#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002812.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_7002812
loop_
_publ_author_name
'Poirier, Valentin'
'Roisnel, Thierry'
'Carpentier, Jean-François'
'Sarazin, Yann'
_publ_section_title
;
 Versatile catalytic systems based on complexes of zinc, magnesium and
 calcium supported by a bulky bis(morpholinomethyl)phenoxy ligand for
 the large-scale immortal ring-opening polymerisation of cyclic esters
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9820
_journal_page_last               9827
_journal_paper_doi               10.1039/b917799j
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H98 Ca2 N6 O6 Si4'
_chemical_formula_sum            'C52 H98 Ca2 N6 O6 Si4'
_chemical_formula_weight         1095.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-05-25T16:52:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                114.588(2)
_cell_angle_beta                 104.771(2)
_cell_angle_gamma                104.561(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5186(6)
_cell_length_b                   13.0169(8)
_cell_length_c                   14.3156(8)
_cell_measurement_reflns_used    8976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.77
_cell_measurement_wavelength     0.71073
_cell_volume                     1574.57(17)
_computing_cell_refinement       'Bruker SMART, 2006'
_computing_data_collection       'Bruker SMART, 2006'
_computing_data_reduction        'Bruker SAINT, 2006'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20185
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0344P)²+0.8216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                6445
_reflns_number_total             7101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917799j.txt
_cod_data_source_block           100K
_cod_original_cell_volume        1574.57(16)
_cod_database_code               7002812
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.01813(4) -0.01112(3) 0.62268(3) 0.01867(9) Uani 1 1 d . . .
N1 N 0.16283(16) -0.08879(13) 0.69713(12) 0.0235(3) Uani 1 1 d . . .
Si1 Si 0.13802(6) -0.23945(4) 0.63247(4) 0.02382(12) Uani 1 1 d . . .
C2 C 0.2278(2) -0.27467(19) 0.53159(16) 0.0349(5) Uani 1 1 d . . .
H2A H 0.1988 -0.2446 0.4808 0.052 Uiso 1 1 calc R . .
H2B H 0.1987 -0.3642 0.4876 0.052 Uiso 1 1 calc R . .
H2C H 0.3325 -0.2336 0.574 0.052 Uiso 1 1 calc R . .
C3 C -0.0594(2) -0.34191(18) 0.55139(17) 0.0382(5) Uani 1 1 d . . .
H3A H -0.1051 -0.3364 0.604 0.057 Uiso 1 1 calc R . .
H3B H -0.0724 -0.4276 0.5061 0.057 Uiso 1 1 calc R . .
H3C H -0.1037 -0.3152 0.5018 0.057 Uiso 1 1 calc R . .
C4 C 0.2065(3) -0.2932(2) 0.73053(17) 0.0435(5) Uani 1 1 d . . .
H4A H 0.3097 -0.2426 0.7765 0.065 Uiso 1 1 calc R . .
H4B H 0.1905 -0.38 0.6866 0.065 Uiso 1 1 calc R . .
H4C H 0.155 -0.2849 0.7797 0.065 Uiso 1 1 calc R . .
Si2 Si 0.30416(5) 0.02449(4) 0.81977(4) 0.02253(12) Uani 1 1 d . . .
C5 C 0.4847(2) 0.03118(19) 0.81809(17) 0.0340(4) Uani 1 1 d . . .
H5A H 0.4917 -0.0466 0.8061 0.051 Uiso 1 1 calc R . .
H5B H 0.5614 0.0999 0.8902 0.051 Uiso 1 1 calc R . .
H5C H 0.495 0.0438 0.757 0.051 Uiso 1 1 calc R . .
C6 C 0.2987(3) 0.0170(2) 0.94721(16) 0.0410(5) Uani 1 1 d . . .
H6A H 0.2095 0.0208 0.9542 0.061 Uiso 1 1 calc R . .
H6B H 0.3815 0.0869 1.0147 0.061 Uiso 1 1 calc R . .
H6C H 0.3023 -0.0607 0.9391 0.061 Uiso 1 1 calc R . .
C7 C 0.3061(2) 0.17982(17) 0.84757(16) 0.0332(4) Uani 1 1 d . . .
H7A H 0.3195 0.1928 0.7875 0.05 Uiso 1 1 calc R . .
H7B H 0.3852 0.245 0.92 0.05 Uiso 1 1 calc R . .
H7C H 0.2145 0.1824 0.8497 0.05 Uiso 1 1 calc R . .
O11 O 0.11286(12) 0.12458(10) 0.57315(9) 0.0207(2) Uani 1 1 d . . .
C12 C 0.23535(17) 0.22674(15) 0.61841(13) 0.0200(3) Uani 1 1 d . . .
C13 C 0.24995(18) 0.34467(16) 0.69594(13) 0.0212(3) Uani 1 1 d . . .
C14 C 0.37131(18) 0.44934(16) 0.73382(13) 0.0214(3) Uani 1 1 d . A .
H14 H 0.3778 0.528 0.7847 0.026 Uiso 1 1 calc R . .
