#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:23:24 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178605 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/16/4071662.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4071662
loop_
_publ_author_name
'Barrett, Anthony G. M.'
'Crimmin, Mark R.'
'Hill, Michael S.'
'Kociok-Köhn, Gabriele'
'MacDougall, Dugald J.'
'Mahon, Mary F.'
'Procopiou, Panayiotis A.'
_publ_section_title
;
 Synthesis, Characterization, and Solution Lability of N-Heterocyclic
 Carbene Adducts of the Heavier Group 2 Bis(trimethylsilyl)amides
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3939
_journal_paper_doi               10.1021/om800299j
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         '2(C39 H72 Ca N4 Si4), C7 H8'
_chemical_formula_sum            'C85 H152 Ca2 N8 Si8'
_chemical_formula_weight         1591.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.1990(10)
_cell_angle_beta                 90.1600(10)
_cell_angle_gamma                103.6750(10)
_cell_formula_units_Z            1
_cell_length_a                   11.5618(2)
_cell_length_b                   12.2760(2)
_cell_length_c                   18.7309(3)
_cell_measurement_reflns_used    33735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2499.03(7)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). 
 Sheldrick, G.M., Institüt für Anorganische Chemie der Universität, 
 Tammanstrasse 4, D-3400 Göttingen, Germany, 1998 
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '309 1.8 degree images with φ and \v scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43885
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         11151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0623P)²+0.3185P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                7911
_reflns_number_total             11151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800299j-file004.cif
_cod_data_source_block           h08msh4
_cod_database_code               4071662
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ca Ca 0.07869(3) 0.19506(3) 0.749899(19) 0.02576(10) Uani 1 1 d .
Si1 Si -0.09278(5) -0.05866(4) 0.69150(3) 0.03520(13) Uani 1 1 d .
Si2 Si -0.12324(4) 0.03043(4) 0.85315(3) 0.03464(13) Uani 1 1 d .
Si3 Si -0.03237(4) 0.41487(4) 0.76595(3) 0.02901(12) Uani 1 1 d .
Si4 Si 0.02724(5) 0.33684(4) 0.60908(3) 0.03414(13) Uani 1 1 d .
N1 N 0.37958(12) 0.33988(11) 0.83926(7) 0.0228(3) Uani 1 1 d .
N2 N 0.37596(12) 0.16745(11) 0.78035(7) 0.0234(3) Uani 1 1 d .
N3 N -0.05538(12) 0.03836(12) 0.77425(8) 0.0300(3) Uani 1 1 d .
N4 N 0.02701(12) 0.32990(12) 0.69851(8) 0.0279(3) Uani 1 1 d .
C1 C 0.30358(14) 0.24224(13) 0.79736(8) 0.0213(3) Uani 1 1 d .
C2 C 0.49376(15) 0.32600(15) 0.84688(10) 0.0297(4) Uani 1 1 d .
H2 H 0.5608 0.3827 0.8731 0.036 Uiso 1 1 calc R
C3 C 0.49156(15) 0.21710(14) 0.81006(10) 0.0295(4) Uani 1 1 d .
H3 H 0.5564 0.1812 0.8053 0.035 Uiso 1 1 calc R
C4 C 0.35193(14) 0.44972(13) 0.87175(9) 0.0238(3) Uani 1 1 d .
C5 C 0.38605(15) 0.53790(14) 0.83504(10) 0.0282(4) Uani 1 1 d .
C6 C 0.44004(17) 0.51901(16) 0.76045(10) 0.0357(4) Uani 1 1 d .
H6 H 0.4487 0.4375 0.7460 0.043 Uiso 1 1 calc R
C7 C 0.3575(2) 0.5340(2) 0.70184(12) 0.0562(6) Uani 1 1 d .
H7A H 0.3935 0.5212 0.6541 0.084 Uiso 1 1 calc R
H7B H 0.3455 0.6127 0.7157 0.084 Uiso 1 1 calc R
H7C H 0.2805 0.4777 0.6980 0.084 Uiso 1 1 calc R
C8 C 0.5634(2) 0.5997(2) 0.76328(13) 0.0586(6) Uani 1 1 d .
