#------------------------------------------------------------------------------
#$Date: 2021-06-04 13:52:06 +0300 (Fri, 04 Jun 2021) $
#$Revision: 265778 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/31/1563143.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_1563143
loop_
_publ_author_name
'Modder, Dieuwertje K.'
'Palumbo, Chad T.'
'Douair, Iskander'
'Scopelliti, Rosario'
'Maron, Laurent'
'Mazzanti, Marinella'
_publ_section_title
;
 Single metal four-electron reduction by U(ii) and masked
 "U(ii)" compounds.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              6153
_journal_page_last               6158
_journal_paper_doi               10.1039/d1sc00668a
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C30 H64 N5 Si6 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C48 H100 K N7 O6 Si6 U'
_chemical_formula_weight         1317.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                103.478(4)
_cell_angle_beta                 101.463(3)
_cell_angle_gamma                90.908(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4770(3)
_cell_length_b                   16.6790(8)
_cell_length_c                   19.0067(8)
_cell_measurement_reflns_used    12607
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6540
_cell_measurement_theta_min      3.9160
_cell_volume                     3460.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -13.00   1.00    4.00    --  -40.91 -57.00 -65.00  100
  2  ω    -55.00  31.00   1.00    4.00    --  -40.91  57.00  76.00   86
  3  ω     -5.00  20.00   1.00    4.00    --   40.91 -57.00 -65.00   25
  4  ω     73.00 100.00   1.00    4.00    --   40.91  57.00  76.00   27
  5  ω     32.00 129.00   1.00   16.00    --  105.15 -57.00 -65.00   97
  6  ω     87.00 177.00   1.00   16.00    --  105.15  57.00  76.00   90
  7  ω    -65.00  33.00   1.00    4.00    --  -40.91  38.00-120.00   98
  8  ω    -80.00  -9.00   1.00    4.00    --  -40.91 125.00  90.00   71
  9  ω     59.00  90.00   1.00    4.00    --   40.91-125.00-120.00   31
 10  ω     34.00 107.00   1.00   16.00    --  105.15-111.00 -90.00   73
 11  ω    109.00 136.00   1.00   16.00    --  105.15 -15.00  60.00   27
 12  ω     31.00 108.00   1.00   16.00    --  105.15-111.00 120.00   77
 13  ω     60.00  90.00   1.00   16.00    --  105.15 -15.00  60.00   30
 14  ω    104.00 132.00   1.00   16.00    --  105.15 111.00 120.00   28
 15  ω     79.00 178.00   1.00   16.00    --  105.15  45.00  30.00   99
 16  ω     79.00 106.00   1.00   16.00    --  105.15 -94.00   0.00   27
 17  ω    104.00 171.00   1.00   16.00    --  105.15  77.00 -60.00   67
 18  ω    104.00 132.00   1.00   16.00    --  105.15 -77.00  90.00   28
 19  ω    105.00 147.00   1.00   16.00    --  105.15  45.00 -90.00   42
 20  ω     24.00  75.00   1.00   16.00    --  105.15 -94.00 -60.00   51
 21  ω     24.00  58.00   1.00   16.00    --  105.15 -15.00  60.00   34
 22  ω     70.00 109.00   1.00   16.00    --  105.15-111.00   0.00   39
 23  ω    117.00 178.00   1.00   16.00    --  105.15  77.00 -30.00   61
 24  ω     29.00 106.00   1.00   16.00    --  105.15 -94.00 150.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0505621000
_diffrn_orient_matrix_UB_12      -0.0624842000
_diffrn_orient_matrix_UB_13      -0.0579272000
_diffrn_orient_matrix_UB_21      0.0864268000
_diffrn_orient_matrix_UB_22      0.0687856000
_diffrn_orient_matrix_UB_23      -0.0055550000
_diffrn_orient_matrix_UB_31      0.0938757000
_diffrn_orient_matrix_UB_32      -0.0205962000
