# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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 
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data_complex7
_database_code_depnum_ccdc_archive 'CCDC 900478'
#TrackingRef 'complex7.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H82 Ca2 N8 O2 Si4'
_chemical_formula_sum            'C42 H82 Ca2 N8 O2 Si4'
_chemical_formula_weight         923.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   15.3218(2)
_cell_length_b                   15.5131(2)
_cell_length_c                   23.0555(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5480.03(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14938
_cell_measurement_theta_min      2.7961
_cell_measurement_theta_max      29.2401

_exptl_crystal_description       parallelpied
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2008
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8642
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29787
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         29.30
_reflns_number_total             6728
_reflns_number_gt                4956
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6728
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1353
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca Ca 0.13232(2) 0.13560(2) 0.446556(16) 0.01350(11) Uani 1 1 d . . .
Si1 Si 0.30908(4) 0.15891(4) 0.36116(2) 0.01865(14) Uani 1 1 d . . .
Si2 Si 0.17610(4) 0.03465(4) 0.31361(2) 0.01900(15) Uani 1 1 d . . .
O O 0.13577(9) 0.20820(10) 0.54016(6) 0.0196(3) Uani 1 1 d . . .
N1 N 0.11722(10) 0.00637(11) 0.49980(7) 0.0142(3) Uani 1 1 d . . .
N2 N -0.01627(10) 0.09790(10) 0.46088(7) 0.0142(3) Uani 1 1 d . . .
N3 N 0.03603(11) 0.25994(11) 0.41191(7) 0.0192(4) Uani 1 1 d . . .
N4 N 0.21423(11) 0.10463(11) 0.36369(7) 0.0176(3) Uani 1 1 d . . .
C1 C 0.19242(12) -0.00437(12) 0.53336(8) 0.0141(4) Uani 1 1 d . . .
C2 C 0.19321(13) -0.00929(13) 0.59402(9) 0.0174(4) Uani 1 1 d . . .
H2A H 0.1397 -0.0140 0.6146 0.021 Uiso 1 1 calc R . .
C3 C 0.27125(14) -0.00735(14) 0.62439(9) 0.0236(5) Uani 1 1 d . . .
H3A H 0.2704 -0.0108 0.6655 0.028 Uiso 1 1 calc R . .
C4 C 0.35059(14) -0.00050(15) 0.59574(10) 0.0262(5) Uani 1 1 d . . .
H4A H 0.4038 0.0006 0.6169 0.031 Uiso 1 1 calc R . .
C5 C 0.35097(13) 0.00466(14) 0.53574(10) 0.0239(5) Uani 1 1 d . . .
H5A H 0.4048 0.0099 0.5156 0.029 Uiso 1 1 calc R . .
C6 C 0.27343(12) 0.00226(13) 0.50487(9) 0.0184(4) Uani 1 1 d . . .
H6A H 0.2749 0.0051 0.4637 0.022 Uiso 1 1 calc R . .
C7 C -0.03836(12) 0.02625(12) 0.48762(8) 0.0123(4) Uani 1 1 d . . .
C8 C -0.08282(13) 0.16039(12) 0.44541(9) 0.0172(4) Uani 1 1 d . . .
H8A H -0.1320 0.1567 0.4731 0.021 Uiso 1 1 calc R . .
H8B H -0.1054 0.1477 0.4061 0.021 Uiso 1 1 calc R . .
C9 C -0.04383(13) 0.25098(13) 0.44673(9) 0.0187(4) Uani 1 1 d . . .
H9A H -0.0879 0.2923 0.4322 0.022 Uiso 1 1 calc R . .
H9B H -0.0305 0.2664 0.4874 0.022 Uiso 1 1 calc R . .
C10 C 0.01615(16) 0.24988(17) 0.34987(9) 0.0312(5) Uani 1 1 d . . .
H10A H -0.0207 0.2978 0.3370 0.047 Uiso 1 1 calc R . .
H10B H -0.0147 0.1953 0.3437 0.047 Uiso 1 1 calc R . .