C15 C 0.48433(18) 0.44336(16) 0.69987(13) 0.0213(3) Uani 1 1 d . . .
C16 C 0.47238(18) 0.32523(16) 0.62869(13) 0.0223(4) Uani 1 1 d . A .
H16 H 0.5491 0.3174 0.6068 0.027 Uiso 1 1 calc R . .
C17 C 0.35222(18) 0.21836(16) 0.58853(13) 0.0203(3) Uani 1 1 d . . .
C21A C 0.61082(19) 0.56174(18) 0.73797(15) 0.0276(4) Uani 0.536(5) 1 d P A 1
C22A C 0.6927(5) 0.6343(5) 0.8702(3) 0.0416(12) Uani 0.536(5) 1 d P A 1
H22A H 0.7341 0.5845 0.8928 0.062 Uiso 0.536(5) 1 calc PR A 1
H22B H 0.625 0.6506 0.9045 0.062 Uiso 0.536(5) 1 calc PR A 1
H22C H 0.7698 0.7128 0.8953 0.062 Uiso 0.536(5) 1 calc PR A 1
C23A C 0.5571(4) 0.6604(4) 0.7175(4) 0.0410(11) Uani 0.536(5) 1 d P A 1
H23A H 0.6409 0.7361 0.7459 0.062 Uiso 0.536(5) 1 calc PR A 1
H23B H 0.4957 0.6801 0.7575 0.062 Uiso 0.536(5) 1 calc PR A 1
H23C H 0.5024 0.6244 0.6368 0.062 Uiso 0.536(5) 1 calc PR A 1
C24A C 0.7178(4) 0.5503(4) 0.6894(4) 0.0375(12) Uani 0.536(5) 1 d P A 1
H24A H 0.7582 0.4956 0.7038 0.056 Uiso 0.536(5) 1 calc PR A 1
H24B H 0.795 0.6321 0.724 0.056 Uiso 0.536(5) 1 calc PR A 1
H24C H 0.6713 0.5156 0.608 0.056 Uiso 0.536(5) 1 calc PR A 1
C21B C 0.61082(19) 0.56174(18) 0.73797(15) 0.0276(4) Uani 0.464(5) 1 d P A 2
C22B C 0.6313(7) 0.6627(5) 0.8380(6) 0.060(2) Uani 0.464(5) 1 d P A 2
H22D H 0.5491 0.6853 0.8251 0.09 Uiso 0.464(5) 1 calc PR A 2
H22E H 0.7196 0.733 0.8627 0.09 Uiso 0.464(5) 1 calc PR A 2
H22F H 0.6396 0.6405 0.8961 0.09 Uiso 0.464(5) 1 calc PR A 2
C23B C 0.5806(6) 0.5712(6) 0.6326(5) 0.063(2) Uani 0.464(5) 1 d P A 2
H23D H 0.4914 0.5836 0.6139 0.094 Uiso 0.464(5) 1 calc PR A 2
H23E H 0.5703 0.4948 0.5699 0.094 Uiso 0.464(5) 1 calc PR A 2
H23F H 0.6605 0.6414 0.6464 0.094 Uiso 0.464(5) 1 calc PR A 2
C24B C 0.7513(4) 0.5326(4) 0.7554(4) 0.0321(11) Uani 0.464(5) 1 d P A 2
H24D H 0.8352 0.6062 0.7795 0.048 Uiso 0.464(5) 1 calc PR A 2
H24E H 0.7383 0.4642 0.6843 0.048 Uiso 0.464(5) 1 calc PR A 2
H24F H 0.7664 0.5095 0.813 0.048 Uiso 0.464(5) 1 calc PR A 2
C31 C 0.34419(18) 0.09291(16) 0.51123(14) 0.0223(4) Uani 1 1 d . A .
H31A H 0.44 0.1012 0.5104 0.027 Uiso 1 1 calc R . .
H31B H 0.3178 0.0374 0.5403 0.027 Uiso 1 1 calc R . .
N32 N 0.23709(15) 0.03715(12) 0.39493(11) 0.0199(3) Uani 1 1 d . . .
C33 C 0.22073(19) -0.09053(15) 0.32351(14) 0.0240(4) Uani 1 1 d . . .
H33A H 0.1755 -0.145 0.3483 0.029 Uiso 1 1 calc R . .
H33B H 0.3161 -0.0918 0.3295 0.029 Uiso 1 1 calc R . .
C34 C 0.1253(2) -0.13597(16) 0.20129(15) 0.0267(4) Uani 1 1 d . . .
H34A H 0.1859 -0.1292 0.1596 0.032 Uiso 1 1 calc R A .
H34B H 0.0586 -0.2238 0.1634 0.032 Uiso 1 1 calc R . .
O35 O 0.04471(14) -0.06134(11) 0.20186(10) 0.0258(3) Uani 1 1 d . . .
C36 C 0.1425(2) 0.05987(16) 0.23460(14) 0.0275(4) Uani 1 1 d . . .
H36A H 0.0939 0.1173 0.2494 0.033 Uiso 1 1 calc R A .
H36B H 0.1714 0.055 0.1728 0.033 Uiso 1 1 calc R . .
