#------------------------------------------------------------------------------
#$Date: 2025-07-06 20:03:33 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300964 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/80/7718010.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_7718010
loop_
_publ_author_name
'Haynes, Matthew D.'
'O'Reilly, Andrea'
'Poole, Alice J. M.'
'Roper, Aisling F.'
'Thum, Stefan'
'Morris, Louis J.'
'Coles, Martyn P.'
'Fulton, J. Robin'
'Harder, Sjoerd'
'Turner, Zoë R'
'O'Hare, Dermot'
_publ_section_title
;
 Heavier alkaline earth and heterobimetallic s-block "ate" complexes of a
 di(amido)siloxane ligand: solid-state structure and dynamic
 solution-phase behaviour.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4542
_journal_page_last               4555
_journal_paper_doi               10.1039/d5dt00044k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C56 H92 Ca2 N4 O2 Si4, C6 H14'
_chemical_formula_sum            'C62 H106 Ca2 N4 O2 Si4'
_chemical_formula_weight         1132.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-18 deposited with the CCDC.	2025-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.787(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.405(3)
_cell_length_b                   10.7081(9)
_cell_length_c                   19.7961(13)
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.2000
_cell_measurement_theta_min      4.4310
_cell_volume                     6649.3(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  29.00   1.00   10.00    --  -41.15  19.00 -90.00   34
  2  ω    -21.00   5.00   1.00   10.00    --  -41.15  37.00 -60.00   26
  3  ω    -57.00 -19.00   1.00   10.00    --  -41.15 -37.00  30.00   38
  4  ω     -5.00  36.00   1.00   10.00    --  -41.15  19.00 -30.00   41
  5  ω   -114.00 -84.00   1.00   10.00    --  -41.15 -37.00  30.00   30
  6  ω     11.00  36.00   1.00   10.00    --  -41.15  19.00 120.00   25
  7  ω    -39.00  20.00   1.00   10.00    --  -41.15  57.00  30.00   59
  8  ω    108.00 177.00   1.00   40.00    --  111.00  77.00 -30.00   69
  9  ω     40.00  66.00   1.00   40.00    --  111.00 -45.00 -60.00   26
 10  ω     42.00  81.00   1.00   40.00    --  111.00 -61.00 120.00   39
 11  ω     99.00 169.00   1.00   40.00    --  111.00 125.00-120.00   70
 12  ω     31.00  93.00   1.00   40.00    --  111.00 -94.00  30.00   62
 13  ω     42.00  69.00   1.00   40.00    --  111.00 -45.00-150.00   27
 14  ω     98.00 124.00   1.00   40.00    --  111.00 125.00 150.00   26
 15  ω     40.00  71.00   1.00   40.00    --  111.00 -45.00   0.00   31
 16  ω     58.00  92.00   1.00   40.00    --  111.00 -61.00 150.00   34
 17  ω     54.00  86.00   1.00   40.00    --  111.00 -61.00-120.00   32
 18  ω    112.00 155.00   1.00   40.00    --  111.00  77.00-120.00   43
 19  ω    106.00 178.00   1.00   40.00    --  111.00  77.00  60.00   72
 20  ω     42.00  72.00   1.00   40.00    --  111.00 -45.00 -90.00   30
 21  ω     41.00  79.00   1.00   40.00    --  111.00-125.00 -90.00   38
 22  ω     44.00  78.00   1.00   40.00    --  111.00-125.00   0.00   34
 23  ω    126.00 167.00   1.00   40.00    --  111.00  45.00 120.00   41
 24  ω     88.00 113.00   1.00   40.00    --  111.00  45.00 120.00   25
 25  ω      0.00  31.00   1.00   10.00    --  -41.15  19.00-120.00   31
 26  ω    -40.00  23.00   1.00   10.00    --  -41.15  57.00-180.00   63
 27  ω     -5.00  21.00   1.00   10.00    --  -41.15  19.00   0.00   26
 28  ω     42.00  89.00   1.00   10.00    --   41.15-125.00 -30.00   47
 29  ω     53.00  79.00   1.00   10.00    --   41.15-125.00 -60.00   26
 30  ω     33.00  87.00   1.00   10.00    --   41.15-125.00 150.00   54
 31  ω    106.00 175.00   1.00   40.00    --  111.00  77.00   0.00   69