_diffrn_orient_matrix_UB_33      0.0622523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14136
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.725
_diffrn_reflns_theta_min         3.938
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.476
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.112
_refine_diff_density_max         5.937
_refine_diff_density_min         -5.122
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         14136
_refine_ls_number_restraints     934
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.1069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1197P)²+86.4352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2799
_refine_ls_wR_factor_ref         0.2818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13270
_reflns_number_total             14136
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -175.1076° 
around [0.95 -0.02 -0.31] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d1sc00668a2.cif
_cod_data_source_block           dkm297_sq
_cod_original_cell_volume        3460.2(3)
_cod_database_code               1563143
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H108 N7 O7 Si6 K1 U1'
_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   0.450
_shelx_estimated_absorpt_t_min   0.202
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.658(3)
 0.342(3)
2. 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
3. Restrained distances
 C31-C32 \\sim C34-C33 \\sim C36-C35 \\sim C48-C47 \\sim C46-C45 \\sim C44-C43
\\sim C37-C38 \\sim C40-C39
 \\sim C42-C41
 with sigma of 0.02
 Si6-C28 \\sim Si6-C29 \\sim Si6-C30 \\sim Si5-C26 \\sim Si5-C25 \\sim Si5-C27
\\sim Si3-C20 \\sim Si3-C21
 \\sim Si3-C19 \\sim Si4-C24 \\sim Si4-C22 \\sim Si4-C23 \\sim Si2-C16 \\sim
Si2-C18 \\sim Si2-C17 \\sim Si1-
 C14 \\sim Si1-C15 \\sim Si1-C13
 with sigma of 0.02
 O3-C39 \\sim O3-C38 \\sim O4-C40 \\sim O4-C41 \\sim O2-C34 \\sim O2-C35 \\sim
O6-C47 \\sim O6-C46 \\sim O5-
 C45 \\sim O5-C44 \\sim O1-C32 \\sim O1-C33
 with sigma of 0.02
 N1-C1 \\sim N2-C7
 with sigma of 0.02
 N7-C42 \\sim N7-C36 \\sim N7-C48 \\sim N6-C31 \\sim N6-C37 \\sim N6-C43
 with sigma of 0.02
 Si4-N4 \\sim Si3-N4 \\sim Si1-N3 \\sim Si2-N3 \\sim Si5-N5 \\sim Si6-N5
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C12(H12), C11(H11), C10(H10), C9(H9),
 C8(H8)
5.c Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C12,C11,C10,C9,C8)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_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 4.403
_oxdiff_exptl_absorpt_empirical_full_min 0.486
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_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_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
U1 U 0.53361(5) 0.66691(3) 0.74237(3) 0.02999(18) Uani 1 1 d . . . . .
Si1 Si 0.4634(4) 0.8452(3) 0.6721(3) 0.0380(10) Uani 1 1 d D . . . .
Si2 Si 0.2833(4) 0.7065(3) 0.6110(3) 0.0422(11) Uani 1 1 d D . . . .
Si3 Si 0.4364(5) 0.4635(3) 0.6759(3) 0.0512(13) Uani 1 1 d D . . . .
Si4 Si 0.4135(4) 0.5215(3) 0.8332(3) 0.0413(11) Uani 1 1 d D . . . .
Si5 Si 0.7793(4) 0.6613(3) 0.6494(3) 0.0423(11) Uani 1 1 d D . . . .
Si6 Si 0.8179(5) 0.5834(4) 0.7750(3) 0.0499(13) Uani 1 1 d D . . . .
N1 N 0.4799(12) 0.7451(8) 0.8443(8) 0.036(3) Uani 1 1 d D . . . .
N2 N 0.6029(11) 0.7634(8) 0.8461(7) 0.034(3) Uani 1 1 d D . . . .
N3 N 0.4192(10) 0.7430(7) 0.6680(8) 0.036(3) Uani 1 1 d D . . . .
N4 N 0.4568(12) 0.5436(8) 0.7564(6) 0.038(3) Uani 1 1 d D . . . .
N5 N 0.7248(10) 0.6347(9) 0.7195(7) 0.037(3) Uani 1 1 d D . . . .