C37 C 0.2768(2) 0.10877(16) 0.34145(14) 0.0236(4) Uani 1 1 d . A .
H37A H 0.3578 0.0973 0.3216 0.028 Uiso 1 1 calc R . .
H37B H 0.3065 0.198 0.3935 0.028 Uiso 1 1 calc R . .
C41 C 0.12889(19) 0.35706(16) 0.73269(14) 0.0258(4) Uani 1 1 d . . .
H41A H 0.0497 0.3488 0.6713 0.031 Uiso 1 1 calc R . .
H41B H 0.091 0.2888 0.7457 0.031 Uiso 1 1 calc R . .
N42 N 0.17416(15) 0.47521(13) 0.83536(12) 0.0235(3) Uani 1 1 d . . .
C43 C 0.2584(2) 0.47899(16) 0.93592(14) 0.0265(4) Uani 1 1 d . . .
H43A H 0.3442 0.4641 0.9289 0.032 Uiso 1 1 calc R . .
H43B H 0.1998 0.4131 0.944 0.032 Uiso 1 1 calc R . .
C44 C 0.3050(2) 0.60431(16) 1.03896(15) 0.0283(4) Uani 1 1 d . . .
H44A H 0.3627 0.6066 1.1069 0.034 Uiso 1 1 calc R . .
H44B H 0.3665 0.6696 1.0318 0.034 Uiso 1 1 calc R . .
O45 O 0.18346(15) 0.62834(12) 1.05147(10) 0.0315(3) Uani 1 1 d . . .
C46 C 0.1001(2) 0.62449(18) 0.95364(16) 0.0321(4) Uani 1 1 d . . .
H46A H 0.1586 0.6908 0.946 0.038 Uiso 1 1 calc R . .
H46B H 0.0153 0.6402 0.9622 0.038 Uiso 1 1 calc R . .
C47 C 0.0497(2) 0.50021(17) 0.84761(15) 0.0276(4) Uani 1 1 d . . .
H47A H -0.0141 0.434 0.8524 0.033 Uiso 1 1 calc R . .
H47B H -0.0056 0.5014 0.7811 0.033 Uiso 1 1 calc R . .
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 0 '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 0.006 '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
_geom_angle_publ_flag
O11 Ca1 N1 118.89(5) . . ?
O11 Ca1 O11 78.32(4) . 2_556 ?
N1 Ca1 O11 116.81(5) . 2_556 ?
O11 Ca1 N32 111.87(4) . 2_556 ?
N1 Ca1 N32 128.88(5) . 2_556 ?
O11 Ca1 N32 78.09(4) 2_556 2_556 ?
O11 Ca1 O35 120.93(4) . 2_556 ?
N1 Ca1 O35 89.70(5) . 2_556 ?
O11 Ca1 O35 135.75(4) 2_556 2_556 ?
N32 Ca1 O35 58.01(4) 2_556 2_556 ?
O11 Ca1 C36 145.97(4) . 2_556 ?
N1 Ca1 C36 83.07(5) . 2_556 ?
O11 Ca1 C36 116.67(5) 2_556 2_556 ?
N32 Ca1 C36 49.46(5) 2_556 2_556 ?
O35 Ca1 C36 27.43(4) 2_556 2_556 ?
O11 Ca1 C12 99.27(4) . 2_556 ?
N1 Ca1 C12 110.86(5) . 2_556 ?
O11 Ca1 C12 21.74(4) 2_556 2_556 ?
N32 Ca1 C12 64.48(4) 2_556 2_556 ?
O35 Ca1 C12 118.18(4) 2_556 2_556 ?
C36 Ca1 C12 95.75(5) 2_556 2_556 ?
O11 Ca1 C33 95.90(4) . 2_556 ?
N1 Ca1 C33 135.98(5) . 2_556 ?
O11 Ca1 C33 94.80(4) 2_556 2_556 ?
N32 Ca1 C33 26.40(4) 2_556 2_556 ?
O35 Ca1 C33 47.47(4) 2_556 2_556 ?
C36 Ca1 C33 54.51(5) 2_556 2_556 ?
C12 Ca1 C33 86.96(4) 2_556 2_556 ?
O11 Ca1 Si2 103.37(3) . . ?
N1 Ca1 Si2 28.20(4) . . ?
O11 Ca1 Si2 140.66(3) 2_556 . ?
N32 Ca1 Si2 133.04(3) 2_556 . ?
O35 Ca1 Si2 77.69(3) 2_556 . ?
C36 Ca1 Si2 84.13(4) 2_556 . ?
C12 Ca1 Si2 138.97(3) 2_556 . ?
C33 Ca1 Si2 123.59(3) 2_556 . ?
O11 Ca1 Si1 125.75(3) . . ?
N1 Ca1 Si1 23.34(4) . . ?
O11 Ca1 Si1 95.05(3) 2_556 . ?
N32 Ca1 Si1 119.28(3) 2_556 . ?
O35 Ca1 Si1 101.27(3) 2_556 . ?
C36 Ca1 Si1 85.09(4) 2_556 . ?
