#------------------------------------------------------------------------------
#$Date: 2026-03-04 12:13:40 +0100 (Wed 04 de Mar de 2026) $
#$Revision: 304746 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/04/7720443.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_7720443
loop_
_publ_author_name
'de Vere-Tucker, Matthew'
'Slawin, Alexandra M. Z.'
'Cordes, David B.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis of heteroleptic calcium amide complexes via manipulation
 of the Schlenk equilibrium.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1708
_journal_page_last               1715
_journal_paper_doi               10.1039/d5dt02949j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C39 H67 Ca N3 Si2'
_chemical_formula_sum            'C39 H67 Ca N3 Si2'
_chemical_formula_weight         674.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-06-04
_audit_creation_method           'by CrystalStructure 4.3'
_audit_update_record
;
2025-12-08 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.1100(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.9210(9)
_cell_length_b                   29.295(2)
_cell_length_c                   13.3529(9)
_cell_measurement_reflns_used    11080
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.90
_cell_volume                     4289.0(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2019/3 (Sheldrick, 2015B)'
_computing_structure_solution    'SHELXT Version 2014/4 (Sheldrick, 2015A)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            127279
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.373
_diffrn_reflns_theta_min         1.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0609P)²+1.8591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7064
_reflns_number_total             7851
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d5dt02949j2.cif
_cod_data_source_block           5
_cod_database_code               7720443
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.55072(3) 0.62488(2) 0.66943(3) 0.05212(13) Uani 1 1 d . . . . .
Si1 Si 0.32388(4) 0.60287(2) 0.42640(4) 0.04256(13) Uani 1 1 d . . . . .
Si2 Si 0.42428(5) 0.70025(2) 0.47641(4) 0.04577(14) Uani 1 1 d . . . . .
N1 N 0.58130(11) 0.60364(4) 0.84509(10) 0.0315(3) Uani 1 1 d . . . . .
N5 N 0.75954(11) 0.61615(4) 0.72736(10) 0.0324(3) Uani 1 1 d . . . . .
N41 N 0.41635(12) 0.64437(5) 0.50102(10) 0.0378(3) Uani 1 1 d . . . . .
C2 C 0.62578(13) 0.56138(5) 0.84957(12) 0.0319(3) Uani 1 1 d . . . . .
C3 C 0.70927(14) 0.54888(5) 0.80440(13) 0.0375(3) Uani 1 1 d . . . . .
H3 H 0.713431 0.516998 0.793254 0.045 Uiso 1 1 calc R U . . .
C4 C 0.78944(13) 0.57589(5) 0.77214(12) 0.0326(3) Uani 1 1 d . . . . .
C6 C 0.52833(14) 0.61645(5) 0.92032(13) 0.0341(3) Uani 1 1 d . . . . .
C7 C 0.40175(15) 0.62308(5) 0.88355(14) 0.0376(3) Uani 1 1 d . . . . .
C8 C 0.35259(17) 0.63690(6) 0.95771(16) 0.0478(4) Uani 1 1 d . . . . .
H8 H 0.267003 0.641207 0.933447 0.057 Uiso 1 1 calc R U . . .
C9 C 0.42562(19) 0.64438(7) 1.06515(16) 0.0541(5) Uani 1 1 d . . . . .
H9 H 0.390518 0.653397 1.114819 0.065 Uiso 1 1 calc R U . . .
C10 C 0.54960(19) 0.63879(6) 1.10063(15) 0.0512(4) Uani 1 1 d . . . . .
H10 H 0.599554 0.644244 1.175021 0.061 Uiso 1 1 calc R U . . .
C11 C 0.60394(16) 0.62527(6) 1.02978(13) 0.0415(4) Uani 1 1 d . . . . .
C12 C 0.31914(15) 0.61830(6) 0.76422(14) 0.0414(4) Uani 1 1 d . . . . .
H12 H 0.362983 0.599326 0.728791 0.050 Uiso 1 1 calc R U . . .
C13 C 0.19768(18) 0.59496(8) 0.74425(19) 0.0625(5) Uani 1 1 d . . . . .
H13A H 0.149381 0.614287 0.772214 0.075 Uiso 1 1 calc R U . . .