 32  ω     77.00 104.00   1.00   40.00    --  111.00 -94.00 -30.00   27
 33  ω    105.00 153.00   1.00   40.00    --  111.00  77.00-150.00   48
 34  ω     98.00 125.00   1.00   40.00    --  111.00 125.00-180.00   27
 35  ω     77.00 110.00   1.00   40.00    --  111.00-125.00 150.00   33
 36  ω     45.00  77.00   1.00   40.00    --  111.00-125.00  90.00   32
 37  ω     58.00  91.00   1.00   40.00    --  111.00 -61.00 -60.00   33
 38  ω     68.00 107.00   1.00   40.00    --  111.00 -94.00 -90.00   39
 39  ω    138.00 174.00   1.00   40.00    --  111.00  45.00 150.00   36
 40  ω     49.00  96.00   1.00   40.00    --  111.00-125.00-180.00   47
 41  ω     38.00  84.00   1.00   40.00    --  111.00 -77.00-180.00   46
 42  ω     40.00  70.00   1.00   40.00    --  111.00 -45.00  30.00   30
 43  ω     77.00 112.00   1.00   40.00    --  111.00-125.00   0.00   35
 44  ω     41.00  66.00   1.00   40.00    --  111.00 -61.00 -30.00   25
 45  ω     67.00 106.00   1.00   40.00    --  111.00 -94.00-180.00   39
 46  ω    148.00 176.00   1.00   40.00    --  111.00 125.00-180.00   28
 47  ω    100.00 173.00   1.00   40.00    --  111.00  45.00 -60.00   73
 48  ω     82.00 107.00   1.00   40.00    --  111.00 -94.00 120.00   25
 49  ω     81.00 107.00   1.00   40.00    --  111.00 -94.00  30.00   26
 50  ω     41.00  67.00   1.00   40.00    --  111.00-125.00-150.00   26
 51  ω     75.00 112.00   1.00   40.00    --  111.00-125.00 -90.00   37
 52  ω     73.00 107.00   1.00   40.00    --  111.00 -94.00-120.00   34
 53  ω     32.00  64.00   1.00   40.00    --  111.00 -94.00 120.00   32
 54  ω    151.00 178.00   1.00   40.00    --  111.00  45.00 120.00   27
 55  ω      2.00  27.00   1.00   10.00    --   38.00  90.00 133.48   25
 56  ω    -17.00  31.00   1.00   10.00    --  -41.15  37.00  90.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0464713000
_diffrn_orient_matrix_UB_12      -0.0275497000
_diffrn_orient_matrix_UB_13      0.0167726000
_diffrn_orient_matrix_UB_21      0.0037883000
_diffrn_orient_matrix_UB_22      0.0939717000
_diffrn_orient_matrix_UB_23      0.0590418000
_diffrn_orient_matrix_UB_31      -0.0153945000
_diffrn_orient_matrix_UB_32      0.1055534000
_diffrn_orient_matrix_UB_33      -0.0479390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40355
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.495
_diffrn_reflns_theta_min         4.363
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       Shard
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0912P)²+3.8214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4365
_reflns_number_total             6929
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00044k2.cif
_cod_data_source_block           002mdh24
_cod_depositor_comments
'Adding full bibliography for 7718002--7718016.cif.'
_cod_database_code               7718010
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C52 H92 Ca2 N4 O2 Si4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.641
_oxdiff_exptl_absorpt_empirical_full_min 0.697
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.44256(2) 0.76723(6) 0.72114(3) 0.04144(18) Uani 1 1 d . . . . .
Si1 Si 0.41361(3) 0.56141(9) 0.62201(5) 0.0479(2) Uani 1 1 d . . . . .
Si2 Si 0.51086(3) 0.65317(8) 0.62299(4) 0.0398(2) Uani 1 1 d . . . . .
O1 O 0.46249(8) 0.6129(2) 0.64486(11) 0.0442(5) Uani 1 1 d . . . . .
N1 N 0.38536(10) 0.6492(3) 0.67448(14) 0.0464(6) Uani 1 1 d . . . . .
N2 N 0.52074(10) 0.7829(2) 0.67078(13) 0.0420(6) Uani 1 1 d . . . . .
C1 C 0.40392(16) 0.5893(5) 0.5291(2) 0.0737(13) Uani 1 1 d . . . . .
H1A H 0.4066 0.6787 0.5196 0.111 Uiso 1 1 calc R U . . .
H1B H 0.3752 0.5611 0.5150 0.111 Uiso 1 1 calc R U . . .