C12 Ca1 Si1 87.52(3) 2_556 . ?
C33 Ca1 Si1 138.33(4) 2_556 . ?
Si2 Ca1 Si1 51.501(13) . . ?
O11 Ca1 Ca1 39.97(3) . 2_556 ?
N1 Ca1 Ca1 127.01(4) . 2_556 ?
O11 Ca1 Ca1 38.35(3) 2_556 2_556 ?
N32 Ca1 Ca1 95.78(3) 2_556 2_556 ?
O35 Ca1 Ca1 142.70(3) 2_556 2_556 ?
C36 Ca1 Ca1 145.04(4) 2_556 2_556 ?
C12 Ca1 Ca1 59.53(3) 2_556 2_556 ?
C33 Ca1 Ca1 96.89(3) 2_556 2_556 ?
Si2 Ca1 Ca1 130.827(17) . 2_556 ?
Si1 Ca1 Ca1 115.336(15) . 2_556 ?
Si2 N1 Si1 123.92(9) . . ?
Si2 N1 Ca1 111.85(7) . . ?
Si1 N1 Ca1 124.09(8) . . ?
N1 Si1 C3 110.05(8) . . ?
N1 Si1 C4 114.70(8) . . ?
C3 Si1 C4 105.07(11) . . ?
N1 Si1 C2 111.98(9) . . ?
C3 Si1 C2 108.17(9) . . ?
C4 Si1 C2 106.45(10) . . ?
C3 Si1 Ca1 82.62(7) . . ?
C4 Si1 Ca1 141.84(7) . . ?
C2 Si1 Ca1 106.28(7) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 Si2 C6 114.37(9) . . ?
N1 Si2 C7 109.47(8) . . ?
C6 Si2 C7 105.80(10) . . ?
N1 Si2 C5 113.63(8) . . ?
C6 Si2 C5 107.46(10) . . ?
C7 Si2 C5 105.46(9) . . ?
C6 Si2 Ca1 122.98(8) . . ?
C7 Si2 Ca1 69.68(6) . . ?
C5 Si2 Ca1 128.98(7) . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 O11 Ca1 137.07(10) . . ?
C12 O11 Ca1 118.48(9) . 2_556 ?
Ca1 O11 Ca1 101.68(4) . 2_556 ?
O11 C12 C13 121.20(14) . . ?
O11 C12 C17 120.99(14) . . ?
C13 C12 C17 117.81(15) . . ?
C13 C12 Ca1 131.67(11) . 2_556 ?
C17 C12 Ca1 97.13(9) . 2_556 ?
C14 C13 C12 120.16(15) . . ?
C14 C13 C41 120.33(15) . . ?
C12 C13 C41 119.43(15) . . ?
C13 C14 C15 122.64(15) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C16 C15 C14 116.44(15) . . ?
C16 C15 C21A 122.98(15) . . ?
C14 C15 C21A 120.57(15) . . ?
C17 C16 C15 122.51(15) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C12 120.20(15) . . ?
C16 C17 C31 120.45(15) . . ?
C12 C17 C31 119.35(15) . . ?
C24A C21A C15 118.1(2) . . ?
C24A C21A C22A 108.1(3) . . ?
C15 C21A C22A 109.2(2) . . ?
C24A C21A C23A 106.2(3) . . ?
C15 C21A C23A 111.95(19) . . ?
C22A C21A C23A 101.9(3) . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
H23D C23B H23E 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N32 C31 C17 111.68(13) . . ?
N32 C31 H31A 109.3 . . ?
C17 C31 H31A 109.3 . . ?
N32 C31 H31B 109.3 . . ?
C17 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C33 N32 C37 108.11(12) . . ?
C33 N32 C31 110.66(13) . . ?
C37 N32 C31 112.51(13) . . ?
C33 N32 Ca1 103.52(10) . 2_556 ?
C37 N32 Ca1 106.74(10) . 2_556 ?
C31 N32 Ca1 114.72(9) . 2_556 ?
N32 C33 C34 107.92(14) . . ?
N32 C33 Ca1 50.07(8) . 2_556 ?
C34 C33 Ca1 83.30(9) . 2_556 ?
N32 C33 H33A 110.1 . . ?
C34 C33 H33A 110.1 . . ?
Ca1 C33 H33A 79.4 2_556 . ?
N32 C33 H33B 110.1 . . ?
C34 C33 H33B 110.1 . . ?
Ca1 C33 H33B 159.8 2_556 . ?
H33A C33 H33B 108.4 . . ?
O35 C34 C33 108.82(13) . . ?
O35 C34 H34A 109.9 . . ?
C33 C34 H34A 109.9 . . ?
O35 C34 H34B 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C34 O35 C36 108.32(14) . . ?
C34 O35 Ca1 111.61(9) . 2_556 ?
C36 O35 Ca1 96.21(9) . 2_556 ?
O35 C36 C37 109.70(14) . . ?
O35 C36 Ca1 56.36(8) . 2_556 ?
C37 C36 Ca1 82.66(9) . 2_556 ?
O35 C36 H36A 109.7 . . ?
