 C10 2.641(3) . ?
Ca1 C4 2.644(3) . ?
Ca1 C1 2.646(3) . ?
Ca1 C8 2.652(3) . ?
Ca1 C5 2.668(3) . ?
Ca1 C6 2.670(3) . ?
Ca1 C7 2.680(3) . ?
O1 C33 1.238(3) . ?
C1 C2 1.410(4) . ?
C1 C5 1.415(4) . ?
C1 C11 1.505(4) . ?
C2 C3 1.413(4) . ?
C2 C12 1.511(4) . ?
C3 C4 1.418(4) . ?
C3 C13 1.509(4) . ?
C4 C5 1.418(4) . ?
C4 C14 1.503(4) . ?
C5 C15 1.511(4) . ?
C6 C7 1.410(4) . ?
C6 C10 1.417(4) . ?
C6 C19 1.508(4) . ?
C7 C8 1.418(4) . ?
C7 C18 1.506(4) . ?
C8 C9 1.413(4) . ?
C8 C17 1.506(4) . ?
C9 C10 1.406(4) . ?
C9 C16 1.508(4) . ?
C10 C20 1.511(4) . ?
C21 C22 1.390(4) . ?
C21 C26 1.391(4) . ?
C21 C33 1.481(4) . ?
C22 C23 1.375(5) . ?
C23 C24 1.378(5) . ?
C24 C25 1.388(5) . ?
C25 C26 1.383(4) . ?
C27 C32 1.389(4) . ?
C27 C28 1.397(4) . ?
C27 C33 1.477(4) . ?
C28 C29 1.372(5) . ?
C29 C30 1.381(5) . ?
C30 C31 1.378(5) . ?
C31 C32 1.387(4) . ?
C34 C39 1.369(9) . ?
C34 C35 1.380(10) . ?
C34 C40 1.494(12) . ?
C35 C36 1.359(10) . ?
C36 C37 1.329(10) . ?
C37 C38 1.388(11) . ?
C38 C39 1.391(10) . ?

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 C2 125.69(8) . . ?
O1 Ca1 C3 130.05(8) . . ?
C2 Ca1 C3 31.13(9) . . ?
O1 Ca1 C9 84.77(8) . . ?
C2 Ca1 C9 130.89(9) . . ?
C3 Ca1 C9 145.09(9) . . ?
O1 Ca1 C10 84.30(8) . . ?
C2 Ca1 C10 148.37(8) . . ?
C3 Ca1 C10 137.17(9) . . ?
C9 Ca1 C10 30.90(9) . . ?
O1 Ca1 C4 100.19(8) . . ?
C2 Ca1 C4 51.45(9) . . ?
C3 Ca1 C4 31.17(8) . . ?
C9 Ca1 C4 171.09(9) . . ?
C10 Ca1 C4 141.61(9) . . ?
O1 Ca1 C1 94.78(8) . . ?
C2 Ca1 C1 30.98(8) . . ?
C3 Ca1 C1 51.37(9) . . ?
C9 Ca1 C1 136.04(9) . . ?
C10 Ca1 C1 166.93(9) . . ?
C4 Ca1 C1 51.40(9) . . ?
O1 Ca1 C8 113.46(9) . . ?
C2 Ca1 C8 101.86(9) . . ?
C3 Ca1 C8 115.03(9) . . ?
C9 Ca1 C8 31.01(9) . . ?
C10 Ca1 C8 51.18(9) . . ?
C4 Ca1 C8 146.05(9) . . ?
C1 Ca1 C8 118.38(9) . . ?
O1 Ca1 C5 80.57(8) . . ?
C2 Ca1 C5 51.06(8) . . ?
C3 Ca1 C5 51.17(8) . . ?
C9 Ca1 C5 157.89(9) . . ?
C10 Ca1 C5 159.13(9) . . ?
C4 Ca1 C5 30.97(9) . . ?
C1 Ca1 C5 30.89(9) . . ?
C8 Ca1 C5 149.22(9) . . ?
O1 Ca1 C6 112.69(8) . . ?
C2 Ca1 C6 121.59(9) . . ?
C3 Ca1 C6 106.50(9) . . ?
C9 Ca1 C6 50.98(8) . . ?
C10 Ca1 C6 30.95(8) . . ?
C4 Ca1 C6 120.11(9) . . ?
C1 Ca1 C6 152.52(9) . . ?
C8 Ca1 C6 50.92(8) . . ?
C5 Ca1 C6 150.91(9) . . ?
O1 Ca1 C7 133.49(8) . . ?
C2 Ca1 C7 97.49(9) . . ?
C3 Ca1 C7 95.51(8) . . ?
C9 Ca1 C7 50.94(8) . . ?
C10 Ca1 C7 50.92(8) . . ?
C4 Ca1 C7 122.06(9) . . ?
C1 Ca1 C7 125.67(9) . . ?