H10C H 0.0706 0.2498 0.3276 0.047 Uiso 1 1 calc R . .
C11 C 0.07301(16) 0.34577(14) 0.42222(12) 0.0302(5) Uani 1 1 d . . .
H11A H 0.0325 0.3898 0.4079 0.045 Uiso 1 1 calc R . .
H11B H 0.1288 0.3510 0.4017 0.045 Uiso 1 1 calc R . .
H11C H 0.0825 0.3539 0.4639 0.045 Uiso 1 1 calc R . .
C12 C 0.2044(2) 0.2557(2) 0.56722(11) 0.0484(8) Uani 1 1 d . . .
H12A H 0.2001 0.3174 0.5564 0.058 Uiso 1 1 calc R . .
H12B H 0.2617 0.2338 0.5539 0.058 Uiso 1 1 calc R . .
C13 C 0.1974(3) 0.2466(3) 0.62868(13) 0.0910(17) Uani 1 1 d . . .
H13A H 0.1986 0.3041 0.6473 0.109 Uiso 1 1 calc R . .
H13B H 0.2472 0.2126 0.6437 0.109 Uiso 1 1 calc R . .
C14 C 0.11555(18) 0.2031(2) 0.64224(11) 0.0436(7) Uani 1 1 d . . .
H14A H 0.0782 0.2401 0.6669 0.052 Uiso 1 1 calc R . .
H14B H 0.1268 0.1483 0.6629 0.052 Uiso 1 1 calc R . .
C15 C 0.07257(15) 0.18647(16) 0.58497(9) 0.0279(5) Uani 1 1 d . . .
H15A H 0.0554 0.1251 0.5818 0.033 Uiso 1 1 calc R . .
H15B H 0.0196 0.2225 0.5809 0.033 Uiso 1 1 calc R . .
C16 C 0.30813(15) 0.24067(17) 0.42160(11) 0.0333(6) Uani 1 1 d . . .
H16A H 0.3599 0.2775 0.4186 0.050 Uiso 1 1 calc R . .
H16B H 0.3086 0.2108 0.4591 0.050 Uiso 1 1 calc R . .
H16C H 0.2554 0.2762 0.4186 0.050 Uiso 1 1 calc R . .
C17 C 0.41003(15) 0.09220(17) 0.37469(11) 0.0333(5) Uani 1 1 d . . .
H17A H 0.4548 0.1071 0.3460 0.050 Uiso 1 1 calc R . .
H17B H 0.3955 0.0309 0.3713 0.050 Uiso 1 1 calc R . .
H17C H 0.4322 0.1040 0.4138 0.050 Uiso 1 1 calc R . .
C18 C 0.33132(18) 0.21721(18) 0.29140(10) 0.0348(6) Uani 1 1 d . . .
H18A H 0.3923 0.2083 0.2801 0.052 Uiso 1 1 calc R . .
H18B H 0.3205 0.2790 0.2967 0.052 Uiso 1 1 calc R . .
H18C H 0.2928 0.1948 0.2610 0.052 Uiso 1 1 calc R . .
C19 C 0.08184(16) -0.02919(16) 0.34319(10) 0.0320(5) Uani 1 1 d . . .
H19A H 0.0664 -0.0750 0.3158 0.048 Uiso 1 1 calc R . .
H19B H 0.0316 0.0090 0.3488 0.048 Uiso 1 1 calc R . .
H19C H 0.0984 -0.0548 0.3805 0.048 Uiso 1 1 calc R . .
C20 C 0.25978(17) -0.04624(16) 0.28883(10) 0.0302(5) Uani 1 1 d . . .
H20A H 0.2508 -0.0590 0.2476 0.045 Uiso 1 1 calc R . .
H20B H 0.2537 -0.0993 0.3115 0.045 Uiso 1 1 calc R . .
H20C H 0.3184 -0.0224 0.2944 0.045 Uiso 1 1 calc R . .
