#------------------------------------------------------------------------------
#$Date: 2025-10-06 11:12:22 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302620 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/91/7719126.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_7719126
loop_
_publ_author_name
'Routh, Kousik'
'Kumar Swain, Rajesha'
'Kumar, Gaurav'
'Pradeep, Chullikkattil P.'
_publ_section_title
;
 Amine functionalized quinolinium polyoxometalates as highly active
 heterogeneous catalysts for solvent-free CO₂ cycloaddition and
 Knoevenagel condensation reactions.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12324
_journal_page_last               12339
_journal_paper_doi               10.1039/d5dt00934k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'O40 Si W12, 4(C10 H10 Cl N2), 2(C3 H7 N O), 4[C3H7NO]'
_chemical_formula_sum            'C58 H82 Cl4 N14 O46 Si W12'
_chemical_formula_weight         4087.361
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7825(3)
_cell_length_b                   27.3941(6)
_cell_length_c                   26.8909(8)
_cell_measurement_reflns_used    10836
_cell_measurement_temperature    150.03(17)
_cell_measurement_theta_max      27.9380
_cell_measurement_theta_min      2.3310
_cell_volume                     9979.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9946
_diffrn_measured_fraction_theta_max 0.8613
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  87.00   1.00   50.00    --   26.84  19.00 -60.00  119
  2  ω    -12.00  86.00   1.00   50.00    --   26.84  57.00 120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0420964000
_diffrn_orient_matrix_UB_12      0.0153215000
_diffrn_orient_matrix_UB_13      -0.0055233000
_diffrn_orient_matrix_UB_21      0.0092016000
_diffrn_orient_matrix_UB_22      0.0085117000
_diffrn_orient_matrix_UB_23      0.0253499000
_diffrn_orient_matrix_UB_31      0.0297121000
_diffrn_orient_matrix_UB_32      0.0190593000
_diffrn_orient_matrix_UB_33      -0.0069140000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.9946
_diffrn_reflns_Laue_measured_fraction_max 0.8613
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33309
_diffrn_reflns_point_group_measured_fraction_full 0.9946
_diffrn_reflns_point_group_measured_fraction_max 0.8613
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.977
_exptl_absorpt_correction_T_max  0.278
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             7449.960
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.158
_refine_diff_density_max         5.8412
_refine_diff_density_min         -3.8391
_refine_diff_density_rms         0.4945
_refine_ls_d_res_high            0.7459
_refine_ls_d_res_low             11.9029
_refine_ls_goodness_of_fit_ref   1.0609
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    88
_refine_ls_number_parameters     891
_refine_ls_number_reflns         21694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0609
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0434P)²+314.9622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -18
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              -13
_reflns_number_gt                15906
_reflns_number_total             21694
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt00934k2.cif
_cod_data_source_block           GK_HY_4_Lt_Mo
_cod_depositor_comments
'Adding full bibliography for 7719124--7719126.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_original_formula_sum        'C58 Cl4 H82 N14 O46 Si1 W12 '
_cod_database_code               7719126
_chemical_oxdiff_formula         'C184  H216  Cl16  N40  O172  Si4  W48  '
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N4(H4a,H4b), N6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C8(H8), C38(H38), C1(H1), C5(H5), C35(H35), C43(H43),
 C36(H36), C28(H28), C26(H26), C25(H25), C18(H18), C11(H11), C22(H22), C16(H16),
  C15(H15), C21(H21), C12(H12), C31(H31), C32(H32), C46(H46)
2.c X=CH2 refined with riding coordinates:
 N2(H2a,H2b), N8(H8a,H8b)
2.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C40(H40a,H40b,H40c), C20(H20a,H20b,H20c), C45(H45a,H45b,
 H45c), C44(H44a,H44b,H44c), C30(H30a,H30b,H30c), C42(H42a,H42b,H42c), C41(H41a,
 H41b,H41c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 640 electrons were 
found in a volume of 3118Å³ in 2 voids per unit cell. 
This is consistent with the presence of 4[C3H7NO] per Formula Unit 
which account for 640 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.801
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 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_refinement_flags_posn
W5 W 0.33340(4) 0.68440(2) 0.45200(2) 0.02636(13) Uani 1.000000 .
W7 W 0.25613(4) 0.70539(2) 0.32744(2) 0.02773(14) Uani 1.000000 .
W2 W 0.55599(4) 0.62116(2) 0.42596(2) 0.02730(14) Uani 1.000000 .
W8 W 0.47494(5) 0.63955(2) 0.30132(2) 0.03133(15) Uani 1.000000 .
W1 W 0.58025(5) 0.72485(2) 0.51465(2) 0.03140(15) Uani 1.000000 .
W6 W 0.28472(5) 0.79892(2) 0.40981(3) 0.03271(15) Uani 1.000000 .
W10 W 0.42260(5) 0.76414(2) 0.25240(2) 0.03349(15) Uani 1.000000 .
W12 W 0.44638(5) 0.85879(2) 0.33304(3) 0.03738(16) Uani 1.000000 .
W3 W 0.73339(5) 0.77789(3) 0.44638(3) 0.04125(18) Uani 1.000000 .
W9 W 0.70380(5) 0.67519(3) 0.35619(3) 0.03959(18) Uani 1.000000 .
W4 W 0.53501(6) 0.83887(2) 0.46948(3) 0.04027(17) Uani 1.000000 .
W11 W 0.64878(5) 0.80038(3) 0.31034(3) 0.04092(18) Uani 1.000000 .
Si1 Si 0.4982(2) 0.74130(10) 0.38340(10) 0.0036(5) Uiso 1.000000 .
Cl4 Cl -0.0126(3) 0.91982(17) 0.05122(15) 0.0441(10) Uani 1.000000 .
Cl1 Cl 0.1892(3) 0.35023(16) 0.44440(18) 0.0482(11) Uani 1.000000 .
Cl2 Cl 0.8116(4) 0.5347(2) 0.45894(19) 0.0547(12) Uani 1.000000 .
O33 O 0.3523(8) 0.6568(4) 0.3172(4) 0.033(2) Uani 1.000000 .
O4 O 0.5980(7) 0.6668(4) 0.4773(4) 0.033(2) Uani 1.000000 .
O34 O 0.4986(7) 0.5978(4) 0.3592(4) 0.033(2) Uani 1.000000 .
O8 O 0.2456(7) 0.6716(3) 0.3889(4) 0.030(2) Uani 1.000000 .
O3 O 0.7103(8) 0.7445(4) 0.5054(4) 0.042(3) Uani 1.000000 .
O7 O 0.4243(7) 0.6390(4) 0.4336(4) 0.030(2) Uani 1.000000 .
O21 O 0.3134(7) 0.7445(4) 0.2821(4) 0.032(2) Uani 1.000000 .
O5 O 0.4441(8) 0.7121(4) 0.4960(4) 0.031(2) Uani 1.000000 .
O2 O 0.5526(9) 0.7925(4) 0.5242(4) 0.039(3) Uani 1.000000 .
O16 O 0.5117(8) 0.8615(4) 0.4011(4) 0.035(2) Uiso 1.000000 .
O19 O 0.3925(8) 0.8310(5) 0.2677(4) 0.045(3) Uani 1.000000 .
O9 O 0.2676(8) 0.7473(4) 0.4534(4) 0.036(3) Uani 1.000000 .
O30 O 0.6784(8) 0.6257(4) 0.4032(4) 0.036(3) Uiso 1.000000 .
O28 O 0.7423(9) 0.7169(4) 0.4120(4) 0.040(3) Uiso 1.000000 .