C37 C36 H36A 109.7 . . ?
Ca1 C36 H36A 74.3 2_556 . ?
O35 C36 H36B 109.7 . . ?
C37 C36 H36B 109.7 . . ?
Ca1 C36 H36B 164.8 2_556 . ?
H36A C36 H36B 108.2 . . ?
N32 C37 C36 106.88(14) . . ?
N32 C37 H37A 110.3 . . ?
C36 C37 H37A 110.3 . . ?
N32 C37 H37B 110.3 . . ?
C36 C37 H37B 110.3 . . ?
H37A C37 H37B 108.6 . . ?
N42 C41 C13 112.95(14) . . ?
N42 C41 H41A 109 . . ?
C13 C41 H41A 109 . . ?
N42 C41 H41B 109 . . ?
C13 C41 H41B 109 . . ?
H41A C41 H41B 107.8 . . ?
C43 N42 C47 109.33(13) . . ?
C43 N42 C41 112.18(14) . . ?
C47 N42 C41 110.80(13) . . ?
N42 C43 C44 109.75(15) . . ?
N42 C43 H43A 109.7 . . ?
C44 C43 H43A 109.7 . . ?
N42 C43 H43B 109.7 . . ?
C44 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
O45 C44 C43 111.05(15) . . ?
O45 C44 H44A 109.4 . . ?
C43 C44 H44A 109.4 . . ?
O45 C44 H44B 109.4 . . ?
C43 C44 H44B 109.4 . . ?
H44A C44 H44B 108 . . ?
C46 O45 C44 109.45(13) . . ?
O45 C46 C47 111.84(16) . . ?
O45 C46 H46A 109.2 . . ?
C47 C46 H46A 109.2 . . ?
O45 C46 H46B 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
N42 C47 C46 109.61(15) . . ?
N42 C47 H47A 109.7 . . ?
C46 C47 H47A 109.7 . . ?
N42 C47 H47B 109.7 . . ?
C46 C47 H47B 109.7 . . ?
H47A C47 H47B 108.2 . . ?
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 O11 2.2657(12) . ?
Ca1 N1 2.3061(14) . ?
Ca1 O11 2.3453(11) 2_556 ?
Ca1 N32 2.5517(14) 2_556 ?
Ca1 O35 2.6123(12) 2_556 ?
Ca1 C36 3.1194(18) 2_556 ?
Ca1 C12 3.2221(16) 2_556 ?
Ca1 C33 3.2352(17) 2_556 ?
Ca1 Si2 3.3331(6) . ?
Ca1 Si1 3.5474(6) . ?
Ca1 Ca1 3.5757(7) 2_556 ?
N1 Si2 1.6968(15) . ?
N1 Si1 1.6970(15) . ?
Si1 C3 1.878(2) . ?
Si1 C4 1.880(2) . ?
Si1 C2 1.8839(19) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
Si2 C6 1.882(2) . ?
Si2 C7 1.8848(19) . ?
Si2 C5 1.886(2) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
O11 C12 1.358(2) . ?
O11 Ca1 2.3453(11) 2_556 ?
C12 C13 1.410(2) . ?
C12 C17 1.415(2) . ?
C12 Ca1 3.2221(16) 2_556 ?
C13 C14 1.392(2) . ?
C13 C41 1.516(2) . ?
C14 C15 1.402(2) . ?
C14 H14 0.95 . ?
C15 C16 1.397(2) . ?
C15 C21A 1.530(2) . ?
C16 C17 1.394(2) . ?
C16 H16 0.95 . ?
C17 C31 1.509(2) . ?
C21A C24A 1.472(4) . ?
C21A C22A 1.577(4) . ?
C21A C23A 1.627(4) . ?
C22A H22A 0.98 . ?
C22A H22B 0.98 . ?
C22A H22C 0.98 . ?
C23A H23A 0.98 . ?
C23A H23B 0.98 . ?
C23A H23C 0.98 . ?
C24A H24A 0.98 . ?
C24A H24B 0.98 . ?
C24A H24C 0.98 . ?
C22B H22D 0.98 . ?
C22B H22E 0.98 . ?
C22B H22F 0.98 . ?
C23B H23D 0.98 . ?
C23B H23E 0.98 . ?
C23B H23F 0.98 . ?
C24B H24D 0.98 . ?
C24B H24E 0.98 . ?
C24B H24F 0.98 . ?
C31 N32 1.481(2) . ?
C31 H31A 0.99 . ?
C31 H31B 0.99 . ?
N32 C33 1.480(2) . ?
N32 C37 1.480(2) . ?
N32 Ca1 2.5518(14) 2_556 ?
C33 C34 1.537(2) . ?
C33 Ca1 3.2353(17) 2_556 ?
C33 H33A 0.99 . ?
C33 H33B 0.99 . ?
C34 O35 1.440(2) . ?
C34 H34A 0.99 . ?
C34 H34B 0.99 . ?
O35 C36 1.446(2) . ?
O35 Ca1 2.6123(12) 2_556 ?
C36 C37 1.542(2) . ?
C36 Ca1 3.1194(18) 2_556 ?