H8A H 0.5953 0.5845 0.7144 0.088 Uiso 1 1 calc R
H8B H 0.6168 0.5860 0.7991 0.088 Uiso 1 1 calc R
H8C H 0.5575 0.6804 0.7782 0.088 Uiso 1 1 calc R
C9 C 0.36761(17) 0.64584(15) 0.86992(11) 0.0360(4) Uani 1 1 d .
H9 H 0.3898 0.7079 0.8468 0.043 Uiso 1 1 calc R
C10 C 0.31795(18) 0.66447(15) 0.93709(11) 0.0383(5) Uani 1 1 d .
H10 H 0.3072 0.7392 0.9601 0.046 Uiso 1 1 calc R
C11 C 0.28361(16) 0.57561(15) 0.97137(10) 0.0324(4) Uani 1 1 d .
H11 H 0.2480 0.5897 1.0173 0.039 Uiso 1 1 calc R
C12 C 0.30016(15) 0.46533(14) 0.93978(9) 0.0264(4) Uani 1 1 d .
C13 C 0.26393(15) 0.36669(14) 0.97779(9) 0.0290(4) Uani 1 1 d .
H13 H 0.2257 0.2950 0.9389 0.035 Uiso 1 1 calc R
C14 C 0.17306(18) 0.38646(18) 1.03568(11) 0.0409(5) Uani 1 1 d .
H14A H 0.1534 0.3205 1.0580 0.061 Uiso 1 1 calc R
H14B H 0.1005 0.3940 1.0121 0.061 Uiso 1 1 calc R
H14C H 0.2070 0.4575 1.0740 0.061 Uiso 1 1 calc R
C15 C 0.37201(18) 0.34313(17) 1.01328(11) 0.0404(5) Uani 1 1 d .
H15A H 0.3452 0.2792 1.0368 0.061 Uiso 1 1 calc R
H15B H 0.4134 0.4129 1.0505 0.061 Uiso 1 1 calc R
H15C H 0.4266 0.3222 0.9753 0.061 Uiso 1 1 calc R
C16 C 0.33932(14) 0.04840(13) 0.73723(9) 0.0261(4) Uani 1 1 d .
C17 C 0.29612(16) -0.03703(14) 0.77522(11) 0.0326(4) Uani 1 1 d .
C18 C 0.28214(18) -0.00740(16) 0.85745(11) 0.0381(4) Uani 1 1 d .
H18 H 0.2684 0.0723 0.8718 0.046 Uiso 1 1 calc R
C19 C 0.3953(2) -0.0052(2) 0.90106(13) 0.0517(6) Uani 1 1 d .
H19A H 0.4635 0.0483 0.8873 0.078 Uiso 1 1 calc R
H19B H 0.4091 -0.0832 0.8898 0.078 Uiso 1 1 calc R
H19C H 0.3855 0.0208 0.9540 0.078 Uiso 1 1 calc R
C20 C 0.1751(2) -0.0892(2) 0.87917(14) 0.0562(6) Uani 1 1 d .
H20A H 0.1695 -0.0665 0.9327 0.084 Uiso 1 1 calc R
H20B H 0.1848 -0.1687 0.8644 0.084 Uiso 1 1 calc R
H20C H 0.1021 -0.0850 0.8543 0.084 Uiso 1 1 calc R
C21 C 0.26870(19) -0.15164(16) 0.73284(13) 0.0464(5) Uani 1 1 d .
H21 H 0.2395 -0.2125 0.7561 0.056 Uiso 1 1 calc R
C22 C 0.2830(2) -0.17855(17) 0.65817(13) 0.0515(6) Uani 1 1 d .
H22 H 0.2637 -0.2573 0.6306 0.062 Uiso 1 1 calc R
C23 C 0.32512(19) -0.09233(16) 0.62320(12) 0.0438(5) Uani 1 1 d .