O22 O 0.4668(8) 0.6989(4) 0.2637(4) 0.032(2) Uani 1.000000 .
O31 O 0.6162(8) 0.6408(4) 0.3045(4) 0.042(3) Uani 1.000000 .
O12 O 0.3389(7) 0.8336(4) 0.3587(4) 0.036(3) Uani 1.000000 .
O13 O 0.4000(8) 0.8197(4) 0.4546(4) 0.037(3) Uani 1.000000 .
O35 O 0.5721(8) 0.5673(4) 0.4558(4) 0.039(3) Uani 1.000000 .
O11 O 0.2079(8) 0.7623(4) 0.3547(4) 0.038(3) Uani 1.000000 .
O20 O 0.3732(8) 0.7639(4) 0.1890(4) 0.042(3) Uani 1.000000 .
O25 O 0.6815(8) 0.7321(4) 0.3163(4) 0.039(3) Uani 1.000000 .
O17 O 0.4125(9) 0.9173(4) 0.3205(5) 0.048(3) Uani 1.000000 .
O6 O 0.2770(8) 0.6510(4) 0.4919(4) 0.037(3) Uani 1.000000 .
O15 O 0.6745(9) 0.8346(4) 0.4699(5) 0.050(3) Uani 1.000000 .
O23 O 0.5538(8) 0.7841(4) 0.2500(5) 0.043(3) Uani 1.000000 .
O38 O 0.5023(8) 0.7777(4) 0.3356(4) 0.033(2) Uani 1.000000 .
O26 O 0.7019(8) 0.8062(4) 0.3804(4) 0.041(3) Uani 1.000000 .
O18 O 0.5764(9) 0.8589(4) 0.3135(5) 0.050(3) Uani 1.000000 .
O39 O 0.3830(7) 0.7347(3) 0.3910(4) 0.025(2) Uani 1.000000 .
O29 O 0.8143(9) 0.6546(5) 0.3443(5) 0.061(4) Uani 1.000000 .
O40 O 0.1526(8) 0.6848(4) 0.2902(4) 0.037(3) Uani 1.000000 .
O36 O 0.5416(7) 0.6883(4) 0.3704(4) 0.031(2) Uani 1.000000 .
O24 O 0.7391(9) 0.8237(4) 0.2828(5) 0.051(3) Uani 1.000000 .
O1 O 0.6064(9) 0.7064(4) 0.5760(4) 0.043(3) Uani 1.000000 .
N1 N 0.2846(9) 0.5195(4) 0.3954(4) 0.027(3) Uiso 1.000000 .
O32 O 0.4428(9) 0.5966(4) 0.2551(4) 0.044(3) Uani 1.000000 .
C9 C 0.2480(11) 0.4747(5) 0.3800(5) 0.026(3) Uiso 1.000000 .
O41 O 0.5875(10) 0.8548(5) 0.1243(5) 0.059(4) Uani 1.000000 .
O10 O 0.1976(9) 0.8389(5) 0.4220(5) 0.051(3) Uani 1.000000 .
C6 C 0.1670(10) 0.3829(5) 0.3483(6) 0.033(4) Uani 1.000000 .
H6 H 0.1402(10) 0.3525(5) 0.3381(6) 0.039(4) Uiso 1.000000 R
O27 O 0.8523(9) 0.7941(5) 0.4646(6) 0.063(4) Uani 1.000000 .
N7 N 0.1194(10) 0.8594(5) 0.2287(5) 0.038(3) Uani 1.000000 .
C39 C 0.0846(11) 0.8978(5) 0.1985(5) 0.027(3) Uiso 1.000000 .
C2 C 0.2486(11) 0.5492(6) 0.3122(6) 0.030(3) Uiso 1.000000 .
H2 H 0.2496(11) 0.5754(6) 0.2903(6) 0.036(4) Uiso 1.000000 R
C8 C 0.2418(9) 0.4379(5) 0.4155(6) 0.027(3) Uani 1.000000 .
H8 H 0.2645(9) 0.4435(5) 0.4498(6) 0.032(4) Uiso 1.000000 R
C38 C 0.0578(10) 0.8909(6) 0.1448(6) 0.030(3) Uani 1.000000 .
H38 H 0.0670(10) 0.8608(6) 0.1304(6) 0.036(4) Uiso 1.000000 R
C7 C 0.2017(11) 0.3932(5) 0.3990(6) 0.031(3) Uani 1.000000 .
N2 N 0.1778(10) 0.4991(5) 0.2433(5) 0.038(3) Uani 1.000000 .
H2a H 0.1797(10) 0.5231(5) 0.2230(5) 0.045(4) Uiso 1.000000 R
H2b H 0.1546(10) 0.4713(5) 0.2317(5) 0.045(4) Uiso 1.000000 R
C1 C 0.2836(11) 0.5557(6) 0.3612(6) 0.030(3) Uani 1.000000 .
H1 H 0.3082(11) 0.5862(6) 0.3723(6) 0.036(4) Uiso 1.000000 R
C5 C 0.1737(11) 0.4191(6) 0.3140(6) 0.032(4) Uani 1.000000 .
H5 H 0.1525(11) 0.4123(6) 0.2798(6) 0.039(4) Uiso 1.000000 R
C37 C 0.0187(12) 0.9292(6) 0.1154(6) 0.033(3) Uani 1.000000 .
C35 C 0.0391(10) 0.9827(5) 0.1851(5) 0.027(3) Uiso 1.000000 .
H35 H 0.0338(10) 1.0137(5) 0.1983(5) 0.032(4) Uiso 1.000000 R
N9 N 0.5338(13) 0.7879(7) 0.0769(6) 0.058(4) Uani 1.000000 .
C10 C 0.3268(12) 0.5286(6) 0.4489(6) 0.038(4) Uani 1.000000 .
H10a H 0.276(2) 0.526(4) 0.4688(8) 0.056(6) Uiso 1.000000 GR
H10b H 0.378(6) 0.505(3) 0.4604(13) 0.056(6) Uiso 1.000000 GR
H10c H 0.355(7) 0.5608(16) 0.4526(9) 0.056(6) Uiso 1.000000 GR
C43 C 0.5497(12) 0.8157(7) 0.1190(7) 0.043(4) Uani 1.000000 .
H43 H 0.5287(12) 0.8027(7) 0.1472(7) 0.052(5) Uiso 1.000000 R
C4 C 0.2108(11) 0.4656(6) 0.3275(6) 0.031(3) Uiso 1.000000 .
C34 C 0.0761(10) 0.9446(6) 0.2187(6) 0.029(3) Uani 1.000000 .
O37 O 0.5621(7) 0.7618(3) 0.4339(4) 0.028(2) Uani 1.000000 .
C36 C 0.0112(10) 0.9760(6) 0.1348(6) 0.032(4) Uani 1.000000 .
H36 H -0.0123(10) 1.0019(6) 0.1136(6) 0.038(4) Uiso 1.000000 R
C40 C 0.1271(14) 0.8113(6) 0.2074(6) 0.047(5) Uani 1.000000 .
H40a H 0.064(3) 0.802(2) 0.188(4) 0.071(7) Uiso 1.000000 GR
H40b H 0.175(7) 0.8120(13) 0.186(4) 0.071(7) Uiso 1.000000 GR
H40c H 0.147(9) 0.7882(10) 0.2341(7) 0.071(7) Uiso 1.000000 GR
N5 N 0.5350(12) 1.0530(6) 0.2347(8) 0.061(5) Uani 1.000000 .