C1 C 0.4036(8) 0.8092(5) 0.8595(7) 0.034(3) Uani 1 1 d DG . . . .
C6 C 0.4485(7) 0.8900(6) 0.8928(7) 0.038(3) Uani 1 1 d G . . . .
H6 H 0.531978 0.903192 0.903804 0.046 Uiso 1 1 calc R U . . .
C5 C 0.3712(9) 0.9515(5) 0.9100(7) 0.043(4) Uani 1 1 d G . . . .
H5 H 0.401903 1.006674 0.932733 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2491(9) 0.9322(6) 0.8939(7) 0.049(4) Uani 1 1 d G . . . .
H4 H 0.196264 0.974167 0.905633 0.058 Uiso 1 1 calc R U . . .
C3 C 0.2042(6) 0.8514(7) 0.8606(7) 0.045(4) Uani 1 1 d G . . . .
H3 H 0.120698 0.838176 0.849603 0.054 Uiso 1 1 calc R U . . .
C2 C 0.2814(8) 0.7899(5) 0.8434(7) 0.043(4) Uani 1 1 d G . . . .
H2 H 0.250771 0.734692 0.820674 0.051 Uiso 1 1 calc R U . . .
C7 C 0.6834(9) 0.7880(7) 0.9131(5) 0.040(3) Uani 1 1 d DG . . . .
C12 C 0.6516(8) 0.8074(8) 0.9817(6) 0.045(4) Uani 1 1 d G . . . .
H12 H 0.570567 0.800796 0.984866 0.054 Uiso 1 1 calc R U . . .
C11 C 0.7383(12) 0.8365(10) 1.0456(5) 0.061(5) Uani 1 1 d G . . . .
H11 H 0.716617 0.849796 1.092474 0.073 Uiso 1 1 calc R U . . .
C10 C 0.8569(10) 0.8462(10) 1.0410(6) 0.066(5) Uani 1 1 d G . . . .
H10 H 0.916167 0.866107 1.084659 0.080 Uiso 1 1 calc R U . . .
C9 C 0.8887(8) 0.8268(9) 0.9724(8) 0.061(5) Uani 1 1 d G . . . .
H9 H 0.969668 0.833417 0.969237 0.073 Uiso 1 1 calc R U . . .
C8 C 0.8019(10) 0.7977(8) 0.9085(6) 0.045(4) Uani 1 1 d G . . . .
H8 H 0.823619 0.784416 0.861628 0.054 Uiso 1 1 calc R U . . .
C13 C 0.6190(12) 0.8745(11) 0.7252(11) 0.046(4) Uani 1 1 d D . . . .
H13A H 0.628596 0.859627 0.772892 0.069 Uiso 1 1 calc R U . . .
H13B H 0.635448 0.934212 0.733692 0.069 Uiso 1 1 calc R U . . .
H13C H 0.674745 0.845095 0.697064 0.069 Uiso 1 1 calc R U . . .
C14 C 0.3705(13) 0.9247(10) 0.7156(8) 0.039(4) Uani 1 1 d D . . . .
H14A H 0.303916 0.933954 0.677825 0.059 Uiso 1 1 calc R U . . .
H14B H 0.419180 0.976549 0.738297 0.059 Uiso 1 1 calc R U . . .
H14C H 0.339349 0.905562 0.753706 0.059 Uiso 1 1 calc R U . . .
C15 C 0.4609(19) 0.8654(14) 0.5786(9) 0.052(5) Uani 1 1 d D . . . .
H15A H 0.507129 0.824846 0.551512 0.079 Uiso 1 1 calc R U . . .
H15B H 0.495910 0.921162 0.584643 0.079 Uiso 1 1 calc R U . . .
H15C H 0.378439 0.860592 0.550841 0.079 Uiso 1 1 calc R U . . .
C16 C 0.1709(17) 0.7863(14) 0.6038(14) 0.063(6) Uani 1 1 d D . . . .
H16A H 0.167091 0.818181 0.653496 0.095 Uiso 1 1 calc R U . . .