H23 H 0.3344 -0.1124 0.5716 0.053 Uiso 1 1 calc R
C24 C 0.35449(16) 0.02410(15) 0.66186(10) 0.0316(4) Uani 1 1 d .
C25 C 0.40209(19) 0.11903(17) 0.62289(10) 0.0405(5) Uani 1 1 d .
H25 H 0.3782 0.1904 0.6502 0.049 Uiso 1 1 calc R
C26 C 0.5383(2) 0.1475(3) 0.62445(14) 0.0679(7) Uani 1 1 d .
H26A H 0.5669 0.2091 0.5992 0.102 Uiso 1 1 calc R
H26B H 0.5642 0.0781 0.5993 0.102 Uiso 1 1 calc R
H26C H 0.5712 0.1737 0.6758 0.102 Uiso 1 1 calc R
C27 C 0.3515(2) 0.0881(2) 0.54267(11) 0.0521(6) Uani 1 1 d .
H27A H 0.3846 0.1522 0.5203 0.078 Uiso 1 1 calc R
H27B H 0.2644 0.0745 0.5416 0.078 Uiso 1 1 calc R
H27C H 0.3732 0.0179 0.5148 0.078 Uiso 1 1 calc R
C28 C -0.0743(2) -0.20803(17) 0.68579(14) 0.0579(6) Uani 1 1 d .
H28A H 0.0076 -0.2033 0.7025 0.087 Uiso 1 1 calc R
H28B H -0.0904 -0.2545 0.6346 0.087 Uiso 1 1 calc R
H28C H -0.1303 -0.2444 0.7172 0.087 Uiso 1 1 calc R
C29 C 0.0102(2) -0.0027(2) 0.62380(13) 0.0488(5) Uani 1 1 d .
H29A H 0.092(3) 0.009(3) 0.6398(17) 0.093(10) Uiso 1 1 d .
H29B H -0.004(2) 0.064(2) 0.6147(14) 0.063(7) Uiso 1 1 d .
H29C H -0.004(2) -0.059(2) 0.5749(16) 0.080(8) Uiso 1 1 d .
C30 C -0.2478(2) -0.0760(2) 0.65351(14) 0.0605(6) Uani 1 1 d .
H30A H -0.3054 -0.1140 0.6835 0.091 Uiso 1 1 calc R
H30B H -0.2582 -0.1234 0.6025 0.091 Uiso 1 1 calc R
H30C H -0.2609 0.0004 0.6547 0.091 Uiso 1 1 calc R
C31 C -0.1751(2) -0.11976(19) 0.86753(14) 0.0563(6) Uani 1 1 d .
H31A H -0.2355 -0.1673 0.8284 0.085 Uiso 1 1 calc R
H31B H -0.2097 -0.1151 0.9156 0.085 Uiso 1 1 calc R
H31C H -0.1071 -0.1550 0.8662 0.085 Uiso 1 1 calc R
C32 C -0.01996(19) 0.11892(18) 0.93530(11) 0.0440(5) Uani 1 1 d .
H32A H 0.0523 0.0901 0.9347 0.066 Uiso 1 1 calc R
H32B H -0.0600 0.1125 0.9807 0.066 Uiso 1 1 calc R
H32C H 0.0017 0.2003 0.9334 0.066 Uiso 1 1 calc R
C33 C -0.26139(19) 0.0878(2) 0.86021(15) 0.0604(6) Uani 1 1 d .
H33A H -0.2408 0.1680 0.8560 0.091 Uiso 1 1 calc R
H33B H -0.2948 0.0852 0.9080 0.091 Uiso 1 1 calc R
H33C H -0.3204 0.0400 0.8204 0.091 Uiso 1 1 calc R
C34 C -0.0117(2) 0.36958(19) 0.85364(11) 0.0380(4) Uani 1 1 d .
H34A H 0.076(2) 0.3822(19) 0.8689(12) 0.056(6) Uiso 1 1 d .
H34B H -0.034(2) 0.421(2) 0.8980(13) 0.055(6) Uiso 1 1 d .