H1C H 0.4249 0.5428 0.5041 0.111 Uiso 1 1 calc R U . . .
C2 C 0.41728(17) 0.3884(4) 0.6331(3) 0.0737(13) Uani 1 1 d . . . . .
H2A H 0.4396 0.3553 0.6052 0.111 Uiso 1 1 calc R U . . .
H2B H 0.3899 0.3501 0.6192 0.111 Uiso 1 1 calc R U . . .
H2C H 0.4243 0.3689 0.6807 0.111 Uiso 1 1 calc R U . . .
C3 C 0.51070(14) 0.6852(3) 0.53052(17) 0.0535(9) Uani 1 1 d . . . . .
H3A H 0.4973 0.6152 0.5057 0.080 Uiso 1 1 calc R U . . .
H3B H 0.5401 0.6954 0.5169 0.080 Uiso 1 1 calc R U . . .
H3C H 0.4946 0.7619 0.5203 0.080 Uiso 1 1 calc R U . . .
C4 C 0.54465(14) 0.5154(3) 0.6466(2) 0.0563(9) Uani 1 1 d . . . . .
H4A H 0.5467 0.5068 0.6960 0.084 Uiso 1 1 calc R U . . .
H4B H 0.5732 0.5270 0.6298 0.084 Uiso 1 1 calc R U . . .
H4C H 0.5318 0.4398 0.6265 0.084 Uiso 1 1 calc R U . . .
C5 C 0.34028(13) 0.6466(4) 0.67464(19) 0.0529(9) Uani 1 1 d . . . . .
C6 C 0.31883(14) 0.5547(4) 0.7129(2) 0.0598(10) Uani 1 1 d . . . . .
C7 C 0.27445(16) 0.5567(5) 0.7129(3) 0.0744(13) Uani 1 1 d . . . . .
H7 H 0.2603 0.4954 0.7384 0.089 Uiso 1 1 calc R U . . .
C8 C 0.25030(16) 0.6442(6) 0.6774(3) 0.0895(17) Uani 1 1 d . . . . .
H8 H 0.2201 0.6426 0.6778 0.107 Uiso 1 1 calc R U . . .
C9 C 0.27081(17) 0.7344(6) 0.6409(3) 0.0837(15) Uani 1 1 d . . . . .
H9 H 0.2543 0.7952 0.6165 0.100 Uiso 1 1 calc R U . . .
C10 C 0.31494(15) 0.7385(5) 0.6393(2) 0.0665(11) Uani 1 1 d . . . . .
C11 C 0.34255(15) 0.4557(4) 0.7538(2) 0.0647(11) Uani 1 1 d . . . . .
H11 H 0.3737 0.4678 0.7476 0.078 Uiso 1 1 calc R U . . .
C12 C 0.33524(18) 0.4662(6) 0.8296(2) 0.0810(15) Uani 1 1 d . . . . .
H12A H 0.3439 0.5494 0.8458 0.122 Uiso 1 1 calc R U . . .
H12B H 0.3522 0.4026 0.8543 0.122 Uiso 1 1 calc R U . . .
H12C H 0.3049 0.4535 0.8373 0.122 Uiso 1 1 calc R U . . .
C13 C 0.33057(19) 0.3224(5) 0.7288(3) 0.0806(14) Uani 1 1 d . . . . .
H13A H 0.3493 0.2613 0.7521 0.121 Uiso 1 1 calc R U . . .
H13B H 0.3340 0.3169 0.6800 0.121 Uiso 1 1 calc R U . . .
H13C H 0.3009 0.3047 0.7386 0.121 Uiso 1 1 calc R U . . .
C14 C 0.33429(16) 0.8427(5) 0.5980(3) 0.0712(12) Uani 1 1 d . . . . .
H14 H 0.3660 0.8359 0.6041 0.085 Uiso 1 1 calc R U . . .
C15 C 0.3225(2) 0.8293(6) 0.5220(3) 0.0932(17) Uani 1 1 d . . . . .
H15A H 0.3295 0.7448 0.5071 0.140 Uiso 1 1 calc R U . . .
H15B H 0.3387 0.8903 0.4966 0.140 Uiso 1 1 calc R U . . .
H15C H 0.2919 0.8443 0.5138 0.140 Uiso 1 1 calc R U . . .
C16 C 0.32158(18) 0.9718(5) 0.6227(3) 0.0853(15) Uani 1 1 d . . . . .