H16B H 0.092528 0.758815 0.578858 0.095 Uiso 1 1 calc R U . . .
H16C H 0.194489 0.823435 0.575300 0.095 Uiso 1 1 calc R U . . .
C17 C 0.2966(19) 0.6569(15) 0.5136(8) 0.059(5) Uani 1 1 d D . . . .
H17A H 0.350792 0.691592 0.497628 0.088 Uiso 1 1 calc R U . . .
H17B H 0.217904 0.650887 0.480728 0.088 Uiso 1 1 calc R U . . .
H17C H 0.328011 0.602318 0.511814 0.088 Uiso 1 1 calc R U . . .
C18 C 0.2121(15) 0.6295(14) 0.6500(13) 0.059(6) Uani 1 1 d D . . . .
H18A H 0.274114 0.604258 0.679580 0.089 Uiso 1 1 calc R U . . .
H18B H 0.165489 0.586558 0.609487 0.089 Uiso 1 1 calc R U . . .
H18C H 0.159549 0.657554 0.681422 0.089 Uiso 1 1 calc R U . . .
C19 C 0.2808(15) 0.4158(16) 0.6406(14) 0.068(6) Uani 1 1 d D . . . .
H19A H 0.224675 0.459488 0.640701 0.102 Uiso 1 1 calc R U . . .
H19B H 0.262955 0.380904 0.672589 0.102 Uiso 1 1 calc R U . . .
H19C H 0.273208 0.382044 0.590075 0.102 Uiso 1 1 calc R U . . .
C20 C 0.482(2) 0.5084(14) 0.6031(10) 0.057(5) Uani 1 1 d D . . . .
H20A H 0.424330 0.547170 0.588785 0.086 Uiso 1 1 calc R U . . .
H20B H 0.485749 0.463865 0.559690 0.086 Uiso 1 1 calc R U . . .
H20C H 0.561169 0.537548 0.622664 0.086 Uiso 1 1 calc R U . . .
C21 C 0.530(2) 0.3747(12) 0.6783(18) 0.083(8) Uani 1 1 d D . . . .
H21A H 0.546688 0.352268 0.628989 0.124 Uiso 1 1 calc R U . . .
H21B H 0.488798 0.331884 0.693311 0.124 Uiso 1 1 calc R U . . .
H21C H 0.605850 0.393064 0.713791 0.124 Uiso 1 1 calc R U . . .
C22 C 0.2506(12) 0.5321(13) 0.8280(12) 0.047(4) Uani 1 1 d D . . . .
H22A H 0.234907 0.590780 0.839963 0.070 Uiso 1 1 calc R U . . .
H22B H 0.224491 0.505286 0.863502 0.070 Uiso 1 1 calc R U . . .
H22C H 0.206756 0.505736 0.777929 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4898(18) 0.5903(14) 0.9244(9) 0.057(5) Uani 1 1 d D . . . .
H23A H 0.576069 0.592996 0.927320 0.085 Uiso 1 1 calc R U . . .
H23B H 0.472166 0.567890 0.964683 0.085 Uiso 1 1 calc R U . . .
H23C H 0.461070 0.645894 0.928726 0.085 Uiso 1 1 calc R U . . .
C24 C 0.4443(19) 0.4149(10) 0.8456(11) 0.050(4) Uani 1 1 d D . . . .
H24A H 0.411427 0.374137 0.799325 0.075 Uiso 1 1 calc R U . . .
H24B H 0.407126 0.404445 0.885041 0.075 Uiso 1 1 calc R U . . .
H24C H 0.530577 0.410560 0.858982 0.075 Uiso 1 1 calc R U . . .
C25 C 0.8902(16) 0.7531(11) 0.6840(13) 0.055(5) Uani 1 1 d D . . . .
H25A H 0.862206 0.794586 0.721562 0.083 Uiso 1 1 calc R U . . .
H25B H 0.898810 0.776998 0.642655 0.083 Uiso 1 1 calc R U . . .
H25C H 0.967436 0.735610 0.705713 0.083 Uiso 1 1 calc R U . . .