C36 H36A 0.99 . ?
C36 H36B 0.99 . ?
C37 H37A 0.99 . ?
C37 H37B 0.99 . ?
C41 N42 1.465(2) . ?
C41 H41A 0.99 . ?
C41 H41B 0.99 . ?
N42 C43 1.459(2) . ?
N42 C47 1.461(2) . ?
C43 C44 1.518(2) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 O45 1.427(2) . ?
C44 H44A 0.99 . ?
C44 H44B 0.99 . ?
O45 C46 1.423(2) . ?
C46 C47 1.522(2) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
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
O11 Ca1 N1 Si2 61.93(9) . . . . ?
O11 Ca1 N1 Si2 153.06(6) 2_556 . . . ?
N32 Ca1 N1 Si2 -110.59(8) 2_556 . . . ?
O35 Ca1 N1 Si2 -63.81(8) 2_556 . . . ?
C36 Ca1 N1 Si2 -90.50(8) 2_556 . . . ?
C12 Ca1 N1 Si2 175.97(7) 2_556 . . . ?
C33 Ca1 N1 Si2 -75.81(10) 2_556 . . . ?
Si1 Ca1 N1 Si2 175.83(16) . . . . ?
Ca1 Ca1 N1 Si2 109.07(7) 2_556 . . . ?
O11 Ca1 N1 Si1 -113.90(9) . . . . ?
O11 Ca1 N1 Si1 -22.77(11) 2_556 . . . ?
N32 Ca1 N1 Si1 73.57(11) 2_556 . . . ?
O35 Ca1 N1 Si1 120.35(9) 2_556 . . . ?
C36 Ca1 N1 Si1 93.67(10) 2_556 . . . ?
C12 Ca1 N1 Si1 0.13(11) 2_556 . . . ?
C33 Ca1 N1 Si1 108.35(9) 2_556 . . . ?
Si2 Ca1 N1 Si1 -175.83(16) . . . . ?
Ca1 Ca1 N1 Si1 -66.77(11) 2_556 . . . ?
Si2 N1 Si1 C3 150.28(11) . . . . ?
Ca1 N1 Si1 C3 -34.38(12) . . . . ?
Si2 N1 Si1 C4 32.08(15) . . . . ?
Ca1 N1 Si1 C4 -152.58(11) . . . . ?
Si2 N1 Si1 C2 -89.38(12) . . . . ?
Ca1 N1 Si1 C2 85.96(11) . . . . ?
Si2 N1 Si1 Ca1 -175.34(18) . . . . ?
O11 Ca1 Si1 N1 80.47(10) . . . . ?
O11 Ca1 Si1 N1 159.71(10) 2_556 . . . ?
N32 Ca1 Si1 N1 -121.12(10) 2_556 . . . ?
O35 Ca1 Si1 N1 -61.63(10) 2_556 . . . ?
C36 Ca1 Si1 N1 -83.89(10) 2_556 . . . ?
C12 Ca1 Si1 N1 -179.87(10) 2_556 . . . ?
C33 Ca1 Si1 N1 -97.25(11) 2_556 . . . ?
Si2 Ca1 Si1 N1 2.51(10) . . . . ?
Ca1 Ca1 Si1 N1 125.72(10) 2_556 . . . ?
O11 Ca1 Si1 C3 -131.87(8) . . . . ?
N1 Ca1 Si1 C3 147.66(12) . . . . ?
O11 Ca1 Si1 C3 -52.63(7) 2_556 . . . ?
N32 Ca1 Si1 C3 26.54(8) 2_556 . . . ?
O35 Ca1 Si1 C3 86.03(7) 2_556 . . . ?
C36 Ca1 Si1 C3 63.77(8) 2_556 . . . ?
C12 Ca1 Si1 C3 -32.22(7) 2_556 . . . ?
C33 Ca1 Si1 C3 50.40(8) 2_556 . . . ?
Si2 Ca1 Si1 C3 150.17(7) . . . . ?
Ca1 Ca1 Si1 C3 -86.62(7) 2_556 . . . ?
O11 Ca1 Si1 C4 123.10(14) . . . . ?
N1 Ca1 Si1 C4 42.63(16) . . . . ?
O11 Ca1 Si1 C4 -157.66(14) 2_556 . . . ?
N32 Ca1 Si1 C4 -78.49(14) 2_556 . . . ?
O35 Ca1 Si1 C4 -19.00(14) 2_556 . . . ?
C36 Ca1 Si1 C4 -41.26(14) 2_556 . . . ?
C12 Ca1 Si1 C4 -137.25(14) 2_556 . . . ?
C33 Ca1 Si1 C4 -54.63(14) 2_556 . . . ?
Si2 Ca1 Si1 C4 45.14(13) . . . . ?
Ca1 Ca1 Si1 C4 168.35(13) 2_556 . . . ?
O11 Ca1 Si1 C2 -25.03(8) . . . . ?
N1 Ca1 Si1 C2 -105.50(12) . . . . ?
O11 Ca1 Si1 C2 54.21(8) 2_556 . . . ?