H34C H -0.055(2) 0.289(2) 0.8498(14) 0.071(8) Uiso 1 1 d .
C35 C 0.0400(2) 0.57417(16) 0.78984(12) 0.0463(5) Uani 1 1 d .
H35A H 0.1259 0.5865 0.8001 0.069 Uiso 1 1 calc R
H35B H 0.0055 0.6132 0.8336 0.069 Uiso 1 1 calc R
H35C H 0.0264 0.6060 0.7483 0.069 Uiso 1 1 calc R
C36 C -0.19675(19) 0.3982(2) 0.75040(13) 0.0564(6) Uani 1 1 d .
H36A H -0.2120 0.4208 0.7052 0.085 Uiso 1 1 calc R
H36B H -0.2251 0.4479 0.7925 0.085 Uiso 1 1 calc R
H36C H -0.2390 0.3172 0.7454 0.085 Uiso 1 1 calc R
C37 C 0.0523(2) 0.48756(19) 0.59668(13) 0.0553(6) Uani 1 1 d .
H37A H -0.0166 0.5187 0.6127 0.083 Uiso 1 1 calc R
H37B H 0.0625 0.4857 0.5445 0.083 Uiso 1 1 calc R
H37C H 0.1242 0.5370 0.6263 0.083 Uiso 1 1 calc R
C38 C -0.1158(2) 0.2513(2) 0.55413(12) 0.0556(6) Uani 1 1 d .
H38A H -0.1297 0.1699 0.5553 0.083 Uiso 1 1 calc R
H38B H -0.1101 0.2570 0.5029 0.083 Uiso 1 1 calc R
H38C H -0.1822 0.2824 0.5755 0.083 Uiso 1 1 calc R
C39 C 0.1488(2) 0.2757(2) 0.56129(12) 0.0499(5) Uani 1 1 d .
H39A H 0.2260 0.3182 0.5875 0.075 Uiso 1 1 calc R
H39B H 0.1495 0.2832 0.5104 0.075 Uiso 1 1 calc R
H39C H 0.1346 0.1936 0.5610 0.075 Uiso 1 1 calc R
C40 C 0.4379(6) 0.5108(5) 0.4856(3) 0.0633(14) Uani 0.50 1 d P
C41 C 0.5532(5) 0.5920(3) 0.5360(2) 0.0936(12) Uani 1 1 d .
H41 H 0.5624 0.6719 0.5588 0.112 Uiso 1 1 calc R
C42 C 0.6384(10) 0.5307(19) 0.5420(8) 0.153(8) Uani 0.50 1 d P
H42 H 0.6702 0.6109 0.5640 0.183 Uiso 0.50 1 calc PR
C43 C 0.6212(11) 0.4062(9) 0.5047(6) 0.087(3) Uani 0.50 1 d P
H43 H 0.6815 0.3665 0.5082 0.105 Uiso 0.50 1 calc PR
C44 C 0.5271(9) 0.3570(8) 0.4696(5) 0.099(2) Uani 0.50 1 d P
H44 H 0.5137 0.2770 0.4455 0.119 Uiso 0.50 1 calc PR
C45 C 0.3303(14) 0.5329(16) 0.4601(8) 0.116(5) Uani 0.50 1 d P
H45A H 0.3342 0.6160 0.4766 0.175 Uiso 0.50 1 calc PR
H45B H 0.2615 0.4894 0.4802 0.175 Uiso 0.50 1 calc PR
H45C H 0.3219 0.5085 0.4060 0.175 Uiso 0.50 1 calc PR
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'
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'
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
N4 Ca N3 124.52(5) . .
N4 Ca C1 115.55(5) . .
N3 Ca C1 119.49(5) . .
N4 Ca C29 98.02(7) . .
N3 Ca C29 66.00(6) . .
C1 Ca C29 113.89(7) . .
N4 Ca C34 65.91(5) . .
N3 Ca C34 95.27(6) . .
C1 Ca C34 102.65(6) . .
C29 Ca C34 143.43(7) . .