H16A H 0.2908 0.9832 0.6148 0.128 Uiso 1 1 calc R U . . .
H16B H 0.3367 1.0359 0.5980 0.128 Uiso 1 1 calc R U . . .
H16C H 0.3291 0.9792 0.6712 0.128 Uiso 1 1 calc R U . . .
C17 C 0.53682(12) 0.8982(3) 0.64679(14) 0.0428(7) Uani 1 1 d . . . . .
C18 C 0.58081(13) 0.9217(3) 0.64318(17) 0.0476(8) Uani 1 1 d . . . . .
C19 C 0.59493(15) 1.0433(4) 0.63077(19) 0.0564(9) Uani 1 1 d . . . . .
H19 H 0.6247 1.0591 0.6297 0.068 Uiso 1 1 calc R U . . .
C20 C 0.56658(15) 1.1411(3) 0.6200(2) 0.0567(9) Uani 1 1 d . . . . .
H20 H 0.5767 1.2238 0.6141 0.068 Uiso 1 1 calc R U . . .
C21 C 0.52348(14) 1.1169(3) 0.61797(17) 0.0525(9) Uani 1 1 d . . . . .
H21 H 0.5040 1.1832 0.6087 0.063 Uiso 1 1 calc R U . . .
C22 C 0.50778(13) 0.9967(3) 0.62927(15) 0.0441(8) Uani 1 1 d . . . . .
C23 C 0.61435(13) 0.8187(4) 0.64770(18) 0.0519(9) Uani 1 1 d . . . . .
H23 H 0.6007 0.7421 0.6657 0.062 Uiso 1 1 calc R U . . .
C24 C 0.62895(19) 0.7883(5) 0.5758(2) 0.0767(14) Uani 1 1 d . . . . .
H24A H 0.6442 0.8601 0.5582 0.115 Uiso 1 1 calc R U . . .
H24B H 0.6040 0.7699 0.5459 0.115 Uiso 1 1 calc R U . . .
H24C H 0.6479 0.7155 0.5780 0.115 Uiso 1 1 calc R U . . .
C25 C 0.65295(16) 0.8496(5) 0.6941(2) 0.0702(12) Uani 1 1 d . . . . .
H25A H 0.6726 0.7783 0.6959 0.105 Uiso 1 1 calc R U . . .
H25B H 0.6436 0.8673 0.7397 0.105 Uiso 1 1 calc R U . . .
H25C H 0.6675 0.9229 0.6767 0.105 Uiso 1 1 calc R U . . .
C26 C 0.46023(12) 0.9762(3) 0.62268(15) 0.0447(8) Uani 1 1 d . . . . .
H26 H 0.4555 0.8839 0.6211 0.054 Uiso 1 1 calc R U . . .
C27 C 0.43774(14) 1.0258(3) 0.68478(18) 0.0529(9) Uani 1 1 d . . . . .
H27A H 0.4530 0.9967 0.7262 0.079 Uiso 1 1 calc R U . . .
H27B H 0.4083 0.9949 0.6837 0.079 Uiso 1 1 calc R U . . .
H27C H 0.4376 1.1173 0.6840 0.079 Uiso 1 1 calc R U . . .
C28 C 0.43899(14) 1.0310(4) 0.55775(18) 0.0534(9) Uani 1 1 d . . . . .
H28A H 0.4379 1.1222 0.5614 0.080 Uiso 1 1 calc R U . . .
H28B H 0.4099 0.9981 0.5514 0.080 Uiso 1 1 calc R U . . .
H28C H 0.4555 1.0076 0.5190 0.080 Uiso 1 1 calc R U . . .
C29 C 0.2890(3) 0.4632(10) 0.5241(6) 0.166(4) Uani 1 1 d . . . . .
H29A H 0.2843 0.4709 0.4750 0.248 Uiso 1 1 calc R U . . .
H29B H 0.3159 0.4191 0.5343 0.248 Uiso 1 1 calc R U . . .
H29C H 0.2905 0.5466 0.5445 0.248 Uiso 1 1 calc R U . . .
C30 C 0.2529(3) 0.3910(9) 0.5527(6) 0.154(4) Uani 1 1 d . . . . .
H30A H 0.2532 0.4041 0.6022 0.185 Uiso 1 1 calc R U . . .
H30B H 0.2255 0.4235 0.5330 0.185 Uiso 1 1 calc R U . . .