H13B H 0.212897 0.565443 0.781798 0.075 Uiso 1 1 calc R U . . .
H13C H 0.152829 0.590160 0.665932 0.075 Uiso 1 1 calc R U . . .
C14 C 0.29761(19) 0.66536(7) 0.71083(16) 0.0534(4) Uani 1 1 d . . . . .
H14A H 0.376261 0.679982 0.724723 0.064 Uiso 1 1 calc R U . . .
H14B H 0.250829 0.684206 0.741350 0.064 Uiso 1 1 calc R U . . .
H14C H 0.251935 0.662095 0.632148 0.064 Uiso 1 1 calc R U . . .
C15 C 0.74160(18) 0.62258(7) 1.07181(15) 0.0539(5) Uani 1 1 d . . . . .
H15 H 0.763163 0.611474 1.010803 0.065 Uiso 1 1 calc R U . . .
C16 C 0.7958(2) 0.58894(11) 1.1665(2) 0.0876(8) Uani 1 1 d . . . . .
H16A H 0.780970 0.600091 1.229375 0.105 Uiso 1 1 calc R U . . .
H16B H 0.883795 0.586194 1.186000 0.105 Uiso 1 1 calc R U . . .
H16C H 0.757265 0.558994 1.144549 0.105 Uiso 1 1 calc R U . . .
C17 C 0.7980(3) 0.66939(11) 1.1046(3) 0.0961(9) Uani 1 1 d . . . . .
H17A H 0.780100 0.680844 1.165664 0.115 Uiso 1 1 calc R U . . .
H17B H 0.763896 0.690339 1.042713 0.115 Uiso 1 1 calc R U . . .
H17C H 0.886522 0.667287 1.126516 0.115 Uiso 1 1 calc R U . . .
C18 C 0.58111(15) 0.52265(5) 0.90242(14) 0.0391(4) Uani 1 1 d . . . . .
H18 H 0.549068 0.537008 0.953829 0.047 Uiso 1 1 calc R U . . .
C19 C 0.47527(19) 0.49813(7) 0.81517(18) 0.0597(5) Uani 1 1 d . . . . .
H19A H 0.446332 0.473495 0.848633 0.072 Uiso 1 1 calc R U . . .
H19B H 0.502475 0.485267 0.760735 0.072 Uiso 1 1 calc R U . . .
H19C H 0.408793 0.519810 0.779899 0.072 Uiso 1 1 calc R U . . .
C20 C 0.67792(19) 0.48824(7) 0.96699(17) 0.0561(5) Uani 1 1 d . . . . .
H20A H 0.700494 0.469584 0.916872 0.067 Uiso 1 1 calc R U . . .
H20B H 0.645620 0.468509 1.008675 0.067 Uiso 1 1 calc R U . . .
H20C H 0.750050 0.504443 1.017059 0.067 Uiso 1 1 calc R U . . .
C21 C 0.91690(15) 0.55628(6) 0.79996(15) 0.0432(4) Uani 1 1 d . . . . .
H21 H 0.958229 0.575577 0.762829 0.052 Uiso 1 1 calc R U . . .
C22 C 0.9203(2) 0.50730(7) 0.7648(2) 0.0610(5) Uani 1 1 d . . . . .
H22A H 0.866612 0.503993 0.687710 0.073 Uiso 1 1 calc R U . . .
H22B H 0.892475 0.486974 0.808660 0.073 Uiso 1 1 calc R U . . .
H22C H 1.003908 0.499248 0.775137 0.073 Uiso 1 1 calc R U . . .
C23 C 0.98841(19) 0.56114(8) 0.92276(19) 0.0663(6) Uani 1 1 d . . . . .
H23A H 1.074143 0.553349 0.941043 0.080 Uiso 1 1 calc R U . . .
H23B H 0.954226 0.540487 0.961247 0.080 Uiso 1 1 calc R U . . .
H23C H 0.982673 0.592686 0.944695 0.080 Uiso 1 1 calc R U . . .
C24 C 0.84104(13) 0.64239(5) 0.69447(13) 0.0364(3) Uani 1 1 d . . . . .