C21 C 0.13365(15) 0.08878(16) 0.24577(9) 0.0281(5) Uani 1 1 d . . .
H21A H 0.1500 0.0545 0.2117 0.042 Uiso 1 1 calc R . .
H21B H 0.1590 0.1466 0.2425 0.042 Uiso 1 1 calc R . .
H21C H 0.0699 0.0933 0.2479 0.042 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ca 0.01263(18) 0.0138(2) 0.01402(19) 0.00093(14) 0.00120(14) -0.00118(14)
Si1 0.0167(3) 0.0210(3) 0.0183(3) 0.0030(2) 0.0024(2) 0.0004(2)
Si2 0.0210(3) 0.0219(3) 0.0141(3) 0.0000(2) 0.0015(2) 0.0000(2)
O 0.0183(7) 0.0229(8) 0.0176(7) -0.0039(6) 0.0016(6) -0.0061(6)
N1 0.0111(7) 0.0163(8) 0.0151(8) 0.0034(6) -0.0012(6) 0.0002(6)
N2 0.0125(7) 0.0124(7) 0.0179(8) 0.0005(6) -0.0005(6) 0.0001(6)
N3 0.0197(8) 0.0147(8) 0.0232(9) 0.0038(7) 0.0021(7) 0.0000(7)
N4 0.0170(8) 0.0214(9) 0.0144(8) 0.0020(6) 0.0015(6) 0.0021(7)
C1 0.0120(8) 0.0109(9) 0.0193(9) 0.0016(7) -0.0017(7) -0.0002(7)
C2 0.0162(9) 0.0169(10) 0.0190(10) 0.0005(8) 0.0004(8) -0.0012(8)
C3 0.0262(11) 0.0249(11) 0.0197(10) 0.0020(8) -0.0057(8) -0.0018(9)
C4 0.0182(10) 0.0299(12) 0.0306(12) 0.0021(9) -0.0087(9) -0.0022(9)
C5 0.0128(9) 0.0261(11) 0.0327(12) 0.0037(9) 0.0004(8) -0.0016(8)
C6 0.0157(9) 0.0205(10) 0.0189(9) 0.0018(8) 0.0023(8) 0.0001(8)
C7 0.0133(9) 0.0126(9) 0.0110(8) -0.0022(7) -0.0003(7) 0.0001(7)
C8 0.0147(9) 0.0144(9) 0.0226(10) 0.0030(8) -0.0003(8) 0.0013(7)
C9 0.0173(9) 0.0139(9) 0.0250(10) 0.0019(8) 0.0019(8) 0.0020(8)
C10 0.0336(12) 0.0363(13) 0.0237(11) 0.0077(10) 0.0029(10) 0.0057(11)
C11 0.0257(11) 0.0156(10) 0.0493(15) 0.0055(10) 0.0048(11) -0.0014(9)
C12 0.0486(16) 0.068(2) 0.0283(13) -0.0169(13) 0.0021(12) -0.0380(16)
C13 0.105(3) 0.138(4) 0.0307(16) 0.013(2) -0.0225(18) -0.093(3)
C14 0.0411(15) 0.068(2) 0.0215(12) -0.0093(12) 0.0029(11) -0.0138(14)
C15 0.0221(11) 0.0393(14) 0.0222(11) -0.0069(9) 0.0050(9) -0.0059(10)
C16 0.0236(11) 0.0416(15) 0.0347(13) -0.0116(11) -0.0021(10) -0.0013(11)
C17 0.0192(10) 0.0336(13) 0.0471(14) 0.0075(11) 0.0022(10) 0.0030(10)
C18 0.0402(14) 0.0350(14) 0.0292(12) 0.0125(10) 0.0062(11) -0.0069(11)
C19 0.0332(13) 0.0374(13) 0.0255(11) -0.0056(10) 0.0037(10) -0.0137(11)
C20 0.0373(13) 0.0269(12) 0.0262(11) 0.0000(9) -0.0009(10) 0.0094(10)
C21 0.0273(11) 0.0377(13) 0.0194(10) -0.0012(9) -0.0024(9) 0.0077(10)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca N4 2.3358(16) . ?