C3 C 0.2104(11) 0.5046(6) 0.2921(6) 0.030(3) Uiso 1.000000 .
C28 C 0.4824(16) 1.0656(8) 0.1456(8) 0.060(5) Uiso 1.000000 .
H28 H 0.4681(16) 1.0980(8) 0.1515(8) 0.071(6) Uiso 1.000000 R
C24 C 0.5388(12) 0.9854(6) 0.1786(6) 0.032(3) Uiso 1.000000 .
C26 C 0.4841(12) 0.9996(7) 0.0886(8) 0.053(5) Uani 1.000000 .
H26 H 0.4713(12) 0.9885(7) 0.0554(8) 0.063(6) Uiso 1.000000 R
C27 C 0.4668(15) 1.0491(8) 0.0997(8) 0.055(5) Uiso 1.000000 .
C25 C 0.5199(12) 0.9681(7) 0.1277(8) 0.049(5) Uani 1.000000 .
H25 H 0.5316(12) 0.9356(7) 0.1208(8) 0.059(6) Uiso 1.000000 R
O14 O 0.5307(10) 0.8906(4) 0.5027(5) 0.053(3) Uani 1.000000 .
C17 C 0.7661(13) 0.4977(8) 0.4085(7) 0.049(5) Uani 1.000000 .
C18 C 0.7430(14) 0.5117(7) 0.3617(7) 0.047(4) Uiso 1.000000 .
H18 H 0.7489(14) 0.5445(7) 0.3539(7) 0.057(5) Uiso 1.000000 R
N3 N 0.6912(15) 0.4954(7) 0.2745(7) 0.072(5) Uiso 1.000000 .
C19 C 0.7083(16) 0.4776(8) 0.3216(8) 0.060(5) Uiso 1.000000 .
C11 C 0.6583(16) 0.4615(8) 0.2355(9) 0.063(6) Uiso 1.000000 .
H11 H 0.6466(16) 0.4721(8) 0.2021(9) 0.075(7) Uiso 1.000000 R
C14 C 0.6978(15) 0.4292(8) 0.3346(8) 0.055(5) Uiso 1.000000 .
N4 N 0.6492(17) 0.3474(8) 0.3017(9) 0.091(7) Uiso 1.000000 .
H4a H 0.640(15) 0.3425(10) 0.333(2) 0.110(8) Uiso 1.000000 GR
H4b H 0.597(9) 0.3351(18) 0.281(5) 0.110(8) Uiso 1.000000 GR
C22 C 0.5838(14) 0.9741(7) 0.2663(8) 0.054(5) Uani 1.000000 .
H22 H 0.6035(14) 0.9540(7) 0.2942(8) 0.065(6) Uiso 1.000000 R
C16 C 0.7521(14) 0.4474(9) 0.4197(10) 0.068(7) Uani 1.000000 .
H16 H 0.7660(14) 0.4365(9) 0.4530(10) 0.081(8) Uiso 1.000000 R
C15 C 0.7186(16) 0.4156(9) 0.3818(8) 0.061(6) Uiso 1.000000 .
H15 H 0.7103(16) 0.3830(9) 0.3897(8) 0.074(7) Uiso 1.000000 R
C29 C 0.5204(12) 1.0354(7) 0.1864(9) 0.051(5) Uani 1.000000 .
C21 C 0.5666(14) 1.0212(8) 0.2740(9) 0.057(5) Uani 1.000000 .
H21 H 0.5764(14) 1.0329(8) 0.3070(9) 0.068(6) Uiso 1.000000 R
C23 C 0.5737(14) 0.9550(7) 0.2201(7) 0.048(4) Uiso 1.000000 .
C20 C 0.7024(19) 0.5446(9) 0.2623(9) 0.077(7) Uiso 1.000000 .
H20a H 0.655(8) 0.5640(12) 0.275(6) 0.116(10) Uiso 1.000000 GR
H20b H 0.768(4) 0.5554(19) 0.277(5) 0.116(10) Uiso 1.000000 GR
H20c H 0.692(12) 0.5482(13) 0.2262(9) 0.116(10) Uiso 1.000000 GR
C12 C 0.6437(17) 0.4147(9) 0.2456(9) 0.068(6) Uiso 1.000000 .
H12 H 0.6210(17) 0.3941(9) 0.2185(9) 0.082(7) Uiso 1.000000 R
C13 C 0.6598(18) 0.3952(9) 0.2926(9) 0.072(6) Uiso 1.000000 .
Cl3 Cl 0.4225(5) 1.0866(3) 0.0484(3) 0.106(3) Uani 1.000000 .
N6 N 0.5925(11) 0.9072(6) 0.2141(6) 0.049(4) Uani 1.000000 .
H6a H 0.553(7) 0.8892(6) 0.228(5) 0.059(5) Uiso 1.000000 GR
H6b H 0.585(10) 0.9007(13) 0.1822(6) 0.059(5) Uiso 1.000000 GR
N10 N 0.9700(14) 0.7649(7) 0.3505(7) 0.064(5) Uiso 1.000000 .
C31 C 0.1421(14) 0.8682(8) 0.2788(7) 0.053(5) Uani 1.000000 .
H31 H 0.1634(14) 0.8416(8) 0.2995(7) 0.064(6) Uiso 1.000000 R
C32 C 0.1372(15) 0.9112(8) 0.3018(8) 0.055(5) Uiso 1.000000 .
H32 H 0.1569(15) 0.9140(8) 0.3367(8) 0.066(6) Uiso 1.000000 R
C33 C 0.1014(12) 0.9522(7) 0.2722(7) 0.045(4) Uani 1.000000 .
N8 N 0.0943(12) 0.9954(6) 0.2934(6) 0.053(4) Uani 1.000000 .
H8a H 0.1115(12) 0.9987(6) 0.3256(6) 0.064(5) Uiso 1.000000 R
H8b H 0.0724(12) 1.0201(6) 0.2749(6) 0.064(5) Uiso 1.000000 R
C45 C 0.9995(16) 0.7281(10) 0.3909(10) 0.088(9) Uani 1.000000 .
H45a H 1.056(9) 0.740(3) 0.414(4) 0.131(14) Uiso 1.000000 GR
H45b H 0.946(5) 0.723(5) 0.408(5) 0.131(14) Uiso 1.000000 GR
H45c H 1.016(13) 0.698(2) 0.3760(12) 0.131(14) Uiso 1.000000 GR
C44 C 0.9660(18) 0.8149(9) 0.3639(9) 0.074(7) Uiso 1.000000 .
H44a H 0.904(5) 0.8216(16) 0.374(6) 0.112(10) Uiso 1.000000 GR
H44b H 1.019(7) 0.8220(17) 0.392(4) 0.112(10) Uiso 1.000000 GR
H44c H 0.973(13) 0.8349(9) 0.335(2) 0.112(10) Uiso 1.000000 GR
O42 O 0.9539(19) 0.7815(9) 0.2709(10) 0.135(8) Uiso 1.000000 .
C30 C 0.518(2) 1.1041(10) 0.2461(11) 0.097(9) Uiso 1.000000 .
H30a H 0.557(12) 1.1246(11) 0.228(6) 0.146(13) Uiso 1.000000 GR
H30b H 0.449(3) 1.112(2) 0.236(7) 0.146(13) Uiso 1.000000 GR
H30c H 0.537(14) 1.110(2) 0.2818(15) 0.146(13) Uiso 1.000000 GR
C46 C 0.962(2) 0.7521(12) 0.3072(12) 0.103(9) Uiso 1.000000 .