C26 C 0.6553(14) 0.6829(12) 0.5772(9) 0.046(4) Uani 1 1 d D . . . .
H26A H 0.596804 0.635358 0.559631 0.068 Uiso 1 1 calc R U . . .
H26B H 0.687539 0.692544 0.535672 0.068 Uiso 1 1 calc R U . . .
H26C H 0.616655 0.731952 0.598587 0.068 Uiso 1 1 calc R U . . .
C27 C 0.854(2) 0.5776(13) 0.5945(13) 0.062(5) Uani 1 1 d D . . . .
H27A H 0.919744 0.559580 0.627709 0.093 Uiso 1 1 calc R U . . .
H27B H 0.885654 0.598551 0.557503 0.093 Uiso 1 1 calc R U . . .
H27C H 0.796469 0.530705 0.569668 0.093 Uiso 1 1 calc R U . . .
C28 C 0.7560(18) 0.5751(12) 0.8568(9) 0.047(4) Uani 1 1 d D . . . .
H28A H 0.718308 0.626030 0.874606 0.071 Uiso 1 1 calc R U . . .
H28B H 0.820582 0.566668 0.896183 0.071 Uiso 1 1 calc R U . . .
H28C H 0.696721 0.528146 0.842616 0.071 Uiso 1 1 calc R U . . .
C29 C 0.9694(13) 0.6381(15) 0.8113(14) 0.069(6) Uani 1 1 d D . . . .
H29A H 1.004072 0.645159 0.769809 0.103 Uiso 1 1 calc R U . . .
H29B H 1.020856 0.605375 0.839805 0.103 Uiso 1 1 calc R U . . .
H29C H 0.962648 0.692403 0.843305 0.103 Uiso 1 1 calc R U . . .
C30 C 0.847(3) 0.4777(12) 0.7243(16) 0.082(8) Uani 1 1 d D . . . .
H30A H 0.841751 0.438498 0.754862 0.124 Uiso 1 1 calc R U . . .
H30B H 0.927369 0.478710 0.713601 0.124 Uiso 1 1 calc R U . . .
H30C H 0.788260 0.460556 0.677753 0.124 Uiso 1 1 calc R U . . .
K1 K 0.8639(4) 1.1848(2) 0.8116(2) 0.0451(9) Uani 1 1 d . . . . .
O1 O 0.6227(13) 1.1832(11) 0.7426(8) 0.064(4) Uani 1 1 d D . . . .
O2 O 0.8070(14) 1.1742(11) 0.6570(8) 0.072(4) Uani 1 1 d D . . . .
O3 O 0.8683(12) 1.2983(8) 0.9489(8) 0.051(3) Uani 1 1 d D . . . .
O4 O 1.0282(15) 1.3239(10) 0.8602(9) 0.067(4) Uani 1 1 d D . . . .
O5 O 0.8234(11) 1.0365(8) 0.8477(8) 0.048(3) Uani 1 1 d D . . . .
O6 O 1.0150(11) 1.0555(8) 0.7813(7) 0.046(3) Uani 1 1 d D . . . .
N6 N 0.6690(12) 1.1673(9) 0.8959(8) 0.049(3) Uani 1 1 d D . . . .
N7 N 1.0596(17) 1.2000(10) 0.7257(9) 0.062(4) Uani 1 1 d D . . . .
C31 C 0.5600(17) 1.1969(17) 0.8601(12) 0.068(6) Uani 1 1 d D . . . .
H31A H 0.568041 1.257864 0.869339 0.082 Uiso 1 1 calc R U . . .
H31B H 0.492614 1.181949 0.880913 0.082 Uiso 1 1 calc R U . . .
C32 C 0.5357(19) 1.159(2) 0.7786(12) 0.082(7) Uani 1 1 d D . . . .
H32A H 0.531365 1.098442 0.770182 0.098 Uiso 1 1 calc R U . . .
H32B H 0.457077 1.175414 0.755815 0.098 Uiso 1 1 calc R U . . .