N4 Ca Si1 113.11(4) . .
N3 Ca Si1 30.68(4) . .
C1 Ca Si1 125.64(4) . .
C29 Ca Si1 35.58(5) . .
C34 Ca Si1 118.37(5) . .
N4 Ca Si3 30.44(4) . .
N3 Ca Si3 112.36(4) . .
C1 Ca Si3 115.47(4) . .
C29 Ca Si3 120.78(6) . .
C34 Ca Si3 35.60(4) . .
Si1 Ca Si3 118.688(16) . .
N4 Ca Si2 122.54(4) . .
N3 Ca Si2 21.66(4) . .
C1 Ca Si2 113.66(3) . .
C29 Ca Si2 87.59(5) . .
C34 Ca Si2 76.13(4) . .
Si1 Ca Si2 52.092(14) . .
Si3 Ca Si2 100.585(15) . .
N4 Ca Si4 21.36(4) . .
N3 Ca Si4 124.34(4) . .
C1 Ca Si4 113.94(3) . .
C29 Ca Si4 79.60(5) . .
C34 Ca Si4 87.24(4) . .
Si1 Ca Si4 102.707(15) . .
Si3 Ca Si4 51.671(13) . .
Si2 Ca Si4 131.893(15) . .
N4 Ca H29A 108.4(6) . .
N3 Ca H29A 74.1(7) . .
C1 Ca H29A 94.5(7) . .
C29 Ca H29A 19.4(7) . .
C34 Ca H29A 162.7(7) . .
Si1 Ca H29A 47.1(7) . .
Si3 Ca H29A 135.9(7) . .
Si2 Ca H29A 95.2(6) . .
Si4 Ca H29A 87.7(6) . .
N4 Ca H29B 79.2(6) . .
N3 Ca H29B 77.2(6) . .
C1 Ca H29B 122.9(5) . .
C29 Ca H29B 18.8(6) . .
C34 Ca H29B 131.5(6) . .
Si1 Ca H29B 47.1(6) . .
Si3 Ca H29B 103.1(6) . .
Si2 Ca H29B 97.5(6) . .
Si4 Ca H29B 61.2(6) . .
H29A Ca H29B 33.6(8) . .
N4 Ca H34A 75.0(5) . .
N3 Ca H34A 105.5(5) . .
C1 Ca H34A 82.3(5) . .
C29 Ca H34A 163.7(5) . .
C34 Ca H34A 20.3(5) . .
Si1 Ca H34A 133.5(5) . .
Si3 Ca H34A 47.8(5) . .
Si2 Ca H34A 84.1(5) . .
Si4 Ca H34A 95.6(5) . .
H29A Ca H34A 176.2(8) . .
H29B Ca H34A 150.2(8) . .
N4 Ca H34C 77.6(5) . .
N3 Ca H34C 75.6(6) . .
C1 Ca H34C 112.9(6) . .
C29 Ca H34C 129.6(6) . .
C34 Ca H34C 19.7(6) . .
Si1 Ca H34C 99.6(6) . .
Si3 Ca H34C 48.0(6) . .
Si2 Ca H34C 57.0(6) . .
Si4 Ca H34C 97.7(5) . .
H29A Ca H34C 146.4(9) . .
H29B Ca H34C 124.1(8) . .
H34A Ca H34C 35.1(7) . .
N3 Si1 C30 114.42(10) . .
N3 Si1 C28 116.30(9) . .
C30 Si1 C28 106.73(11) . .
N3 Si1 C29 107.04(9) . .
C30 Si1 C29 106.10(12) . .
C28 Si1 C29 105.43(12) . .
N3 Si1 Ca 44.22(5) . .
C30 Si1 Ca 119.69(8) . .
C28 Si1 Ca 133.57(8) . .
C29 Si1 Ca 63.34(8) . .
N3 Si2 C32 110.32(8) . .
N3 Si2 C33 112.71(10) . .
C32 Si2 C33 106.78(11) . .
N3 Si2 C31 115.51(10) . .
C32 Si2 C31 106.48(10) . .