H46 H 0.962(2) 0.7189(12) 0.3003(12) 0.123(11) Uiso 1.000000 R
C42 C 0.475(2) 0.7454(11) 0.0739(11) 0.100(10) Uani 1.000000 .
H42a H 0.515(4) 0.7172(12) 0.071(8) 0.150(14) Uiso 1.000000 GR
H42b H 0.446(13) 0.743(4) 0.104(4) 0.150(14) Uiso 1.000000 GR
H42c H 0.423(9) 0.747(4) 0.045(5) 0.150(14) Uiso 1.000000 GR
C41 C 0.564(2) 0.8070(12) 0.0314(11) 0.112(11) Uani 1.000000 .
H41a H 0.523(12) 0.834(6) 0.019(5) 0.168(16) Uiso 1.000000 GR
H41b H 0.632(6) 0.817(8) 0.039(2) 0.168(16) Uiso 1.000000 GR
H41c H 0.557(17) 0.782(3) 0.006(3) 0.168(16) Uiso 1.000000 GR
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Si 0.08192 0.07060 6.29150 3.03530 1.98910 1.54100 2.43860 32.33370 0.67850
81.69370 1.14069998264
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
W -0.66836 6.76498 29.08180 15.43000 14.43270 5.11982 1.72029 9.22590 0.32170
57.05600 9.88749980927
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 26 -18 0.1090
-12 -26 18 0.1090
-3 18 34 0.1213
3 -18 -34 0.1213
-19 6 14 0.0850
0 -3 -37 0.1135
10 24 19 0.1073
2 5 36 0.1137
-15 19 -10 0.0934
7 -31 16 0.0756
19 5 -2 0.0649
-8 34 12 0.0923
10 -15 25 0.0682
-20 0 6 0.0921
18 -4 -20 0.0646
6 -36 -7 0.1086
-9 -4 36 0.0983
-13 28 7 0.0742
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
O7 W5 O8 89.4(4) . . ?
O5 W5 O8 156.9(4) . . ?
O5 W5 O7 86.1(4) . . ?
O9 W5 O8 87.6(4) . . ?
O9 W5 O7 156.5(4) . . ?
O9 W5 O5 87.6(5) . . ?
O6 W5 O8 99.9(5) . . ?
O6 W5 O7 102.3(5) . . ?
O6 W5 O5 103.2(5) . . ?
O6 W5 O9 101.2(5) . . ?
O39 W5 O8 72.9(4) . . ?
O39 W5 O7 84.9(4) . . ?
O39 W5 O5 84.1(4) . . ?
O39 W5 O9 72.0(4) . . ?
O39 W5 O6 170.0(4) . . ?
O8 W7 O33 87.3(4) . . ?
O21 W7 O33 85.4(4) . . ?
O21 W7 O8 158.2(4) . . ?
O11 W7 O33 156.9(5) . . ?
O11 W7 O8 88.6(4) . . ?
O11 W7 O21 90.0(5) . . ?
O39 W7 O33 84.3(4) . . ?
O39 W7 O8 72.7(4) . . ?
O39 W7 O21 86.1(4) . . ?
O39 W7 O11 72.8(4) . . ?
O40 W7 O33 102.3(5) . . ?
O40 W7 O8 99.3(5) . . ?
O40 W7 O21 102.3(5) . . ?
O40 W7 O11 100.8(5) . . ?
O40 W7 O39 169.6(5) . . ?
O34 W2 O4 157.4(4) . . ?
O7 W2 O4 85.5(4) . . ?
O7 W2 O34 87.2(4) . . ?
O30 W2 O4 91.2(5) . . ?
O30 W2 O34 87.6(4) . . ?
O30 W2 O7 157.9(4) . . ?
O35 W2 O4 103.9(5) . . ?
O35 W2 O34 98.6(5) . . ?
O35 W2 O7 102.5(5) . . ?
O35 W2 O30 99.4(5) . . ?
O36 W2 O4 85.7(4) . . ?
O36 W2 O34 72.3(4) . . ?
O36 W2 O7 84.2(4) . . ?
O36 W2 O30 73.8(4) . . ?
O36 W2 O35 168.6(5) . . ?
O34 W8 O33 89.5(4) . . ?
O22 W8 O33 86.5(4) . . ?
O22 W8 O34 158.0(5) . . ?
O31 W8 O33 157.8(5) . . ?
O31 W8 O34 87.4(4) . . ?
O31 W8 O22 88.2(4) . . ?
O36 W8 O33 85.0(4) . . ?
O36 W8 O34 73.2(4) . . ?
O36 W8 O22 84.9(4) . . ?
O36 W8 O31 73.0(4) . . ?
O32 W8 O33 102.4(5) . . ?
O32 W8 O34 99.4(5) . . ?
O32 W8 O22 102.6(5) . . ?
O32 W8 O31 99.7(5) . . ?
O32 W8 O36 169.6(5) . . ?
O3 W1 O4 87.3(5) . . ?
O5 W1 O4 85.7(4) . . ?
O5 W1 O3 157.0(5) . . ?
O2 W1 O4 156.5(4) . . ?
O2 W1 O3 87.7(5) . . ?
O2 W1 O5 90.1(5) . . ?
O1 W1 O4 103.6(5) . . ?
O1 W1 O3 99.9(5) . . ?
O1 W1 O5 103.1(5) . . ?
O1 W1 O2 99.8(5) . . ?
O37 W1 O4 82.9(4) . . ?
O37 W1 O3 72.9(4) . . ?
O37 W1 O5 84.5(4) . . ?
O37 W1 O2 73.7(4) . . ?
O37 W1 O1 170.2(4) . . ?
O12 W6 O9 157.5(4) . . ?
O13 W6 O9 91.0(5) . . ?
O13 W6 O12 85.1(5) . . ?
O11 W6 O9 88.5(5) . . ?
O11 W6 O12 86.5(5) . . ?
O11 W6 O13 156.7(4) . . ?
O39 W6 O9 73.3(4) . . ?
O39 W6 O12 84.3(4) . . ?
O39 W6 O13 85.0(4) . . ?
O39 W6 O11 72.5(4) . . ?
O10 W6 O9 100.9(5) . . ?
O10 W6 O12 101.5(5) . . ?
O10 W6 O13 102.9(5) . . ?
O10 W6 O11 100.1(5) . . ?
O10 W6 O39 170.5(5) . . ?
O19 W10 O21 87.8(5) . . ?
O22 W10 O21 85.5(4) . . ?
O22 W10 O19 158.8(5) . . ?
O20 W10 O21 102.5(5) . . ?
O20 W10 O19 98.8(5) . . ?
O20 W10 O22 102.3(5) . . ?
O23 W10 O21 157.5(5) . . ?
O23 W10 O19 88.7(5) . . ?
O23 W10 O22 89.8(5) . . ?
O23 W10 O20 100.0(5) . . ?
O38 W10 O21 84.9(4) . . ?
O38 W10 O19 74.2(4) . . ?
O38 W10 O22 85.2(4) . . ?
O38 W10 O20 169.7(5) . . ?
O38 W10 O23 72.8(4) . . ?
O19 W12 O16 158.7(5) . . ?
O12 W12 O16 85.7(5) . . ?
O12 W12 O19 89.6(5) . . ?
O17 W12 O16 102.8(5) . . ?
O17 W12 O19 98.5(6) . . ?
O17 W12 O12 102.3(5) . . ?
O38 W12 O16 85.0(4) . . ?
O38 W12 O19 74.0(5) . . ?
O38 W12 O12 85.3(4) . . ?
O38 W12 O17 169.3(5) . . ?