C25 C 0.85088(15) 0.63228(6) 0.59506(14) 0.0437(4) Uani 1 1 d . . . . .
C26 C 0.92040(17) 0.66147(8) 0.55973(17) 0.0563(5) Uani 1 1 d . . . . .
H26 H 0.927706 0.655390 0.492669 0.068 Uiso 1 1 calc R U . . .
C27 C 0.97845(19) 0.69882(7) 0.6200(2) 0.0646(6) Uani 1 1 d . . . . .
H27 H 1.024895 0.718383 0.594214 0.078 Uiso 1 1 calc R U . . .
C28 C 0.96944(19) 0.70787(7) 0.7170(2) 0.0594(5) Uani 1 1 d . . . . .
H28 H 1.010768 0.733628 0.758201 0.071 Uiso 1 1 calc R U . . .
C29 C 0.90102(15) 0.68019(6) 0.75698(16) 0.0458(4) Uani 1 1 d . . . . .
C30 C 0.78809(17) 0.59164(7) 0.52518(14) 0.0517(4) Uani 1 1 d . . . . .
H30 H 0.754889 0.572188 0.568712 0.062 Uiso 1 1 calc R U . . .
C31 C 0.8753(2) 0.56217(9) 0.49415(19) 0.0665(6) Uani 1 1 d . . . . .
H31A H 0.944678 0.553097 0.560193 0.080 Uiso 1 1 calc R U . . .
H31B H 0.904654 0.579670 0.446746 0.080 Uiso 1 1 calc R U . . .
H31C H 0.832334 0.534855 0.455616 0.080 Uiso 1 1 calc R U . . .
C32 C 0.6806(2) 0.60697(11) 0.42301(18) 0.0786(7) Uani 1 1 d . . . . .
H32A H 0.709863 0.627443 0.380425 0.094 Uiso 1 1 calc R U . . .
H32B H 0.621163 0.623101 0.444045 0.094 Uiso 1 1 calc R U . . .
H32C H 0.641807 0.580211 0.379013 0.094 Uiso 1 1 calc R U . . .
C33 C 0.89401(17) 0.69150(6) 0.86537(17) 0.0529(5) Uani 1 1 d . . . . .
H33 H 0.844288 0.667280 0.881408 0.064 Uiso 1 1 calc R U . . .
C34 C 1.0200(2) 0.69197(8) 0.9584(2) 0.0671(6) Uani 1 1 d . . . . .
H34A H 1.067671 0.717480 0.948284 0.081 Uiso 1 1 calc R U . . .
H34B H 1.061988 0.663188 0.958711 0.081 Uiso 1 1 calc R U . . .
H34C H 1.011025 0.695553 1.027863 0.081 Uiso 1 1 calc R U . . .
C35 C 0.8313(3) 0.73743(9) 0.8615(2) 0.0834(8) Uani 1 1 d . . . . .
H35A H 0.749115 0.736746 0.803980 0.100 Uiso 1 1 calc R U . . .
H35B H 0.878786 0.761783 0.846326 0.100 Uiso 1 1 calc R U . . .
H35C H 0.825977 0.743167 0.931819 0.100 Uiso 1 1 calc R U . . .
C42 C 0.3846(3) 0.54776(8) 0.4989(2) 0.0883(8) Uani 1 1 d . . . . .
H42A H 0.371761 0.546839 0.567001 0.106 Uiso 1 1 calc R U . . .
H42B H 0.472047 0.545517 0.515112 0.106 Uiso 1 1 calc R U . . .
H42C H 0.341776 0.522127 0.452483 0.106 Uiso 1 1 calc R U . . .
C43 C 0.3174(3) 0.59792(11) 0.28502(19) 0.0817(8) Uani 1 1 d . . . . .
H43A H 0.400147 0.594276 0.287484 0.098 Uiso 1 1 calc R U . . .
H43B H 0.280533 0.625572 0.243973 0.098 Uiso 1 1 calc R U . . .
H43C H 0.268065 0.571323 0.249288 0.098 Uiso 1 1 calc R U . . .
C44 C 0.16212(19) 0.60737(9) 0.4119(2) 0.0694(6) Uani 1 1 d . . . . .