C33 Si2 C31 104.44(11) . .
N3 Si2 Ca 30.34(5) . .
C32 Si2 Ca 85.03(6) . .
C33 Si2 Ca 106.49(8) . .
C31 Si2 Ca 142.04(8) . .
N4 Si3 C35 116.62(9) . .
N4 Si3 C36 114.27(9) . .
C35 Si3 C36 107.11(11) . .
N4 Si3 C34 107.04(9) . .
C35 Si3 C34 104.43(10) . .
C36 Si3 C34 106.48(11) . .
N4 Si3 Ca 43.53(5) . .
C35 Si3 Ca 131.19(7) . .
C36 Si3 Ca 121.70(8) . .
C34 Si3 Ca 63.78(7) . .
N4 Si4 C39 110.75(9) . .
N4 Si4 C37 114.22(9) . .
C39 Si4 C37 106.03(11) . .
N4 Si4 C38 112.98(9) . .
C39 Si4 C38 106.14(11) . .
C37 Si4 C38 106.15(11) . .
N4 Si4 Ca 29.50(5) . .
C39 Si4 Ca 85.26(7) . .
C37 Si4 Ca 138.75(7) . .
C38 Si4 Ca 108.43(8) . .
C1 N1 C2 112.34(13) . .
C1 N1 C4 126.86(13) . .
C2 N1 C4 120.77(13) . .
C1 N2 C3 112.54(13) . .
C1 N2 C16 125.48(13) . .
C3 N2 C16 121.98(13) . .
Si2 N3 Si1 125.91(8) . .
Si2 N3 Ca 128.00(8) . .
Si1 N3 Ca 105.10(7) . .
Si3 N4 Si4 124.32(8) . .
Si3 N4 Ca 106.03(7) . .
Si4 N4 Ca 129.14(8) . .
N1 C1 N2 102.15(13) . .
N1 C1 Ca 132.85(11) . .
N2 C1 Ca 124.94(10) . .
C3 C2 N1 106.72(14) . .
C3 C2 H2 126.6 . .
N1 C2 H2 126.6 . .
C2 C3 N2 106.25(14) . .
C2 C3 H3 126.9 . .
N2 C3 H3 126.9 . .
C12 C4 C5 123.35(15) . .
C12 C4 N1 119.05(14) . .
C5 C4 N1 117.47(15) . .
C9 C5 C4 116.84(16) . .
C9 C5 C6 120.41(16) . .
C4 C5 C6 122.75(15) . .
C5 C6 C8 111.96(16) . .
C5 C6 C7 110.59(17) . .
C8 C6 C7 110.32(17) . .
C5 C6 H6 107.9 . .
C8 C6 H6 107.9 . .
C7 C6 H6 107.9 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C9 C5 121.33(17) . .
C10 C9 H9 119.3 . .
C5 C9 H9 119.3 . .
C9 C10 C11 120.54(17) . .
C9 C10 H10 119.7 . .
C11 C10 H10 119.7 . .
C10 C11 C12 121.19(17) . .
C10 C11 H11 119.4 . .
C12 C11 H11 119.4 . .
C11 C12 C4 116.74(16) . .
C11 C12 C13 121.62(16) . .
C4 C12 C13 121.64(15) . .
C12 C13 C14 113.32(15) . .
C12 C13 C15 111.97(14) . .
C14 C13 C15 109.20(16) . .
C12 C13 H13 107.4 . .
C14 C13 H13 107.4 . .
C15 C13 H13 107.4 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C24 C16 C17 123.71(16) . .
C24 C16 N2 118.70(15) . .
C17 C16 N2 117.50(15) . .
C21 C17 C16 116.15(18) . .
C21 C17 C18 121.61(17) . .
C16 C17 C18 122.23(15) . .
C17 C18 C20 112.41(18) . .
C17 C18 C19 111.73(17) . .
C20 C18 C19 109.94(17) . .
C17 C18 H18 107.5 . .
C20 C18 H18 107.5 . .
C19 C18 H18 107.5 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C18 C20 H20A 109.5 . .