N32 Ca1 Si1 C2 133.38(8) 2_556 . . . ?
O35 Ca1 Si1 C2 -167.13(8) 2_556 . . . ?
C36 Ca1 Si1 C2 170.61(8) 2_556 . . . ?
C12 Ca1 Si1 C2 74.62(8) 2_556 . . . ?
C33 Ca1 Si1 C2 157.24(8) 2_556 . . . ?
Si2 Ca1 Si1 C2 -102.99(7) . . . . ?
Ca1 Ca1 Si1 C2 20.22(7) 2_556 . . . ?
Si1 N1 Si2 C6 -71.21(13) . . . . ?
Ca1 N1 Si2 C6 112.95(10) . . . . ?
Si1 N1 Si2 C7 170.30(11) . . . . ?
Ca1 N1 Si2 C7 -5.54(11) . . . . ?
Si1 N1 Si2 C5 52.69(14) . . . . ?
Ca1 N1 Si2 C5 -123.15(9) . . . . ?
Si1 N1 Si2 Ca1 175.84(16) . . . . ?
O11 Ca1 Si2 N1 -127.44(9) . . . . ?
O11 Ca1 Si2 N1 -39.64(10) 2_556 . . . ?
N32 Ca1 Si2 N1 94.34(9) 2_556 . . . ?
O35 Ca1 Si2 N1 113.30(9) 2_556 . . . ?
C36 Ca1 Si2 N1 86.27(9) 2_556 . . . ?
C12 Ca1 Si2 N1 -5.74(9) 2_556 . . . ?
C33 Ca1 Si2 N1 126.02(9) 2_556 . . . ?
Si1 Ca1 Si2 N1 -2.11(8) . . . . ?
Ca1 Ca1 Si2 N1 -94.13(8) 2_556 . . . ?
O11 Ca1 Si2 C6 143.06(9) . . . . ?
N1 Ca1 Si2 C6 -89.50(12) . . . . ?
O11 Ca1 Si2 C6 -129.14(10) 2_556 . . . ?
N32 Ca1 Si2 C6 4.84(10) 2_556 . . . ?
O35 Ca1 Si2 C6 23.80(9) 2_556 . . . ?
C36 Ca1 Si2 C6 -3.23(9) 2_556 . . . ?
C12 Ca1 Si2 C6 -95.25(10) 2_556 . . . ?
C33 Ca1 Si2 C6 36.52(10) 2_556 . . . ?
Si1 Ca1 Si2 C6 -91.61(9) . . . . ?
Ca1 Ca1 Si2 C6 176.36(9) 2_556 . . . ?
O11 Ca1 Si2 C7 46.99(8) . . . . ?
N1 Ca1 Si2 C7 174.43(11) . . . . ?
O11 Ca1 Si2 C7 134.79(9) 2_556 . . . ?
N32 Ca1 Si2 C7 -91.23(9) 2_556 . . . ?
O35 Ca1 Si2 C7 -72.27(8) 2_556 . . . ?
C36 Ca1 Si2 C7 -99.30(8) 2_556 . . . ?
C12 Ca1 Si2 C7 168.68(9) 2_556 . . . ?
C33 Ca1 Si2 C7 -59.55(8) 2_556 . . . ?
Si1 Ca1 Si2 C7 172.32(7) . . . . ?
Ca1 Ca1 Si2 C7 80.29(8) 2_556 . . . ?
O11 Ca1 Si2 C5 -46.80(9) . . . . ?
N1 Ca1 Si2 C5 80.63(12) . . . . ?
O11 Ca1 Si2 C5 41.00(10) 2_556 . . . ?
N32 Ca1 Si2 C5 174.97(9) 2_556 . . . ?
O35 Ca1 Si2 C5 -166.07(9) 2_556 . . . ?
C36 Ca1 Si2 C5 166.91(9) 2_556 . . . ?
C12 Ca1 Si2 C5 74.89(10) 2_556 . . . ?
C33 Ca1 Si2 C5 -153.35(9) 2_556 . . . ?
Si1 Ca1 Si2 C5 78.53(9) . . . . ?
Ca1 Ca1 Si2 C5 -13.50(9) 2_556 . . . ?
N1 Ca1 O11 C12 -45.25(15) . . . . ?
O11 Ca1 O11 C12 -159.57(16) 2_556 . . . ?
N32 Ca1 O11 C12 128.49(14) 2_556 . . . ?
O35 Ca1 O11 C12 63.64(15) 2_556 . . . ?
C36 Ca1 O11 C12 79.57(17) 2_556 . . . ?
C12 Ca1 O11 C12 -165.40(12) 2_556 . . . ?
C33 Ca1 O11 C12 106.73(14) 2_556 . . . ?
Si2 Ca1 O11 C12 -19.87(14) . . . . ?
Si1 Ca1 O11 C12 -71.75(14) . . . . ?
Ca1 Ca1 O11 C12 -159.57(16) 2_556 . . . ?
N1 Ca1 O11 Ca1 114.32(5) . . . 2_556 ?
O11 Ca1 O11 Ca1 0 2_556 . . 2_556 ?