C31 C 0.2556(3) 0.2584(9) 0.5388(4) 0.137(3) Uani 1 1 d . . . . .
H31A H 0.2352 0.2116 0.5658 0.164 Uiso 1 1 calc R U . . .
H31B H 0.2847 0.2273 0.5505 0.164 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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 N1 65.82(10) . . ?
O1 Ca1 N2 119.65(9) . 2_656 ?
O1 Ca1 N2 61.94(9) . . ?
N1 Ca1 N2 125.45(9) . . ?
N1 Ca1 N2 135.83(10) . 2_656 ?
N2 Ca1 N2 85.32(9) 2_656 . ?
O1 Si1 N1 98.80(14) . . ?
O1 Si1 C1 108.42(19) . . ?
O1 Si1 C2 104.2(2) . . ?
N1 Si1 C1 116.79(19) . . ?
N1 Si1 C2 120.80(19) . . ?
C2 Si1 C1 106.3(2) . . ?
O1 Si2 Ca1 101.87(9) . 2_656 ?
O1 Si2 N2 102.22(14) . . ?
O1 Si2 C3 110.25(17) . . ?
O1 Si2 C4 104.28(16) . . ?
N2 Si2 Ca1 35.18(9) . 2_656 ?
N2 Si2 C3 112.84(15) . . ?
N2 Si2 C4 114.87(17) . . ?
C3 Si2 Ca1 140.26(13) . 2_656 ?
C3 Si2 C4 111.53(19) . . ?
C4 Si2 Ca1 81.33(14) . 2_656 ?
Si1 O1 Ca1 97.85(11) . . ?
Si2 O1 Ca1 105.20(12) . . ?
Si2 O1 Si1 148.89(15) . . ?
Si1 N1 Ca1 97.30(14) . . ?
C5 N1 Ca1 139.0(2) . . ?
C5 N1 Si1 123.2(2) . . ?
Ca1 N2 Ca1 94.18(9) 2_656 . ?
Si2 N2 Ca1 90.59(12) . . ?
Si2 N2 Ca1 120.58(14) . 2_656 ?
C17 N2 Ca1 101.3(2) . 2_656 ?
C17 N2 Ca1 121.3(2) . . ?
C17 N2 Si2 125.5(2) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 120.7(4) . . ?
N1 C5 C10 121.3(4) . . ?
C10 C5 C6 117.9(4) . . ?
C5 C6 C11 122.3(4) . . ?
C7 C6 C5 119.1(5) . . ?
C7 C6 C11 118.6(4) . . ?
C6 C7 H7 118.8 . . ?
C8 C7 C6 122.4(5) . . ?
C8 C7 H7 118.8 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.9(5) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 119.2 . . ?
C8 C9 C10 121.7(5) . . ?
C10 C9 H9 119.2 . . ?
C5 C10 C14 122.6(4) . . ?
C9 C10 C5 120.0(5) . . ?
C9 C10 C14 117.3(5) . . ?
C6 C11 H11 107.7 . . ?
C6 C11 C12 112.3(4) . . ?
C6 C11 C13 111.7(4) . . ?
C12 C11 H11 107.7 . . ?
C12 C11 C13 109.5(4) . . ?
C13 C11 H11 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14 107.6 . . ?
C10 C14 C15 111.9(5) . . ?
C15 C14 H14 107.6 . . ?
C16 C14 C10 111.9(4) . . ?
C16 C14 H14 107.6 . . ?
C16 C14 C15 110.1(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 Ca1 51.03(15) . 2_656 ?
N2 C17 C22 119.3(3) . . ?
C18 C17 Ca1 87.5(2) . 2_656 ?
C18 C17 N2 122.4(3) . . ?
C18 C17 C22 118.2(3) . . ?
C22 C17 Ca1 131.6(2) . 2_656 ?
C17 C18 C23 123.0(3) . . ?
C19 C18 C17 119.6(4) . . ?
C19 C18 C23 117.3(4) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 C18 121.5(4) . . ?
C20 C19 H19 119.2 . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.1(4) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 119.3 . . ?
C20 C21 C22 121.4(4) . . ?
C22 C21 H21 119.3 . . ?
C17 C22 C26 122.2(3) . . ?
C21 C22 C17 119.5(4) . . ?
C21 C22 C26 118.3(3) . . ?
C18 C23 H23 107.8 . . ?