C33 C 0.603(2) 1.149(2) 0.6655(10) 0.095(8) Uani 1 1 d D . . . .
H33A H 0.519604 1.155006 0.642132 0.113 Uiso 1 1 calc R U . . .
H33B H 0.616015 1.088752 0.656037 0.113 Uiso 1 1 calc R U . . .
C34 C 0.6865(19) 1.191(2) 0.6329(15) 0.101(9) Uani 1 1 d D . . . .
H34A H 0.664449 1.172877 0.578265 0.121 Uiso 1 1 calc R U . . .
H34B H 0.678697 1.251450 0.647040 0.121 Uiso 1 1 calc R U . . .
C35 C 0.889(2) 1.2172(18) 0.6302(15) 0.087(7) Uani 1 1 d D . . . .
H35A H 0.892287 1.276921 0.653910 0.105 Uiso 1 1 calc R U . . .
H35B H 0.862014 1.209758 0.576115 0.105 Uiso 1 1 calc R U . . .
C36 C 1.009(2) 1.1850(18) 0.6469(11) 0.076(6) Uani 1 1 d D . . . .
H36A H 1.003116 1.124781 0.624723 0.092 Uiso 1 1 calc R U . . .
H36B H 1.063390 1.211304 0.623259 0.092 Uiso 1 1 calc R U . . .
C37 C 0.7074(18) 1.2197(12) 0.9707(10) 0.057(4) Uani 1 1 d D . . . .
H37A H 0.766704 1.190790 0.999475 0.069 Uiso 1 1 calc R U . . .
H37B H 0.637793 1.226413 0.994559 0.069 Uiso 1 1 calc R U . . .
C38 C 0.7607(17) 1.3035(13) 0.9750(13) 0.062(5) Uani 1 1 d D . . . .
H38A H 0.703278 1.332492 0.945123 0.074 Uiso 1 1 calc R U . . .
H38B H 0.776561 1.336228 1.026997 0.074 Uiso 1 1 calc R U . . .
C39 C 0.9278(19) 1.3761(11) 0.9581(14) 0.062(5) Uani 1 1 d D . . . .
H39A H 0.939998 1.407485 1.010412 0.075 Uiso 1 1 calc R U . . .
H39B H 0.879352 1.408445 0.926890 0.075 Uiso 1 1 calc R U . . .
C40 C 1.0451(19) 1.3624(14) 0.9363(11) 0.064(5) Uani 1 1 d D . . . .
H40A H 1.091247 1.416044 0.946887 0.077 Uiso 1 1 calc R U . . .
H40B H 1.091061 1.327182 0.965628 0.077 Uiso 1 1 calc R U . . .
C41 C 1.1390(19) 1.3149(17) 0.8383(13) 0.077(6) Uani 1 1 d D . . . .
H41A H 1.185179 1.274918 0.861787 0.092 Uiso 1 1 calc R U . . .
H41B H 1.186060 1.368582 0.853398 0.092 Uiso 1 1 calc R U . . .
C42 C 1.114(3) 1.2842(14) 0.7559(12) 0.078(7) Uani 1 1 d D . . . .
H42A H 1.059867 1.322159 0.734387 0.094 Uiso 1 1 calc R U . . .
H42B H 1.189239 1.287582 0.738978 0.094 Uiso 1 1 calc R U . . .
C43 C 0.6561(15) 1.0818(11) 0.9000(12) 0.051(4) Uani 1 1 d D . . . .
H43A H 0.602173 1.050282 0.854148 0.061 Uiso 1 1 calc R U . . .
H43B H 0.617837 1.079775 0.941933 0.061 Uiso 1 1 calc R U . . .
C44 C 0.7713(15) 1.0401(13) 0.9097(10) 0.049(4) Uani 1 1 d D . . . .
H44A H 0.826589 1.071282 0.955111 0.059 Uiso 1 1 calc R U . . .
H44B H 0.756227 0.983515 0.915214 0.059 Uiso 1 1 calc R U . . .
C45 C 0.9101(16) 0.9772(12) 0.8409(10) 0.049(4) Uani 1 1 d D . . . .