H44A H 0.127024 0.636055 0.375258 0.083 Uiso 1 1 calc R U . . .
H44B H 0.159061 0.606796 0.484214 0.083 Uiso 1 1 calc R U . . .
H44C H 0.115307 0.581614 0.368778 0.083 Uiso 1 1 calc R U . . .
C45 C 0.5470(2) 0.72521(7) 0.6022(2) 0.0676(6) Uani 1 1 d . . . . .
H45A H 0.624934 0.710174 0.615259 0.081 Uiso 1 1 calc R U . . .
H45B H 0.525337 0.720391 0.665055 0.081 Uiso 1 1 calc R U . . .
H45C H 0.554405 0.757999 0.591655 0.081 Uiso 1 1 calc R U . . .
C46 C 0.4704(3) 0.71516(10) 0.3620(2) 0.0957(9) Uani 1 1 d . . . . .
H46A H 0.406505 0.705457 0.292866 0.115 Uiso 1 1 calc R U . . .
H46B H 0.546886 0.699597 0.372245 0.115 Uiso 1 1 calc R U . . .
H46C H 0.481913 0.748244 0.360742 0.115 Uiso 1 1 calc R U . . .
C47 C 0.2807(2) 0.73250(8) 0.4524(2) 0.0777(7) Uani 1 1 d . . . . .
H47A H 0.260036 0.729616 0.516310 0.093 Uiso 1 1 calc R U . . .
H47B H 0.214223 0.720009 0.388433 0.093 Uiso 1 1 calc R U . . .
H47C H 0.292550 0.764780 0.439955 0.093 Uiso 1 1 calc R U . . .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Ca Ca 0.2262 0.3064
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(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
_geom_angle_publ_flag
N41 Ca1 N5 127.55(5) . . ?
N41 Ca1 N1 147.55(5) . . ?
N5 Ca1 N1 84.87(4) . . ?
N41 Ca1 C2 148.92(5) . . ?
N5 Ca1 C2 73.12(4) . . ?
N1 Ca1 C2 27.01(4) . . ?
N41 Ca1 C4 138.63(5) . . ?
N5 Ca1 C4 24.44(4) . . ?
N1 Ca1 C4 70.34(4) . . ?
C2 Ca1 C4 51.88(4) . . ?
N41 Ca1 C3 144.38(5) . . ?
N5 Ca1 C3 51.61(4) . . ?
N1 Ca1 C3 51.93(4) . . ?
C2 Ca1 C3 27.31(4) . . ?
C4 Ca1 C3 27.54(4) . . ?
N41 Ca1 C45 62.89(6) . . ?
N5 Ca1 C45 95.39(5) . . ?
N1 Ca1 C45 122.18(6) . . ?
C2 Ca1 C45 145.48(6) . . ?
C4 Ca1 C45 119.66(5) . . ?
C3 Ca1 C45 144.62(5) . . ?
N41 Si1 C43 114.43(10) . . ?
N41 Si1 C44 114.91(9) . . ?
C43 Si1 C44 105.68(12) . . ?
N41 Si1 C42 106.63(10) . . ?
C43 Si1 C42 108.05(14) . . ?
C44 Si1 C42 106.74(14) . . ?
N41 Si2 C46 116.44(11) . . ?
N41 Si2 C47 114.08(9) . . ?
C46 Si2 C47 106.58(14) . . ?
N41 Si2 C45 106.65(9) . . ?
C46 Si2 C45 105.27(14) . . ?
C47 Si2 C45 107.11(12) . . ?
C2 N1 C6 119.18(12) . . ?
C2 N1 Ca1 101.31(9) . . ?
C6 N1 Ca1 134.76(10) . . ?
C4 N5 C24 121.81(12) . . ?
C4 N5 Ca1 108.50(9) . . ?
C24 N5 Ca1 127.38(9) . . ?
Si2 N41 Si1 131.55(8) . . ?
Si2 N41 Ca1 111.60(7) . . ?
Si1 N41 Ca1 116.77(7) . . ?
N1 C2 C3 123.98(13) . . ?
N1 C2 C18 120.03(13) . . ?
C3 C2 C18 115.94(13) . . ?