C18 C23 C24 109.4(3) . . ?
C24 C23 H23 107.8 . . ?
C25 C23 C18 114.0(3) . . ?
C25 C23 H23 107.8 . . ?
C25 C23 C24 109.7(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26 107.0 . . ?
C22 C26 C27 111.8(3) . . ?
C22 C26 C28 113.9(3) . . ?
C27 C26 H26 107.0 . . ?
C28 C26 H26 107.0 . . ?
C28 C26 C27 109.8(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 C29 112.3(9) . . ?
C31 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C30 C31 C31 106.6(10) . 7_556 ?
C30 C31 H31A 110.4 . . ?
C30 C31 H31B 110.4 . . ?
C31 C31 H31A 110.4 7_556 . ?
C31 C31 H31B 110.4 7_556 . ?
H31A C31 H31B 108.6 . . ?
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 2.344(2) . ?
Ca1 N1 2.349(3) . ?
Ca1 N2 2.386(3) 2_656 ?
Ca1 N2 2.700(3) . ?
Si1 O1 1.673(3) . ?
Si1 N1 1.685(3) . ?
Si1 C1 1.873(4) . ?
Si1 C2 1.869(5) . ?
Si2 Ca1 3.5656(11) 2_656 ?
Si2 O1 1.657(3) . ?
Si2 N2 1.700(3) . ?
Si2 C3 1.862(3) . ?
Si2 C4 1.864(4) . ?
N1 C5 1.416(5) . ?
N2 Ca1 2.386(3) 2_656 ?
N2 C17 1.425(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.431(6) . ?
C5 C10 1.427(6) . ?
C6 C7 1.394(6) . ?
C6 C11 1.508(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(7) . ?
C10 C14 1.527(7) . ?
C11 H11 1.0000 . ?
C11 C12 1.534(6) . ?
C11 C13 1.551(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14 1.0000 . ?
C14 C15 1.539(7) . ?
C14 C16 1.526(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Ca1 3.010(3) 2_656 ?
C17 C18 1.409(5) . ?
C17 C22 1.426(5) . ?
C18 C19 1.402(5) . ?
C18 C23 1.525(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.384(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.400(5) . ?
C22 C26 1.509(6) . ?
C23 H23 1.0000 . ?
C23 C24 1.550(5) . ?
C23 C25 1.522(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.542(5) . ?
C26 C28 1.535(5) . ?
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 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C30 1.507(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.449(12) . ?
C31 C31 1.571(15) 7_556 ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 Si2 O1 Ca1 38.24(10) 2_656 . . . ?
Ca1 Si2 O1 Si1 174.6(3) 2_656 . . . ?
Ca1 Si2 N2 Ca1 -95.20(15) 2_656 . . . ?
Ca1 Si2 N2 C17 134.5(4) 2_656 . . . ?
Ca1 N1 C5 C6 -105.1(4) . . . . ?
Ca1 N1 C5 C10 72.1(5) . . . . ?
Ca1 N2 C17 Ca1 102.05(19) . . . 2_656 ?
Ca1 N2 C17 C18 156.7(2) . . . . ?
Ca1 N2 C17 C18 54.7(3) 2_656 . . . ?
Ca1 N2 C17 C22 -19.6(4) . . . . ?
Ca1 N2 C17 C22 -121.7(3) 2_656 . . . ?
Ca1 C17 C18 C19 -129.3(3) 2_656 . . . ?
Ca1 C17 C18 C23 54.8(3) 2_656 . . . ?
Ca1 C17 C22 C21 105.8(3) 2_656 . . . ?
Ca1 C17 C22 C26 -73.9(4) 2_656 . . . ?
Si1 N1 C5 C6 85.1(4) . . . . ?
Si1 N1 C5 C10 -97.7(4) . . . . ?
Si2 N2 C17 Ca1 -141.3(3) . . . 2_656 ?
Si2 N2 C17 C18 -86.6(4) . . . . ?
Si2 N2 C17 C22 97.0(3) . . . . ?
O1 Si1 N1 Ca1 4.16(14) . . . . ?
O1 Si1 N1 C5 177.4(3) . . . . ?
O1 Si2 N2 Ca1 93.32(17) . . . 2_656 ?
O1 Si2 N2 Ca1 -1.88(12) . . . . ?
O1 Si2 N2 C17 -132.1(3) . . . . ?
N1 Si1 O1 Ca1 -4.17(14) . . . . ?