Ca N1 2.3620(16) . ?
Ca N2 2.3736(16) . ?
Ca O 2.4348(14) . ?
Ca N3 2.5565(17) . ?
Ca C1 3.0932(19) . ?
Ca C16 3.201(3) . ?
Ca C9 3.238(2) . ?
Ca Si1 3.3678(7) . ?
Ca Si2 3.5068(7) . ?
Si1 N4 1.6807(18) . ?
Si1 C18 1.876(2) . ?
Si1 C16 1.884(2) . ?
Si1 C17 1.887(2) . ?
Si2 N4 1.6890(18) . ?
Si2 C20 1.883(2) . ?
Si2 C19 1.879(2) . ?
Si2 C21 1.891(2) . ?
O C12 1.428(3) . ?
O C15 1.456(3) . ?
N1 C7 1.342(2) 5_556 ?
N1 C1 1.398(2) . ?
N2 C7 1.315(2) . ?
N2 C8 1.452(2) . ?
N3 C11 1.466(3) . ?
N3 C9 1.470(3) . ?
N3 C10 1.471(3) . ?
C1 C2 1.401(3) . ?
C1 C6 1.408(3) . ?
C2 C3 1.386(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.388(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.385(3) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 N1 1.342(2) 5_556 ?
C7 C7 1.540(4) 5_556 ?
C8 C9 1.527(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.428(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.458(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.498(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
N4 Ca N1 107.64(6) . . ?
N4 Ca N2 125.34(6) . . ?
N1 Ca N2 67.95(5) . . ?
N4 Ca O 143.94(6) . . ?
N1 Ca O 86.22(5) . . ?
N2 Ca O 90.66(5) . . ?
N4 Ca N3 102.10(6) . . ?
N1 Ca N3 138.27(5) . . ?
N2 Ca N3 71.09(5) . . ?
O Ca N3 86.59(5) . . ?
N4 Ca C1 103.00(6) . . ?
N1 Ca C1 25.46(5) . . ?
N2 Ca C1 91.29(5) . . ?
O Ca C1 75.21(5) . . ?
N3 Ca C1 154.64(5) . . ?
N4 Ca C16 60.37(6) . . ?
N1 Ca C16 127.45(6) . . ?
N2 Ca C16 163.28(6) . . ?
O Ca C16 84.57(5) . . ?
N3 Ca C16 92.59(6) . . ?
C1 Ca C16 102.90(6) . . ?
N4 Ca C9 124.22(6) . . ?
N1 Ca C9 112.76(5) . . ?
N2 Ca C9 48.45(5) . . ?
O Ca C9 76.19(5) . . ?
N3 Ca C9 26.16(5) . . ?
C1 Ca C9 129.44(5) . . ?
C16 Ca C9 114.84(6) . . ?
N4 Ca Si1 27.36(4) . . ?
N1 Ca Si1 118.28(4) . . ?
N2 Ca Si1 151.53(4) . . ?
O Ca Si1 116.81(4) . . ?
N3 Ca Si1 101.56(4) . . ?
C1 Ca Si1 102.37(4) . . ?
C16 Ca Si1 33.22(4) . . ?
C9 Ca Si1 127.70(4) . . ?
N4 Ca Si2 24.56(4) . . ?
N1 Ca Si2 95.39(4) . . ?
N2 Ca Si2 101.25(4) . . ?
O Ca Si2 167.72(4) . . ?
N3 Ca Si2 100.04(4) . . ?
C1 Ca Si2 101.25(4) . . ?
C16 Ca Si2 84.80(4) . . ?
C9 Ca Si2 114.04(4) . . ?
Si1 Ca Si2 51.913(15) . . ?
N4 Si1 C18 115.36(10) . . ?
N4 Si1 C16 107.75(10) . . ?
C18 Si1 C16 108.11(12) . . ?
N4 Si1 C17 115.35(10) . . ?