N1 C2 Ca1 51.69(7) . . ?
C3 C2 Ca1 81.38(9) . . ?
C18 C2 Ca1 143.80(10) . . ?
C2 C3 C4 131.04(14) . . ?
C2 C3 Ca1 71.31(9) . . ?
C4 C3 Ca1 75.40(9) . . ?
C2 C3 H3 114.5 . . ?
C4 C3 H3 114.5 . . ?
Ca1 C3 H3 133.7 . . ?
N5 C4 C3 122.84(14) . . ?
N5 C4 C21 121.15(13) . . ?
C3 C4 C21 115.90(13) . . ?
N5 C4 Ca1 47.07(7) . . ?
C3 C4 Ca1 77.06(9) . . ?
C21 C4 Ca1 165.22(11) . . ?
C7 C6 C11 119.97(14) . . ?
C7 C6 N1 120.03(14) . . ?
C11 C6 N1 119.87(14) . . ?
C8 C7 C6 119.02(16) . . ?
C8 C7 C12 119.53(15) . . ?
C6 C7 C12 121.34(14) . . ?
C9 C8 C7 121.19(17) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 119.78(16) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 121.49(18) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 118.49(16) . . ?
C10 C11 C15 119.14(16) . . ?
C6 C11 C15 122.32(14) . . ?
C7 C12 C14 109.16(15) . . ?
C7 C12 C13 113.91(15) . . ?
C14 C12 C13 110.41(16) . . ?
C7 C12 H12 107.7 . . ?
C14 C12 H12 107.7 . . ?
C13 C12 H12 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 110.72(19) . . ?
C11 C15 C16 112.61(18) . . ?
C17 C15 C16 110.4(2) . . ?
C11 C15 H15 107.6 . . ?
C17 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 C19 109.77(16) . . ?
C20 C18 C2 115.29(14) . . ?
C19 C18 C2 109.25(14) . . ?
C20 C18 H18 107.4 . . ?
C19 C18 H18 107.4 . . ?
C2 C18 H18 107.4 . . ?
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 C4 115.19(15) . . ?
C22 C21 C23 110.44(16) . . ?
C4 C21 C23 107.96(15) . . ?
C22 C21 H21 107.7 . . ?
C4 C21 H21 107.7 . . ?
C23 C21 H21 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C29 C24 C25 121.02(15) . . ?
C29 C24 N5 119.26(15) . . ?
C25 C24 N5 119.47(14) . . ?
C26 C25 C24 118.01(18) . . ?
C26 C25 C30 119.23(17) . . ?
C24 C25 C30 122.76(15) . . ?
C27 C26 C25 121.3(2) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 120.02(18) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 121.7(2) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C24 117.95(18) . . ?
C28 C29 C33 119.80(18) . . ?
C24 C29 C33 122.25(15) . . ?
C25 C30 C32 110.93(19) . . ?
C25 C30 C31 112.73(16) . . ?
C32 C30 C31 110.21(17) . . ?
C25 C30 H30 107.6 . . ?
C32 C30 H30 107.6 . . ?
C31 C30 H30 107.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C33 C34 111.88(17) . . ?
C29 C33 C35 111.63(18) . . ?
C34 C33 C35 109.29(18) . . ?
C29 C33 H33 108.0 . . ?
C34 C33 H33 108.0 . . ?
C35 C33 H33 108.0 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Si1 C44 H44A 109.5 . . ?
Si1 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si1 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si2 C45 Ca1 78.85(7) . . ?
Si2 C45 H45A 109.5 . . ?
Ca1 C45 H45A 67.3 . . ?
Si2 C45 H45B 109.5 . . ?
Ca1 C45 H45B 65.8 . . ?
H45A C45 H45B 109.5 . . ?
Si2 C45 H45C 109.5 . . ?
Ca1 C45 H45C 171.6 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si2 C46 H46A 109.5 . . ?
Si2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
Si2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si2 C47 H47A 109.5 . . ?
Si2 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
Si2 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
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 N41 2.2631(13) . ?
Ca1 N5 2.3128(13) . ?
Ca1 N1 2.3131(12) . ?
Ca1 C2 2.8908(15) . ?