N1 Si1 O1 Si2 -141.9(3) . . . . ?
N1 C5 C6 C7 178.7(4) . . . . ?
N1 C5 C6 C11 -0.9(6) . . . . ?
N1 C5 C10 C9 -179.3(4) . . . . ?
N1 C5 C10 C14 1.5(6) . . . . ?
N2 Si2 O1 Ca1 2.24(14) . . . . ?
N2 Si2 O1 Si1 138.6(3) . . . . ?
N2 C17 C18 C19 -168.7(3) . . . . ?
N2 C17 C18 C23 15.4(5) . . . . ?
N2 C17 C22 C21 168.0(3) . . . . ?
N2 C17 C22 C26 -11.7(4) . . . . ?
C1 Si1 O1 Ca1 117.99(19) . . . . ?
C1 Si1 O1 Si2 -19.8(4) . . . . ?
C1 Si1 N1 Ca1 -111.7(2) . . . . ?
C1 Si1 N1 C5 61.6(4) . . . . ?
C2 Si1 O1 Ca1 -129.16(17) . . . . ?
C2 Si1 O1 Si2 93.1(3) . . . . ?
C2 Si1 N1 Ca1 116.5(2) . . . . ?
C2 Si1 N1 C5 -70.2(4) . . . . ?
C3 Si2 O1 Ca1 -117.97(15) . . . . ?
C3 Si2 O1 Si1 18.4(4) . . . . ?
C3 Si2 N2 Ca1 -148.28(18) . . . 2_656 ?
C3 Si2 N2 Ca1 116.52(16) . . . . ?
C3 Si2 N2 C17 -13.7(4) . . . . ?
C4 Si2 O1 Ca1 122.19(16) . . . . ?
C4 Si2 O1 Si1 -101.4(3) . . . . ?
C4 Si2 N2 Ca1 -114.12(16) . . . . ?
C4 Si2 N2 Ca1 -18.9(2) . . . 2_656 ?
C4 Si2 N2 C17 115.6(3) . . . . ?
C5 C6 C7 C8 0.0(7) . . . . ?
C5 C6 C11 C12 117.6(4) . . . . ?
C5 C6 C11 C13 -118.9(4) . . . . ?
C5 C10 C14 C15 113.9(5) . . . . ?
C5 C10 C14 C16 -122.0(5) . . . . ?
C6 C5 C10 C9 -2.0(6) . . . . ?
C6 C5 C10 C14 178.7(4) . . . . ?
C6 C7 C8 C9 -0.8(9) . . . . ?
C7 C6 C11 C12 -62.1(5) . . . . ?
C7 C6 C11 C13 61.4(5) . . . . ?
C7 C8 C9 C10 0.2(9) . . . . ?
C8 C9 C10 C5 1.2(8) . . . . ?
C8 C9 C10 C14 -179.5(5) . . . . ?
C9 C10 C14 C15 -65.4(6) . . . . ?
C9 C10 C14 C16 58.7(6) . . . . ?
C10 C5 C6 C7 1.4(6) . . . . ?
C10 C5 C6 C11 -178.2(4) . . . . ?
C11 C6 C7 C8 179.6(5) . . . . ?
C17 C18 C19 C20 -1.9(5) . . . . ?
C17 C18 C23 C24 101.8(4) . . . . ?
C17 C18 C23 C25 -134.9(4) . . . . ?
C17 C22 C26 C27 102.9(3) . . . . ?
C17 C22 C26 C28 -131.9(3) . . . . ?
C18 C17 C22 C21 -8.5(4) . . . . ?
C18 C17 C22 C26 171.8(3) . . . . ?
C18 C19 C20 C21 -3.4(6) . . . . ?
C19 C18 C23 C24 -74.2(5) . . . . ?
C19 C18 C23 C25 49.1(5) . . . . ?
C19 C20 C21 C22 2.6(6) . . . . ?
C20 C21 C22 C17 3.4(5) . . . . ?
C20 C21 C22 C26 -176.9(3) . . . . ?
C21 C22 C26 C27 -76.8(4) . . . . ?
C21 C22 C26 C28 48.4(4) . . . . ?
C22 C17 C18 C19 7.7(5) . . . . ?
C22 C17 C18 C23 -168.2(3) . . . . ?
C23 C18 C19 C20 174.3(3) . . . . ?
C29 C30 C31 C31 -71.6(13) . . . 7_556 ?