C8 Ca1 C7 30.84(9) . . ?
C5 Ca1 C7 145.94(8) . . ?
C6 Ca1 C7 30.57(9) . . ?
C33 O1 Ca1 174.4(2) . . ?
C2 C1 C5 107.9(2) . . ?
C2 C1 C11 125.6(3) . . ?
C5 C1 C11 126.5(3) . . ?
C2 C1 Ca1 73.95(15) . . ?
C5 C1 Ca1 75.41(15) . . ?
C11 C1 Ca1 116.41(19) . . ?
C1 C2 C3 108.3(2) . . ?
C1 C2 C12 125.0(3) . . ?
C3 C2 C12 126.5(3) . . ?
C1 C2 Ca1 75.06(15) . . ?
C3 C2 Ca1 74.47(15) . . ?
C12 C2 Ca1 120.06(19) . . ?
C2 C3 C4 108.0(2) . . ?
C2 C3 C13 126.2(3) . . ?
C4 C3 C13 125.5(3) . . ?
C2 C3 Ca1 74.40(15) . . ?
C4 C3 Ca1 74.84(15) . . ?
C13 C3 Ca1 121.97(19) . . ?
C3 C4 C5 107.6(2) . . ?
C3 C4 C14 125.2(3) . . ?
C5 C4 C14 127.0(3) . . ?
C3 C4 Ca1 73.99(15) . . ?
C5 C4 Ca1 75.46(16) . . ?
C14 C4 Ca1 119.89(19) . . ?
C1 C5 C4 108.1(2) . . ?
C1 C5 C15 125.8(3) . . ?
C4 C5 C15 125.9(3) . . ?
C1 C5 Ca1 73.70(15) . . ?
C4 C5 Ca1 73.56(15) . . ?
C15 C5 Ca1 123.09(18) . . ?
C7 C6 C10 108.0(2) . . ?
C7 C6 C19 125.0(3) . . ?
C10 C6 C19 126.8(3) . . ?
C7 C6 Ca1 75.11(16) . . ?
C10 C6 Ca1 73.42(15) . . ?
C19 C6 Ca1 121.26(19) . . ?
C6 C7 C8 108.0(2) . . ?
C6 C7 C18 125.1(3) . . ?
C8 C7 C18 126.3(3) . . ?
C6 C7 Ca1 74.32(15) . . ?
C8 C7 Ca1 73.49(15) . . ?
C18 C7 Ca1 125.2(2) . . ?
C9 C8 C7 107.7(2) . . ?
C9 C8 C17 126.2(3) . . ?
C7 C8 C17 125.8(3) . . ?
C9 C8 Ca1 73.82(15) . . ?
C7 C8 Ca1 75.67(15) . . ?
C17 C8 Ca1 121.7(2) . . ?
C10 C9 C8 108.4(2) . . ?
C10 C9 C16 126.5(3) . . ?
C8 C9 C16 125.0(3) . . ?
C10 C9 Ca1 74.82(15) . . ?
C8 C9 Ca1 75.17(16) . . ?
C16 C9 Ca1 119.60(18) . . ?
C9 C10 C6 107.9(2) . . ?
C9 C10 C20 125.9(3) . . ?
C6 C10 C20 126.2(3) . . ?
C9 C10 Ca1 74.28(15) . . ?
C6 C10 Ca1 75.62(15) . . ?
C20 C10 Ca1 116.81(18) . . ?
C22 C21 C26 119.1(3) . . ?
C22 C21 C33 120.2(3) . . ?
C26 C21 C33 120.4(3) . . ?
C23 C22 C21 121.0(3) . . ?
C22 C23 C24 119.7(3) . . ?
C23 C24 C25 120.2(3) . . ?
C26 C25 C24 120.1(3) . . ?
C25 C26 C21 119.9(3) . . ?
C32 C27 C28 118.8(3) . . ?
C32 C27 C33 121.0(3) . . ?
C28 C27 C33 120.1(2) . . ?
C29 C28 C27 121.1(3) . . ?
C28 C29 C30 119.3(3) . . ?
C31 C30 C29 120.8(3) . . ?
C30 C31 C32 119.9(3) . . ?
C31 C32 C27 120.0(3) . . ?
O1 C33 C27 119.4(3) . . ?
O1 C33 C21 119.4(3) . . ?
C27 C33 C21 121.1(2) . . ?
C39 C34 C35 118.9(7) . . ?
C39 C34 C40 123.5(8) . . ?
C35 C34 C40 117.6(7) . . ?
C36 C35 C34 119.3(7) . . ?
C37 C36 C35 123.0(8) . . ?
C36 C37 C38 119.1(8) . . ?
C37 C38 C39 118.9(7) . . ?
C34 C39 C38 120.7(8) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.052
_database_code_depnum_ccdc_archive 'CCDC 1021901'