Ca1 C4 2.9958(15) . ?
Ca1 C3 3.0172(17) . ?
Ca1 C45 3.068(2) . ?
Si1 N41 1.6804(14) . ?
Si1 C43 1.864(2) . ?
Si1 C44 1.866(2) . ?
Si1 C42 1.876(2) . ?
Si2 N41 1.6796(14) . ?
Si2 C46 1.867(3) . ?
Si2 C47 1.869(2) . ?
Si2 C45 1.889(2) . ?
N1 C2 1.3387(19) . ?
N1 C6 1.4306(19) . ?
N5 C4 1.307(2) . ?
N5 C24 1.4362(19) . ?
C2 C3 1.400(2) . ?
C2 C18 1.538(2) . ?
C3 C4 1.431(2) . ?
C3 H3 0.9500 . ?
C4 C21 1.528(2) . ?
C6 C7 1.405(2) . ?
C6 C11 1.408(2) . ?
C7 C8 1.394(2) . ?
C7 C12 1.515(2) . ?
C8 C9 1.372(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(2) . ?
C10 H10 0.9500 . ?
C11 C15 1.514(3) . ?
C12 C14 1.527(3) . ?
C12 C13 1.527(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.514(3) . ?
C15 C16 1.531(3) . ?
C15 H15 1.0000 . ?
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 C20 1.520(2) . ?
C18 C19 1.520(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 1.515(3) . ?
C21 C23 1.529(3) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C29 1.402(2) . ?
C24 C25 1.409(2) . ?
C25 C26 1.396(2) . ?
C25 C30 1.517(3) . ?
C26 C27 1.373(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.367(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.396(3) . ?
C28 H28 0.9500 . ?
C29 C33 1.519(3) . ?
C30 C32 1.527(3) . ?
C30 C31 1.528(3) . ?
C30 H30 1.0000 . ?
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 C34 1.528(3) . ?
C33 C35 1.530(3) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C46 Si2 N41 Si1 -65.66(17) . . . . ?
C47 Si2 N41 Si1 59.18(16) . . . . ?
C45 Si2 N41 Si1 177.22(12) . . . . ?
C46 Si2 N41 Ca1 117.73(14) . . . . ?
C47 Si2 N41 Ca1 -117.43(12) . . . . ?
C45 Si2 N41 Ca1 0.61(11) . . . . ?
C43 Si1 N41 Si2 52.64(16) . . . . ?
C44 Si1 N41 Si2 -69.92(15) . . . . ?
C42 Si1 N41 Si2 172.04(14) . . . . ?
C43 Si1 N41 Ca1 -130.89(12) . . . . ?
C44 Si1 N41 Ca1 106.55(11) . . . . ?
C42 Si1 N41 Ca1 -11.49(14) . . . . ?
C6 N1 C2 C3 -160.64(15) . . . . ?
Ca1 N1 C2 C3 40.29(17) . . . . ?
C6 N1 C2 C18 22.1(2) . . . . ?
Ca1 N1 C2 C18 -136.98(12) . . . . ?
C6 N1 C2 Ca1 159.07(15) . . . . ?
N1 C2 C3 C4 18.8(3) . . . . ?
C18 C2 C3 C4 -163.84(17) . . . . ?
Ca1 C2 C3 C4 49.66(18) . . . . ?
N1 C2 C3 Ca1 -30.88(13) . . . . ?
C18 C2 C3 Ca1 146.49(13) . . . . ?
C24 N5 C4 C3 -179.24(14) . . . . ?
Ca1 N5 C4 C3 -15.34(18) . . . . ?
C24 N5 C4 C21 4.9(2) . . . . ?
Ca1 N5 C4 C21 168.77(12) . . . . ?
C24 N5 C4 Ca1 -163.90(17) . . . . ?
C2 C3 C4 N5 -36.8(3) . . . . ?
Ca1 C3 C4 N5 11.46(13) . . . . ?
C2 C3 C4 C21 139.29(18) . . . . ?
Ca1 C3 C4 C21 -172.45(13) . . . . ?
C2 C3 C4 Ca1 -48.26(17) . . . . ?
C2 N1 C6 C7 -109.44(16) . . . . ?