O18 W12 O16 87.9(5) . . ?
O18 W12 O19 88.5(5) . . ?
O18 W12 O12 157.3(5) . . ?
O18 W12 O17 100.3(5) . . ?
O18 W12 O38 72.4(4) . . ?
O28 W3 O3 91.1(5) . . ?
O15 W3 O3 88.2(5) . . ?
O15 W3 O28 158.8(5) . . ?
O26 W3 O3 157.3(4) . . ?
O26 W3 O28 86.0(5) . . ?
O26 W3 O15 86.5(5) . . ?
O27 W3 O3 100.8(6) . . ?
O27 W3 O28 103.0(7) . . ?
O27 W3 O15 98.0(6) . . ?
O27 W3 O26 101.9(5) . . ?
O37 W3 O3 73.4(4) . . ?
O37 W3 O28 85.4(4) . . ?
O37 W3 O15 74.1(4) . . ?
O37 W3 O26 83.9(4) . . ?
O37 W3 O27 170.1(6) . . ?
O28 W9 O30 87.9(5) . . ?
O31 W9 O30 87.9(5) . . ?
O31 W9 O28 157.7(5) . . ?
O25 W9 O30 157.5(5) . . ?
O25 W9 O28 86.8(5) . . ?
O25 W9 O31 88.7(5) . . ?
O29 W9 O30 99.5(5) . . ?
O29 W9 O28 102.7(7) . . ?
O29 W9 O31 99.6(6) . . ?
O29 W9 O25 102.9(5) . . ?
O36 W9 O30 73.1(4) . . ?
O36 W9 O28 85.1(4) . . ?
O36 W9 O31 72.7(4) . . ?
O36 W9 O25 84.7(4) . . ?
O36 W9 O29 169.3(6) . . ?
O16 W4 O2 157.6(5) . . ?
O13 W4 O2 87.7(5) . . ?
O13 W4 O16 84.4(5) . . ?
O15 W4 O2 88.3(5) . . ?
O15 W4 O16 90.9(5) . . ?
O15 W4 O13 157.2(5) . . ?
O37 W4 O2 73.4(4) . . ?
O37 W4 O16 84.9(4) . . ?
O37 W4 O13 83.7(4) . . ?
O37 W4 O15 73.6(4) . . ?
O14 W4 O2 99.3(6) . . ?
O14 W4 O16 102.9(6) . . ?
O14 W4 O13 102.4(6) . . ?
O14 W4 O15 100.4(6) . . ?
O14 W4 O37 170.5(5) . . ?
O23 W11 O25 87.5(5) . . ?
O38 W11 O25 85.3(4) . . ?
O38 W11 O23 72.3(4) . . ?
O26 W11 O25 87.6(5) . . ?
O26 W11 O23 158.0(4) . . ?
O26 W11 O38 85.9(4) . . ?
O18 W11 O25 159.1(5) . . ?
O18 W11 O23 87.3(5) . . ?
O18 W11 O38 73.8(4) . . ?
O18 W11 O26 89.6(5) . . ?
O24 W11 O25 102.9(5) . . ?
O24 W11 O23 99.1(6) . . ?
O24 W11 O38 168.0(5) . . ?
O24 W11 O26 102.9(5) . . ?
O24 W11 O18 97.8(6) . . ?
O39 Si1 O38 109.8(5) . . ?
O36 Si1 O38 107.9(5) . . ?
O36 Si1 O39 109.1(5) . . ?
O37 Si1 O38 111.3(5) . . ?
O37 Si1 O39 109.3(5) . . ?
O37 Si1 O36 109.4(5) . . ?
W8 O33 W7 151.0(6) . . ?
W1 O4 W2 152.4(6) . . ?
W8 O34 W2 122.6(6) . . ?
W7 O8 W5 122.4(5) . . ?
W3 O3 W1 122.8(6) . . ?
W2 O7 W5 151.1(6) . . ?
W10 O21 W7 151.8(6) . . ?
W1 O5 W5 151.9(6) . . ?
W4 O2 W1 122.4(6) . . ?
W4 O16 W12 152.5(6) . . ?
W12 O19 W10 120.2(6) . . ?
W6 O9 W5 122.7(5) . . ?
W9 O30 W2 122.3(6) . . ?
W9 O28 W3 151.3(7) . . ?
W10 O22 W8 151.0(6) . . ?
W9 O31 W8 122.5(6) . . ?
W12 O12 W6 151.3(6) . . ?
W4 O13 W6 152.8(7) . . ?
W6 O11 W7 122.8(6) . . ?
W11 O25 W9 149.5(7) . . ?
W4 O15 W3 122.1(6) . . ?
W11 O23 W10 122.5(6) . . ?
W12 O38 W10 91.6(4) . . ?
W11 O38 W10 92.5(4) . . ?
W11 O38 W12 92.1(3) . . ?
Si1 O38 W10 125.3(6) . . ?
Si1 O38 W12 122.8(6) . . ?
Si1 O38 W11 123.3(6) . . ?
W11 O26 W3 150.1(6) . . ?
W11 O18 W12 121.7(6) . . ?
W7 O39 W5 92.0(3) . . ?
W6 O39 W5 92.0(3) . . ?
W6 O39 W7 91.8(3) . . ?
Si1 O39 W5 124.3(5) . . ?
Si1 O39 W7 123.6(5) . . ?
Si1 O39 W6 123.7(5) . . ?
W8 O36 W2 91.9(4) . . ?
W9 O36 W2 90.7(3) . . ?
W9 O36 W8 91.7(4) . . ?
Si1 O36 W2 123.4(5) . . ?
Si1 O36 W8 124.9(6) . . ?
Si1 O36 W9 124.3(5) . . ?
C1 N1 C9 119.9(12) . . ?
C10 N1 C9 120.4(12) . . ?
C10 N1 C1 119.7(13) . . ?
C8 C9 N1 120.5(13) . . ?
C4 C9 N1 120.1(13) . . ?
C4 C9 C8 119.3(13) . . ?
C7 C6 H6 121.3(9) . . ?
C5 C6 H6 121.3(9) . . ?
C5 C6 C7 117.4(14) . . ?
C40 N7 C39 120.6(13) . . ?
C31 N7 C39 116.7(15) . . ?
C31 N7 C40 122.6(15) . . ?
C38 C39 N7 119.7(14) . . ?
C34 C39 N7 121.3(14) . . ?
C34 C39 C38 119.1(14) . . ?
C1 C2 H2 118.6(9) . . ?
C3 C2 H2 118.6(9) . . ?
C3 C2 C1 122.9(15) . . ?
H8 C8 C9 120.3(8) . . ?
C7 C8 C9 119.3(14) . . ?
C7 C8 H8 120.3(9) . . ?
H38 C38 C39 120.6(9) . . ?
C37 C38 C39 118.9(14) . . ?
C37 C38 H38 120.6(9) . . ?
C6 C7 Cl1 119.6(12) . . ?
C8 C7 Cl1 117.6(13) . . ?
C8 C7 C6 122.7(14) . . ?
H2b N2 H2a 120.0 . . ?
C3 N2 H2a 120.0 . . ?
C3 N2 H2b 120.0 . . ?
C2 C1 N1 122.2(14) . . ?
H1 C1 N1 118.9(8) . . ?
H1 C1 C2 118.9(9) . . ?
H5 C5 C6 118.2(9) . . ?
C4 C5 C6 123.6(15) . . ?
C4 C5 H5 118.2(9) . . ?
C38 C37 Cl4 117.8(12) . . ?
C36 C37 Cl4 119.4(12) . . ?