H45A H 0.873319 0.921708 0.836702 0.059 Uiso 1 1 calc R U . . .
H45B H 0.975062 0.990529 0.885465 0.059 Uiso 1 1 calc R U . . .
C46 C 0.9599(17) 0.9768(10) 0.7737(10) 0.047(4) Uani 1 1 d D . . . .
H46A H 1.018831 0.934256 0.768218 0.056 Uiso 1 1 calc R U . . .
H46B H 0.895113 0.963253 0.728978 0.056 Uiso 1 1 calc R U . . .
C47 C 1.0866(19) 1.0519(12) 0.7284(12) 0.056(5) Uani 1 1 d D . . . .
H47A H 1.037091 1.032434 0.677915 0.067 Uiso 1 1 calc R U . . .
H47B H 1.149083 1.012593 0.735282 0.067 Uiso 1 1 calc R U . . .
C48 C 1.143(2) 1.1365(11) 0.7374(13) 0.062(5) Uani 1 1 d D . . . .
H48A H 1.192852 1.154503 0.787915 0.074 Uiso 1 1 calc R U . . .
H48B H 1.196907 1.132699 0.702086 0.074 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'
K K 0.3868 1.0657 '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'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -4 12 0.0559
0 4 -12 0.0559
7 -2 -2 0.1387
-7 2 2 0.1297
7 0 -7 0.1305
4 0 8 0.1148
0 11 0 0.0932
2 -10 5 0.0860
-2 -9 -3 0.0750
5 -9 0 0.0992
3 -7 -6 0.0950
-4 8 4 0.1214
-5 1 10 0.1103
-7 -4 3 0.1281
6 5 -6 0.1438
-3 -9 6 0.0872
5 8 -3 0.1280
-6 6 3 0.1176
-5 4 9 0.1084
1 -1 12 0.0574
-4 -6 10 0.0850
0 -11 4 0.0519
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
N1 U1 Si3 121.1(4) . . ?
N1 U1 N3 90.5(5) . . ?
N1 U1 N4 94.4(4) . . ?
N1 U1 N5 130.2(5) . . ?
N2 U1 Si3 143.2(4) . . ?
N2 U1 N1 37.1(5) . . ?
N2 U1 N3 102.0(5) . . ?
N2 U1 N4 116.3(4) . . ?
N2 U1 N5 94.4(5) . . ?
N3 U1 Si3 108.1(3) . . ?
N3 U1 N5 117.4(4) . . ?
N4 U1 Si3 28.1(3) . . ?
N4 U1 N3 120.9(4) . . ?
N4 U1 N5 103.2(5) . . ?
N5 U1 Si3 90.1(4) . . ?
N3 Si1 C13 112.1(7) . . ?
N3 Si1 C14 115.1(7) . . ?
N3 Si1 C15 113.2(9) . . ?
C13 Si1 C15 105.4(10) . . ?
C14 Si1 C13 105.7(8) . . ?
C14 Si1 C15 104.5(8) . . ?
N3 Si2 C16 115.1(9) . . ?
N3 Si2 C17 112.5(9) . . ?
N3 Si2 C18 108.9(8) . . ?
C16 Si2 C17 106.3(11) . . ?
C16 Si2 C18 104.3(10) . . ?
C18 Si2 C17 109.5(12) . . ?
N4 Si3 U1 38.5(4) . . ?
N4 Si3 C19 115.2(9) . . ?
N4 Si3 C20 106.6(9) . . ?
N4 Si3 C21 117.4(12) . . ?
C19 Si3 U1 129.5(9) . . ?
C19 Si3 C20 109.0(12) . . ?
C20 Si3 U1 68.1(7) . . ?
C21 Si3 U1 125.5(9) . . ?
C21 Si3 C19 104.6(13) . . ?
C21 Si3 C20 103.2(11) . . ?
N4 Si4 C22 111.2(9) . . ?
N4 Si4 C23 114.6(8) . . ?
N4 Si4 C24 114.5(8) . . ?