N32 Ca1 O11 Ca1 -71.94(5) 2_556 . . 2_556 ?
O35 Ca1 O11 Ca1 -136.79(4) 2_556 . . 2_556 ?
C36 Ca1 O11 Ca1 -120.86(8) 2_556 . . 2_556 ?
C12 Ca1 O11 Ca1 -5.83(5) 2_556 . . 2_556 ?
C33 Ca1 O11 Ca1 -93.70(5) 2_556 . . 2_556 ?
Si2 Ca1 O11 Ca1 139.70(3) . . . 2_556 ?
Si1 Ca1 O11 Ca1 87.82(4) . . . 2_556 ?
Ca1 O11 C12 C13 -83.7(2) . . . . ?
Ca1 O11 C12 C13 119.17(14) 2_556 . . . ?
Ca1 O11 C12 C17 96.79(17) . . . . ?
Ca1 O11 C12 C17 -60.33(18) 2_556 . . . ?
Ca1 O11 C12 Ca1 157.11(18) . . . 2_556 ?
O11 C12 C13 C14 -174.47(15) . . . . ?
C17 C12 C13 C14 5.0(2) . . . . ?
Ca1 C12 C13 C14 -126.07(15) 2_556 . . . ?
O11 C12 C13 C41 2.2(2) . . . . ?
C17 C12 C13 C41 -178.24(15) . . . . ?
Ca1 C12 C13 C41 50.7(2) 2_556 . . . ?
C12 C13 C14 C15 -1.4(3) . . . . ?
C41 C13 C14 C15 -178.09(16) . . . . ?
C13 C14 C15 C16 -2.6(2) . . . . ?
C13 C14 C15 C21A 176.02(16) . . . . ?
C14 C15 C16 C17 2.9(2) . . . . ?
C21A C15 C16 C17 -175.66(16) . . . . ?
C15 C16 C17 C12 0.7(3) . . . . ?
C15 C16 C17 C31 179.63(15) . . . . ?
O11 C12 C17 C16 174.79(15) . . . . ?
C13 C12 C17 C16 -4.7(2) . . . . ?
Ca1 C12 C17 C16 140.72(13) 2_556 . . . ?
O11 C12 C17 C31 -4.1(2) . . . . ?
C13 C12 C17 C31 176.37(15) . . . . ?
Ca1 C12 C17 C31 -38.19(16) 2_556 . . . ?
C16 C15 C21A C24A 5.4(3) . . . . ?
C14 C15 C21A C24A -173.1(3) . . . . ?
C16 C15 C21A C22A -118.6(3) . . . . ?
C14 C15 C21A C22A 62.9(3) . . . . ?
C16 C15 C21A C23A 129.3(2) . . . . ?
C14 C15 C21A C23A -49.3(3) . . . . ?
C16 C17 C31 N32 -109.07(17) . . . . ?
C12 C17 C31 N32 69.8(2) . . . . ?
C17 C31 N32 C33 -174.40(14) . . . . ?
C17 C31 N32 C37 64.54(17) . . . . ?
C17 C31 N32 Ca1 -57.73(16) . . . 2_556 ?
C37 N32 C33 C34 -48.48(17) . . . . ?
C31 N32 C33 C34 -172.11(14) . . . . ?
Ca1 N32 C33 C34 64.50(13) 2_556 . . . ?
C37 N32 C33 Ca1 -112.97(13) . . . 2_556 ?
C31 N32 C33 Ca1 123.40(13) . . . 2_556 ?
N32 C33 C34 O35 -20.08(19) . . . . ?
Ca1 C33 C34 O35 24.10(12) 2_556 . . . ?
C33 C34 O35 C36 72.00(16) . . . . ?
C33 C34 O35 Ca1 -32.70(16) . . . 2_556 ?
C34 O35 C36 C37 -48.89(17) . . . . ?
Ca1 O35 C36 C37 66.35(13) 2_556 . . . ?
C34 O35 C36 Ca1 -115.23(11) . . . 2_556 ?
C33 N32 C37 C36 70.62(16) . . . . ?
C31 N32 C37 C36 -166.87(13) . . . . ?
Ca1 N32 C37 C36 -40.19(13) 2_556 . . . ?
O35 C36 C37 N32 -19.61(18) . . . . ?
Ca1 C36 C37 N32 30.64(10) 2_556 . . . ?
C14 C13 C41 N42 -20.2(2) . . . . ?
C12 C13 C41 N42 163.06(16) . . . . ?
C13 C41 N42 C43 -75.65(19) . . . . ?
C13 C41 N42 C47 161.86(16) . . . . ?
C47 N42 C43 C44 -58.00(18) . . . . ?
C41 N42 C43 C44 178.67(14) . . . . ?
N42 C43 C44 O45 59.49(19) . . . . ?
C43 C44 O45 C46 -58.82(19) . . . . ?
C44 O45 C46 C47 58.29(19) . . . . ?
C43 N42 C47 C46 56.94(19) . . . . ?
C41 N42 C47 C46 -178.92(16) . . . . ?
O45 C46 C47 N42 -57.9(2) . . . . ?