C36 C37 C38 122.6(15) . . ?
C34 C35 H35 118.5(9) . . ?
C36 C35 H35 118.5(10) . . ?
C36 C35 C34 123.0(15) . . ?
C42 N9 C43 121.1(18) . . ?
C41 N9 C43 118(2) . . ?
C41 N9 C42 120(2) . . ?
H10a C10 N1 109.5 . . ?
H10b C10 N1 109.5 . . ?
H10b C10 H10a 109.5 . . ?
H10c C10 N1 109.5 . . ?
H10c C10 H10a 109.5 . . ?
H10c C10 H10b 109.5 . . ?
N9 C43 O41 127.6(18) . . ?
H43 C43 O41 116.2(12) . . ?
H43 C43 N9 116.2(11) . . ?
C5 C4 C9 117.6(14) . . ?
C3 C4 C9 118.8(14) . . ?
C3 C4 C5 123.6(14) . . ?
C35 C34 C39 118.1(14) . . ?
C33 C34 C39 119.9(15) . . ?
C33 C34 C35 121.9(15) . . ?
W3 O37 W1 90.9(3) . . ?
W4 O37 W1 90.5(4) . . ?
W4 O37 W3 90.2(3) . . ?
Si1 O37 W1 125.8(5) . . ?
Si1 O37 W3 125.0(6) . . ?
Si1 O37 W4 123.9(5) . . ?
C35 C36 C37 118.2(15) . . ?
H36 C36 C37 120.9(9) . . ?
H36 C36 C35 120.9(10) . . ?
H40a C40 N7 109.5 . . ?
H40b C40 N7 109.5 . . ?
H40b C40 H40a 109.5 . . ?
H40c C40 N7 109.5 . . ?
H40c C40 H40a 109.5 . . ?
H40c C40 H40b 109.5 . . ?
C21 N5 C29 118.5(17) . . ?
C30 N5 C29 122(2) . . ?
C30 N5 C21 119(2) . . ?
N2 C3 C2 121.5(14) . . ?
C4 C3 C2 116.1(14) . . ?
C4 C3 N2 122.4(14) . . ?
C27 C28 H28 119.5(14) . . ?
C29 C28 H28 119.5(13) . . ?
C29 C28 C27 121(2) . . ?
C29 C24 C25 117.2(16) . . ?
C23 C24 C25 122.8(16) . . ?
C23 C24 C29 120.0(17) . . ?
C27 C26 H26 120.4(12) . . ?
C25 C26 H26 120.4(13) . . ?
C25 C26 C27 119(2) . . ?
C26 C27 C28 122(2) . . ?
Cl3 C27 C28 121.6(18) . . ?
Cl3 C27 C26 116.5(16) . . ?
C26 C25 C24 120.1(18) . . ?
H25 C25 C24 120.0(10) . . ?
H25 C25 C26 120.0(13) . . ?
C18 C17 Cl2 125.5(18) . . ?
C16 C17 Cl2 116.5(16) . . ?
C16 C17 C18 118(2) . . ?
H18 C18 C17 119.3(13) . . ?
C19 C18 C17 121(2) . . ?
C19 C18 H18 119.3(12) . . ?
C11 N3 C19 116(2) . . ?
C20 N3 C19 124(2) . . ?
C20 N3 C11 120(2) . . ?
N3 C19 C18 117(2) . . ?
C14 C19 C18 117.9(19) . . ?
C14 C19 N3 126(2) . . ?
H11 C11 N3 119.2(13) . . ?
C12 C11 N3 122(2) . . ?
C12 C11 H11 119.2(15) . . ?
C15 C14 C19 120(2) . . ?
C13 C14 C19 117(2) . . ?
C13 C14 C15 123(2) . . ?
H4b N4 H4a 107.0 . . ?
C13 N4 H4a 111.2 . . ?
C13 N4 H4b 111.0 . . ?
C21 C22 H22 118.9(14) . . ?
C23 C22 H22 118.9(12) . . ?
C23 C22 C21 122(2) . . ?
H16 C16 C17 120.0(13) . . ?
C15 C16 C17 120(2) . . ?
C15 C16 H16 120.0(15) . . ?
C16 C15 C14 122(2) . . ?
H15 C15 C14 118.9(14) . . ?
H15 C15 C16 118.9(15) . . ?
C28 C29 N5 120(2) . . ?
C24 C29 N5 119.0(17) . . ?
C24 C29 C28 121(2) . . ?
C22 C21 N5 122(2) . . ?
H21 C21 N5 118.9(12) . . ?
H21 C21 C22 118.9(14) . . ?
C22 C23 C24 118.0(18) . . ?
N6 C23 C24 121.6(17) . . ?
N6 C23 C22 120.3(18) . . ?
H20a C20 N3 109.5 . . ?
H20b C20 N3 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 N3 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
H12 C12 C11 117.8(15) . . ?
C13 C12 C11 124(2) . . ?
C13 C12 H12 117.8(16) . . ?
N4 C13 C14 120(2) . . ?
C12 C13 C14 116(2) . . ?
C12 C13 N4 123(2) . . ?
H6a N6 C23 110.7 . . ?
H6b N6 C23 109.1 . . ?
H6b N6 H6a 109.0 . . ?
C44 N10 C45 119(2) . . ?
C46 N10 C45 118(3) . . ?
C46 N10 C44 122(2) . . ?
H31 C31 N7 116.6(11) . . ?
C32 C31 N7 126.8(19) . . ?
C32 C31 H31 116.6(12) . . ?
H32 C32 C31 120.6(12) . . ?
C33 C32 C31 118.7(19) . . ?
C33 C32 H32 120.6(11) . . ?
C32 C33 C34 116.5(17) . . ?
N8 C33 C34 122.6(18) . . ?
N8 C33 C32 120.9(18) . . ?
H8a N8 C33 120.0 . . ?
H8b N8 C33 120.0 . . ?
H8b N8 H8a 120.0 . . ?
H45a C45 N10 109.5 . . ?
H45b C45 N10 109.5 . . ?
H45b C45 H45a 109.5 . . ?
H45c C45 N10 109.5 . . ?
H45c C45 H45a 109.5 . . ?
H45c C45 H45b 109.5 . . ?
H44a C44 N10 109.5 . . ?
H44b C44 N10 109.5 . . ?
H44b C44 H44a 109.5 . . ?
H44c C44 N10 109.5 . . ?
H44c C44 H44a 109.5 . . ?
H44c C44 H44b 109.5 . . ?
H30a C30 N5 109.5 . . ?
H30b C30 N5 109.5 . . ?
H30b C30 H30a 109.5 . . ?
H30c C30 N5 109.5 . . ?
H30c C30 H30a 109.5 . . ?
H30c C30 H30b 109.5 . . ?
O42 C46 N10 123(3) . . ?
H46 C46 N10 118(2) . . ?
H46 C46 O42 118(2) . . ?
H42a C42 N9 109.5 . . ?
H42b C42 N9 109.5 . . ?
H42b C42 H42a 109.5 . . ?
H42c C42 N9 109.5 . . ?
H42c C42 H42a 109.5 . . ?
H42c C42 H42b 109.5 . . ?
H41a C41 N9 109.5 . . ?
H41b C41 N9 109.5 . . ?
H41b C41 H41a 109.5 . . ?
H41c C41 N9 109.5 . . ?
H41c C41 H41a 109.5 . . ?
H41c C41 H41b 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
W5 O8 1.927(10) . ?
W5 O7 1.893(10) . ?
W5 O5 1.908(10) . ?