Ca1 N1 C6 C7 41.0(2) . . . . ?
C2 N1 C6 C11 74.65(19) . . . . ?
Ca1 N1 C6 C11 -134.91(13) . . . . ?
C11 C6 C7 C8 -2.2(2) . . . . ?
N1 C6 C7 C8 -178.09(14) . . . . ?
C11 C6 C7 C12 174.08(15) . . . . ?
N1 C6 C7 C12 -1.8(2) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C12 C7 C8 C9 -175.85(16) . . . . ?
C7 C8 C9 C10 0.8(3) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C9 C10 C11 C6 -1.3(3) . . . . ?
C9 C10 C11 C15 176.14(18) . . . . ?
C7 C6 C11 C10 2.6(2) . . . . ?
N1 C6 C11 C10 178.47(15) . . . . ?
C7 C6 C11 C15 -174.77(16) . . . . ?
N1 C6 C11 C15 1.1(2) . . . . ?
C8 C7 C12 C14 80.70(19) . . . . ?
C6 C7 C12 C14 -95.53(18) . . . . ?
C8 C7 C12 C13 -43.2(2) . . . . ?
C6 C7 C12 C13 140.56(17) . . . . ?
C10 C11 C15 C17 -64.4(3) . . . . ?
C6 C11 C15 C17 112.9(2) . . . . ?
C10 C11 C15 C16 59.8(3) . . . . ?
C6 C11 C15 C16 -122.9(2) . . . . ?
N1 C2 C18 C20 -142.86(16) . . . . ?
C3 C2 C18 C20 39.7(2) . . . . ?
Ca1 C2 C18 C20 152.14(15) . . . . ?
N1 C2 C18 C19 92.99(18) . . . . ?
C3 C2 C18 C19 -84.49(18) . . . . ?
Ca1 C2 C18 C19 28.0(2) . . . . ?
N5 C4 C21 C22 -132.99(17) . . . . ?
C3 C4 C21 C22 50.8(2) . . . . ?
Ca1 C4 C21 C22 -99.0(4) . . . . ?
N5 C4 C21 C23 103.08(18) . . . . ?
C3 C4 C21 C23 -73.09(19) . . . . ?
Ca1 C4 C21 C23 137.1(4) . . . . ?
C4 N5 C24 C29 -105.57(17) . . . . ?
Ca1 N5 C24 C29 93.76(16) . . . . ?
C4 N5 C24 C25 80.15(19) . . . . ?
Ca1 N5 C24 C25 -80.53(17) . . . . ?
C29 C24 C25 C26 -1.1(2) . . . . ?
N5 C24 C25 C26 173.09(14) . . . . ?
C29 C24 C25 C30 179.70(16) . . . . ?
N5 C24 C25 C30 -6.1(2) . . . . ?
C24 C25 C26 C27 0.4(3) . . . . ?
C30 C25 C26 C27 179.69(18) . . . . ?
C25 C26 C27 C28 0.4(3) . . . . ?
C26 C27 C28 C29 -0.7(3) . . . . ?
C27 C28 C29 C24 0.0(3) . . . . ?
C27 C28 C29 C33 179.79(18) . . . . ?
C25 C24 C29 C28 0.8(2) . . . . ?
N5 C24 C29 C28 -173.34(15) . . . . ?
C25 C24 C29 C33 -178.90(16) . . . . ?
N5 C24 C29 C33 6.9(2) . . . . ?
C26 C25 C30 C32 -71.8(2) . . . . ?
C24 C25 C30 C32 107.45(19) . . . . ?
C26 C25 C30 C31 52.4(2) . . . . ?
C24 C25 C30 C31 -128.41(18) . . . . ?
C28 C29 C33 C34 -59.0(2) . . . . ?
C24 C29 C33 C34 120.74(19) . . . . ?
C28 C29 C33 C35 63.8(2) . . . . ?
C24 C29 C33 C35 -116.4(2) . . . . ?
N41 Si2 C45 Ca1 -0.43(8) . . . . ?
C46 Si2 C45 Ca1 -124.72(10) . . . . ?
C47 Si2 C45 Ca1 122.10(9) . . . . ?