C18 Si1 C17 104.90(12) . . ?
C16 Si1 C17 104.67(11) . . ?
N4 Si1 Ca 39.69(6) . . ?
C18 Si1 Ca 134.34(9) . . ?
C16 Si1 Ca 68.51(8) . . ?
C17 Si1 Ca 120.24(8) . . ?
N4 Si2 C20 113.59(10) . . ?
N4 Si2 C19 110.88(9) . . ?
C20 Si2 C19 106.40(12) . . ?
N4 Si2 C21 113.51(10) . . ?
C20 Si2 C21 106.21(10) . . ?
C19 Si2 C21 105.66(11) . . ?
N4 Si2 Ca 35.08(6) . . ?
C20 Si2 Ca 133.88(7) . . ?
C19 Si2 Ca 76.77(7) . . ?
C21 Si2 Ca 117.32(8) . . ?
C12 O C15 107.42(16) . . ?
C12 O Ca 129.95(14) . . ?
C15 O Ca 120.50(12) . . ?
C7 N1 C1 125.28(16) 5_556 . ?
C7 N1 Ca 121.38(12) 5_556 . ?
C1 N1 Ca 107.95(12) . . ?
C7 N2 C8 119.92(16) . . ?
C7 N2 Ca 121.35(12) . . ?
C8 N2 Ca 118.36(12) . . ?
C11 N3 C9 108.60(17) . . ?
C11 N3 C10 109.52(18) . . ?
C9 N3 C10 110.41(17) . . ?
C11 N3 Ca 114.29(13) . . ?
C9 N3 Ca 103.79(11) . . ?
C10 N3 Ca 110.08(13) . . ?
Si1 N4 Si2 126.68(10) . . ?
Si1 N4 Ca 112.95(8) . . ?
Si2 N4 Ca 120.36(9) . . ?
N1 C1 C2 124.50(17) . . ?
N1 C1 C6 117.36(17) . . ?
C2 C1 C6 117.53(17) . . ?
N1 C1 Ca 46.59(9) . . ?
C2 C1 Ca 133.38(13) . . ?
C6 C1 Ca 84.80(12) . . ?
C3 C2 C1 120.71(19) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 121.1(2) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C5 C4 C3 118.89(19) . . ?
C5 C4 H4A 120.6 . . ?
C3 C4 H4A 120.6 . . ?
C6 C5 C4 120.52(19) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C5 C6 C1 121.21(19) . . ?
C5 C6 H6A 119.4 . . ?
C1 C6 H6A 119.4 . . ?
N2 C7 N1 130.68(17) . 5_556 ?
N2 C7 C7 115.1(2) . 5_556 ?
N1 C7 C7 114.1(2) 5_556 5_556 ?
N2 C8 C9 109.57(16) . . ?
N2 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N2 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N3 C9 C8 113.69(16) . . ?
N3 C9 Ca 50.05(9) . . ?
C8 C9 Ca 79.48(11) . . ?
N3 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
Ca C9 H9A 157.9 . . ?
N3 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
Ca C9 H9B 87.9 . . ?
H9A C9 H9B 107.7 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O C12 C13 109.1(2) . . ?
O C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
O C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 C14 108.9(2) . . ?
C12 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
C12 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C13 C14 C15 105.6(2) . . ?
C13 C14 H14A 110.6 . . ?
C15 C14 H14A 110.6 . . ?
C13 C14 H14B 110.6 . . ?
C15 C14 H14B 110.6 . . ?
H14A C14 H14B 108.8 . . ?
O C15 C14 107.06(18) . . ?
O C15 H15A 110.3 . . ?
C14 C15 H15A 110.3 . . ?
O C15 H15B 110.3 . . ?
C14 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
Si1 C16 Ca 78.27(8) . . ?
Si1 C16 H16A 109.5 . . ?
Ca C16 H16A 172.3 . . ?
Si1 C16 H16B 109.5 . . ?
Ca C16 H16B 66.8 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
Ca C16 H16C 66.8 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.897
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.076