W5 O9 1.952(11) . ?
W5 O6 1.703(10) . ?
W5 O39 2.339(9) . ?
W7 O33 1.933(10) . ?
W7 O8 1.922(10) . ?
W7 O21 1.899(10) . ?
W7 O11 1.893(11) . ?
W7 O39 2.350(10) . ?
W7 O40 1.683(10) . ?
W2 O4 1.874(11) . ?
W2 O34 1.933(11) . ?
W2 O7 1.927(9) . ?
W2 O30 1.902(11) . ?
W2 O35 1.673(11) . ?
W2 O36 2.353(10) . ?
W8 O33 1.879(10) . ?
W8 O34 1.909(10) . ?
W8 O22 1.908(10) . ?
W8 O31 1.934(11) . ?
W8 O36 2.334(11) . ?
W8 O32 1.709(12) . ?
W1 O4 1.920(11) . ?
W1 O3 1.932(11) . ?
W1 O5 1.884(10) . ?
W1 O2 1.918(11) . ?
W1 O1 1.699(11) . ?
W1 O37 2.368(10) . ?
W6 O9 1.879(11) . ?
W6 O12 1.930(11) . ?
W6 O13 1.896(11) . ?
W6 O11 1.936(12) . ?
W6 O39 2.332(10) . ?
W6 O10 1.701(12) . ?
W10 O21 1.908(10) . ?
W10 O19 1.940(13) . ?
W10 O22 1.894(10) . ?
W10 O20 1.714(11) . ?
W10 O23 1.901(11) . ?
W10 O38 2.335(11) . ?
W12 O16 1.886(11) . ?
W12 O19 1.932(12) . ?
W12 O12 1.877(10) . ?
W12 O17 1.685(11) . ?
W12 O38 2.348(11) . ?
W12 O18 1.958(13) . ?
W3 O3 1.908(11) . ?
W3 O28 1.924(11) . ?
W3 O15 1.914(14) . ?
W3 O26 1.912(11) . ?
W3 O27 1.681(12) . ?
W3 O37 2.364(9) . ?
W9 O30 1.930(11) . ?
W9 O28 1.883(11) . ?
W9 O31 1.911(13) . ?
W9 O25 1.885(10) . ?
W9 O29 1.709(11) . ?
W9 O36 2.364(9) . ?
W4 O2 1.926(10) . ?
W4 O16 1.911(10) . ?
W4 O13 1.904(11) . ?
W4 O15 1.924(12) . ?
W4 O37 2.376(10) . ?
W4 O14 1.682(12) . ?
W11 O25 1.924(11) . ?
W11 O23 1.940(12) . ?
W11 O38 2.330(10) . ?
W11 O26 1.899(12) . ?
W11 O18 1.898(13) . ?
W11 O24 1.687(11) . ?
Si1 O38 1.636(10) . ?
Si1 O39 1.647(10) . ?
Si1 O36 1.633(11) . ?
Si1 O37 1.579(10) . ?
Cl4 C37 1.719(16) . ?
Cl1 C7 1.727(16) . ?
Cl2 C17 1.718(19) . ?
N1 C9 1.362(18) . ?
N1 C1 1.350(18) . ?
N1 C10 1.472(19) . ?
C9 C8 1.40(2) . ?
C9 C4 1.43(2) . ?
O41 C43 1.19(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.39(2) . ?
C6 C5 1.37(2) . ?
N7 C39 1.364(18) . ?
N7 C40 1.45(2) . ?
N7 C31 1.35(2) . ?
C39 C38 1.43(2) . ?
C39 C34 1.41(2) . ?
C2 H2 0.9300 . ?
C2 C1 1.33(2) . ?
C2 C3 1.40(2) . ?
C8 H8 0.9300 . ?
C8 C7 1.38(2) . ?
C38 H38 0.9300 . ?
C38 C37 1.36(2) . ?
N2 H2a 0.8600 . ?
N2 H2b 0.8600 . ?
N2 C3 1.316(19) . ?
C1 H1 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.40(2) . ?
C37 C36 1.40(2) . ?
C35 H35 0.9300 . ?
C35 C34 1.41(2) . ?
C35 C36 1.35(2) . ?
N9 C43 1.35(2) . ?
N9 C42 1.42(3) . ?
N9 C41 1.46(3) . ?
C10 H10a 0.9600 . ?
C10 H10b 0.9600 . ?
C10 H10c 0.9600 . ?
C43 H43 0.9300 . ?
C4 C3 1.43(2) . ?
C34 C33 1.43(2) . ?
C36 H36 0.9300 . ?
C40 H40a 0.9600 . ?
C40 H40b 0.9600 . ?
C40 H40c 0.9600 . ?
N5 C29 1.36(3) . ?
N5 C21 1.38(3) . ?
N5 C30 1.46(3) . ?
C28 H28 0.9300 . ?
C28 C27 1.29(3) . ?
C28 C29 1.40(3) . ?
C24 C25 1.43(2) . ?
C24 C29 1.42(2) . ?
C24 C23 1.40(2) . ?
C26 H26 0.9300 . ?
C26 C27 1.42(3) . ?
C26 C25 1.38(2) . ?
C27 Cl3 1.74(2) . ?
C25 H25 0.9300 . ?
C17 C18 1.30(3) . ?
C17 C16 1.43(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.44(3) . ?
N3 C19 1.34(3) . ?
N3 C11 1.41(3) . ?
N3 C20 1.40(3) . ?
C19 C14 1.39(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.34(3) . ?
C14 C15 1.30(3) . ?
C14 C13 1.48(3) . ?
N4 H4a 0.8776 . ?
N4 H4b 0.8887 . ?
N4 C13 1.34(3) . ?
C22 H22 0.9300 . ?
C22 C21 1.33(3) . ?
C22 C23 1.33(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.35(3) . ?
C15 H15 0.9300 . ?
C21 H21 0.9300 . ?
C23 N6 1.35(2) . ?
C20 H20a 0.9600 . ?
C20 H20b 0.9600 . ?
C20 H20c 0.9600 . ?
C12 H12 0.9300 . ?
C12 C13 1.35(3) . ?
N6 H6a 0.8616 . ?
N6 H6b 0.8618 . ?
N10 C45 1.48(3) . ?
N10 C44 1.42(3) . ?
N10 C46 1.20(3) . ?
C31 H31 0.9300 . ?
C31 C32 1.34(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.41(3) . ?
C33 N8 1.32(2) . ?
N8 H8a 0.8600 . ?
N8 H8b 0.8600 . ?
C45 H45a 0.9600 . ?
C45 H45b 0.9600 . ?
C45 H45c 0.9600 . ?
C44 H44a 0.9600 . ?
C44 H44b 0.9600 . ?
C44 H44c 0.9600 . ?
O42 C46 1.25(3) . ?
C30 H30a 0.9600 . ?
C30 H30b 0.9600 . ?
C30 H30c 0.9600 . ?
C46 H46 0.9300 . ?
C42 H42a 0.9600 . ?
C42 H42b 0.9600 . ?
C42 H42c 0.9600 . ?
C41 H41a 0.9600 . ?
C41 H41b 0.9600 . ?
C41 H41c 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4b O42 0.8887 2.06(9) 2.84(4) 146(14) 2_645
N6 H6b O41 0.8618 2.01(2) 2.80(2) 151.9(8) .
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
W5 O39 Si1 O38 177.8(6) . . . . ?
W5 O39 Si1 O36 59.7(7) . . . . ?
W5 O39 Si1 O37 -59.9(7) . . . . ?