C18 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C18 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C22 C21 C17 121.54(19) . .
C22 C21 H21 119.2 . .
C17 C21 H21 119.2 . .
C23 C22 C21 120.41(18) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C24 121.34(19) . .
C22 C23 H23 119.3 . .
C24 C23 H23 119.3 . .
C16 C24 C23 116.86(17) . .
C16 C24 C25 122.10(16) . .
C23 C24 C25 121.04(17) . .
C24 C25 C26 110.96(18) . .
C24 C25 C27 112.87(17) . .
C26 C25 C27 109.16(18) . .
C24 C25 H25 107.9 . .
C26 C25 H25 107.9 . .
C27 C25 H25 107.9 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
Si1 C28 H28A 109.5 . .
Si1 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
Si1 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
Si1 C29 Ca 81.08(8) . .
Si1 C29 H29A 111.2(18) . .
Ca C29 H29A 69.3(18) . .
Si1 C29 H29B 112.2(16) . .
Ca C29 H29B 67.4(15) . .
H29A C29 H29B 111(2) . .
Si1 C29 H29C 110.6(16) . .
Ca C29 H29C 167.9(15) . .
H29A C29 H29C 108(2) . .
H29B C29 H29C 104(2) . .
Si1 C30 H30A 109.5 . .
Si1 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
Si1 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
Si2 C31 H31A 109.5 . .
Si2 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
Si2 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
Si2 C32 H32A 109.5 . .
Si2 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
Si2 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
Si2 C33 H33A 109.5 . .
Si2 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
Si2 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
Si3 C34 Ca 80.62(7) . .
Si3 C34 H34A 112.1(13) . .
Ca C34 H34A 72.9(13) . .
Si3 C34 H34B 113.1(13) . .
Ca C34 H34B 166.0(13) . .
H34A C34 H34B 98.4(18) . .
Si3 C34 H34C 111.9(15) . .
Ca C34 H34C 65.0(15) . .
H34A C34 H34C 110.8(19) . .
H34B C34 H34C 109.7(19) . .
Si3 C35 H35A 109.5 . .
Si3 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
Si3 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
Si3 C36 H36A 109.5 . .
Si3 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
Si3 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
Si4 C37 H37A 109.5 . .
Si4 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
Si4 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
Si4 C38 H38A 109.5 . .
Si4 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
Si4 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
Si4 C39 H39A 109.5 . .
Si4 C39 H39B 109.5 . .
H39A C39 H39B 109.5 . .
Si4 C39 H39C 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
C42 C40 C41 75.9(13) 2_666 2_666
C42 C40 C43 78.0(13) 2_666 2_666
C41 C40 C43 153.7(10) 2_666 2_666
C41 C40 C45 115.5(10) 2_666 .
C42 C40 C44 126.1(14) 2_666 2_666
C41 C40 C44 157.6(8) 2_666 2_666
C43 C40 C44 48.2(5) 2_666 2_666
C45 C40 C44 86.9(8) . 2_666
C42 C40 C41 172.1(14) 2_666 .
C41 C40 C41 111.5(5) 2_666 .
C43 C40 C41 94.4(7) 2_666 .
C45 C40 C41 133.1(9) . .
C44 C40 C41 46.3(4) 2_666 .
C42 C40 C40 141.6(15) 2_666 2_666
C41 C40 C40 65.8(5) 2_666 2_666
C43 C40 C40 139.9(10) 2_666 2_666
C45 C40 C40 178.5(10) . 2_666
C44 C40 C40 91.9(8) 2_666 2_666
C41 C40 C40 45.7(4) . 2_666
C42 C41 C40 111.5(9) . .
C42 C41 H41 124.2 . .
C40 C41 H41 124.2 . .
C45 C42 C40 98(3) 2_666 2_666
C45 C42 C41 158(2) 2_666 .
C40 C42 C41 61.0(8) 2_666 .
C40 C42 C43 61.7(12) 2_666 .
C41 C42 C43 122.6(11) . .