W7 O39 Si1 O38 57.6(7) . . . . ?
W7 O39 Si1 O36 -60.5(7) . . . . ?
W7 O39 Si1 O37 179.9(5) . . . . ?
W2 O36 Si1 O38 179.1(6) . . . . ?
W2 O36 Si1 O39 -61.7(7) . . . . ?
W2 O36 Si1 O37 57.9(7) . . . . ?
W8 O36 Si1 O38 -60.2(7) . . . . ?
W8 O36 Si1 O39 59.0(7) . . . . ?
W8 O36 Si1 O37 178.5(5) . . . . ?
W1 O37 Si1 O38 178.8(6) . . . . ?
W1 O37 Si1 O39 57.4(7) . . . . ?
W1 O37 Si1 O36 -62.0(7) . . . . ?
W6 O39 Si1 O38 -61.7(7) . . . . ?
W6 O39 Si1 O36 -179.7(6) . . . . ?
W6 O39 Si1 O37 60.7(7) . . . . ?
W10 O38 Si1 O39 -59.6(7) . . . . ?
W10 O38 Si1 O36 59.2(7) . . . . ?
W10 O38 Si1 O37 179.2(6) . . . . ?
W12 O38 Si1 O39 60.1(7) . . . . ?
W12 O38 Si1 O36 179.0(6) . . . . ?
W12 O38 Si1 O37 -61.0(7) . . . . ?
W3 O37 Si1 O38 -59.4(7) . . . . ?
W3 O37 Si1 O39 179.2(5) . . . . ?
W3 O37 Si1 O36 59.8(7) . . . . ?
W9 O36 Si1 O38 61.1(7) . . . . ?
W9 O36 Si1 O39 -179.6(6) . . . . ?
W9 O36 Si1 O37 -60.1(7) . . . . ?
W4 O37 Si1 O38 59.1(7) . . . . ?
W4 O37 Si1 O39 -62.3(7) . . . . ?
W4 O37 Si1 O36 178.2(5) . . . . ?
W11 O38 Si1 O39 178.5(6) . . . . ?
W11 O38 Si1 O36 -62.6(7) . . . . ?
W11 O38 Si1 O37 57.4(8) . . . . ?
Cl4 C37 C38 C39 179.9(11) . . . . ?
Cl4 C37 C36 C35 -178.0(11) . . . . ?
Cl1 C7 C6 C5 176.5(11) . . . . ?
Cl1 C7 C8 C9 -176.3(10) . . . . ?
Cl2 C17 C18 C19 177.9(16) . . . . ?
Cl2 C17 C16 C15 -178.5(15) . . . . ?
N1 C9 C8 C7 178.1(13) . . . . ?
N1 C9 C4 C5 -179.6(14) . . . . ?
N1 C9 C4 C3 -1.8(16) . . . . ?
N1 C1 C2 C3 -0.2(18) . . . . ?
C9 C8 C7 C6 0.2(15) . . . . ?
C9 C4 C5 C6 3.1(17) . . . . ?
C9 C4 C3 C2 1.0(16) . . . . ?
C9 C4 C3 N2 179.7(14) . . . . ?
O41 C43 N9 C42 -170(2) . . . . ?
O41 C43 N9 C41 -1(3) . . . . ?
C6 C5 C4 C3 -174.7(15) . . . . ?
N7 C39 C38 C37 176.9(14) . . . . ?
N7 C39 C34 C35 -179.8(14) . . . . ?
N7 C39 C34 C33 -1.9(17) . . . . ?
N7 C31 C32 C33 2(2) . . . . ?
C39 C38 C37 C36 5.6(15) . . . . ?
C39 C34 C35 C36 0.4(15) . . . . ?
C39 C34 C33 C32 1.9(16) . . . . ?
C39 C34 C33 N8 -179.5(14) . . . . ?
C2 C3 C4 C5 178.7(13) . . . . ?
C38 C37 C36 C35 -3.7(18) . . . . ?
N2 C3 C4 C5 -2.5(18) . . . . ?
C37 C36 C35 C34 0.6(16) . . . . ?
C35 C34 C33 C32 179.7(16) . . . . ?
C35 C34 C33 N8 -1.7(16) . . . . ?
C34 C33 C32 C31 -2.1(18) . . . . ?
N5 C29 C28 C27 -178.9(19) . . . . ?
N5 C29 C24 C25 178.2(15) . . . . ?
N5 C29 C24 C23 -1.4(19) . . . . ?
N5 C21 C22 C23 2(2) . . . . ?
C28 C27 C26 C25 -1(2) . . . . ?
C28 C29 C24 C25 1.8(19) . . . . ?
C28 C29 C24 C23 -177.7(17) . . . . ?
C24 C25 C26 C27 0(2) . . . . ?
C24 C23 C22 C21 -3(2) . . . . ?
C17 C18 C19 N3 -177(2) . . . . ?
C17 C18 C19 C14 2(2) . . . . ?
C17 C16 C15 C14 -0(2) . . . . ?
C18 C19 N3 C11 179.4(19) . . . . ?
C18 C19 N3 C20 -2(3) . . . . ?
C18 C19 C14 C15 0(2) . . . . ?
C18 C19 C14 C13 179(2) . . . . ?
N3 C19 C14 C15 178(2) . . . . ?
N3 C19 C14 C13 -3(3) . . . . ?
N3 C11 C12 C13 -1(3) . . . . ?
C19 C14 C15 C16 -1(3) . . . . ?
C19 C14 C13 N4 179(2) . . . . ?
C19 C14 C13 C12 3(2) . . . . ?
C11 C12 C13 C14 -1(3) . . . . ?
C11 C12 C13 N4 -177(2) . . . . ?
C31 C32 C33 N8 179.3(18) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.0059 25.9269 -17.9233 -0.0092 -0.1232 0.9748
-12.0059 -25.9269 17.9233 0.0092 0.1232 -0.9748
-3.0424 18.0971 33.9376 0.2179 0.9864 0.0199
3.0424 -18.0971 -33.9376 -0.2179 -0.9864 -0.0199
-18.9374 6.0924 13.9134 0.8137 0.2303 -0.5427
0.0756 -3.0916 -36.9395 0.1535 -0.9620 0.1987
9.9351 24.0232 19.0082 -0.1551 0.7778 0.6216
1.9191 5.0837 35.9484 -0.2014 0.9722 -0.0946
-14.8936 19.0250 -10.0303 0.9739 -0.2294 -0.0106
6.9070 -30.9896 15.9904 -0.8539 0.2051 -0.4960
18.9217 4.9399 -1.9307 -0.7102 0.1672 0.6697
-7.9590 34.0621 11.9606 0.7909 0.5199 0.3300
9.8882 -14.9723 24.9894 -0.7837 0.5970 -0.1643
-19.9212 0.0742 5.9218 0.8070 -0.0326 -0.6314
17.9564 -4.1037 -19.9064 -0.7088 -0.3743 0.5929
5.9558 -36.0444 -6.9762 -0.7644 -0.4288 -0.4618
-9.0385 -3.8859 35.9088 0.1226 0.7940 -0.5909
-12.9308 28.0631 6.9504 0.9359 0.2961 0.1026
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.019 0.000 0.500 1537.1 319.8 '8 C3H7NO'
2 -0.032 0.500 0.000 1537.1 319.8 '8 C3H7NO'
3 0.113 0.354 0.549 11.2 0.0 ?
4 0.387 0.854 0.951 11.2 0.0 ?
5 0.613 0.146 0.049 11.2 0.0 ?
6 0.887 0.646 0.451 11.2 0.0 ?