C45 C42 H42 131.1 2_666 .
C40 C42 H42 131.1 2_666 .
C41 C42 H42 70.2 . .
C43 C42 H42 165.3 . .
C44 C43 C42 117.3(10) . .
C44 C43 H43 121.4 . .
C42 C43 H43 121.4 . .
C43 C44 C41 122.3(9) . 2_666
C43 C44 C40 54.9(7) . 2_666
C41 C44 C40 67.4(5) 2_666 2_666
C43 C44 H44 118.8 . .
C41 C44 H44 118.8 2_666 .
C40 C44 H44 173.6 2_666 .
C40 C45 H45A 109.5 . .
C40 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C40 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca N4 2.2955(14) .
Ca N3 2.3099(14) .
Ca C1 2.6285(16) .
Ca C29 2.893(2) .
Ca C34 2.913(2) .
Ca Si1 3.1976(6) .
Ca Si3 3.2035(6) .
Ca Si2 3.6038(6) .
Ca Si4 3.6157(6) .
Ca H29A 2.71(3) .
Ca H29B 2.68(2) .
Ca H34A 2.79(2) .
Ca H34C 2.65(3) .
Si1 N3 1.6897(16) .
Si1 C30 1.871(2) .
Si1 C28 1.873(2) .
Si1 C29 1.883(2) .
Si2 N3 1.6883(16) .
Si2 C32 1.879(2) .
Si2 C33 1.885(2) .
Si2 C31 1.885(2) .
Si3 N4 1.6888(15) .
Si3 C35 1.876(2) .
Si3 C36 1.877(2) .
Si3 C34 1.890(2) .
Si4 N4 1.6980(15) .
Si4 C39 1.876(2) .
Si4 C37 1.876(2) .
Si4 C38 1.881(2) .
N1 C1 1.364(2) .
N1 C2 1.382(2) .
N1 C4 1.447(2) .
N2 C1 1.366(2) .
N2 C3 1.383(2) .
N2 C16 1.447(2) .
C2 C3 1.340(2) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 C12 1.399(2) .
C4 C5 1.402(2) .
C5 C9 1.392(2) .
C5 C6 1.520(3) .
C6 C8 1.525(3) .
C6 C7 1.525(3) .
C6 H6 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.375(3) .
C9 H9 0.9500 .
C10 C11 1.378(3) .
C10 H10 0.9500 .
C11 C12 1.396(2) .
C11 H11 0.9500 .
C12 C13 1.528(2) .
C13 C14 1.529(3) .
C13 C15 1.532(3) .
C13 H13 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C24 1.390(3) .
C16 C17 1.406(2) .
C17 C21 1.396(3) .
C17 C18 1.512(3) .
C18 C20 1.523(3) .
C18 C19 1.531(3) .
C18 H18 1.0000 .
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 C22 1.376(3) .
C21 H21 0.9500 .
C22 C23 1.373(3) .
C22 H22 0.9500 .
C23 C24 1.394(3) .
C23 H23 0.9500 .
C24 C25 1.520(3) .
C25 C26 1.529(3) .
C25 C27 1.534(3) .
C25 H25 1.0000 .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.96(3) .
C29 H29B 0.93(3) .
C29 H29C 0.99(3) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 1.01(2) .
C34 H34B 0.99(3) .
C34 H34C 0.99(3) .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C40 C42 0.980(13) 2_666
C40 C41 1.256(7) 2_666
C40 C43 1.333(12) 2_666
C40 C45 1.439(15) .
C40 C44 1.587(12) 2_666
C40 C41 1.601(9) .
C40 C40 1.633(14) 2_666
C41 C42 1.393(16) .
C41 H41 0.9500 .
C42 C45 0.93(2) 2_666
C42 C40 0.980(13) 2_666
C42 C43 1.48(2) .
C42 H42 0.9500 .
C43 C44 1.214(12) .
C43 H43 0.9500 .
C44 C41 1.253(9) 2_666
C44 C40 1.587(12) 2_666
C44 H44 0.9500 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