C22 Si4 C23 105.9(10) . . ?
C22 Si4 C24 106.7(9) . . ?
C24 Si4 C23 103.3(11) . . ?
N5 Si5 C25 112.5(9) . . ?
N5 Si5 C26 111.0(7) . . ?
N5 Si5 C27 114.8(10) . . ?
C26 Si5 C25 109.4(10) . . ?
C27 Si5 C25 106.3(10) . . ?
C27 Si5 C26 102.4(10) . . ?
N5 Si6 C28 111.0(8) . . ?
N5 Si6 C29 112.0(10) . . ?
N5 Si6 C30 113.0(11) . . ?
C28 Si6 C29 107.0(11) . . ?
C28 Si6 C30 109.2(12) . . ?
C30 Si6 C29 104.3(13) . . ?
N2 N1 U1 69.9(7) . . ?
C1 N1 U1 136.7(11) . . ?
C1 N1 N2 120.5(12) . . ?
N1 N2 U1 73.0(7) . . ?
C7 N2 U1 149.0(10) . . ?
C7 N2 N1 120.4(12) . . ?
Si1 N3 U1 121.0(5) . . ?
Si2 N3 U1 123.5(6) . . ?
Si2 N3 Si1 115.3(7) . . ?
Si3 N4 U1 113.4(5) . . ?
Si4 N4 U1 129.4(6) . . ?
Si4 N4 Si3 117.2(8) . . ?
Si5 N5 U1 122.9(6) . . ?
Si5 N5 Si6 116.8(7) . . ?
Si6 N5 U1 120.3(6) . . ?
C6 C1 N1 121.2(9) . . ?
C6 C1 C2 120.0 . . ?
C2 C1 N1 118.7(9) . . ?
C5 C6 C1 120.0 . . ?
C6 C5 C4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C2 C3 C4 120.0 . . ?
C3 C2 C1 120.0 . . ?
N2 C7 C12 124.3(9) . . ?
N2 C7 C8 115.6(9) . . ?
C12 C7 C8 120.0 . . ?
C11 C12 C7 120.0 . . ?
C12 C11 C10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C10 C9 C8 120.0 . . ?
C9 C8 C7 120.0 . . ?
O1 K1 O2 61.7(4) . . ?
O1 K1 O3 100.7(4) . . ?
O1 K1 O4 126.1(5) . . ?
O1 K1 N6 59.9(4) . . ?
O1 K1 N7 120.0(5) . . ?
O2 K1 N6 120.8(5) . . ?
O2 K1 N7 58.9(5) . . ?
O3 K1 O2 140.8(5) . . ?
O3 K1 N6 60.9(4) . . ?
O3 K1 N7 119.8(4) . . ?
O4 K1 O2 100.6(5) . . ?
O4 K1 O3 59.7(4) . . ?
O4 K1 N6 120.1(4) . . ?
O4 K1 N7 60.6(4) . . ?
O5 K1 O1 91.1(5) . . ?
O5 K1 O2 113.6(5) . . ?
O5 K1 O3 100.7(4) . . ?
O5 K1 O4 138.9(5) . . ?
O5 K1 O6 60.0(3) . . ?
O5 K1 N6 60.2(4) . . ?
O5 K1 N7 119.2(4) . . ?
O6 K1 O1 125.6(5) . . ?
O6 K1 O2 87.4(4) . . ?
O6 K1 O3 127.6(4) . . ?
O6 K1 O4 101.5(4) . . ?
O6 K1 N6 120.0(4) . . ?
O6 K1 N7 59.4(4) . . ?
N6 K1 N7 179.3(5) . . ?
C32 O1 K1 117.8(12) . . ?
C33 O1 K1 111.9(13) . . ?
C33 O1 C32 115.4(19) . . ?
C34 O2 K1 111.9(14) . . ?
C35 O2 K1 115.4(14) . . ?
C35 O2 C34 113.3(19) . . ?
C38 O3 K1 116.6(12) . . ?
C39 O3 K1 115.2(12) . . ?
C39 O3 C38 113.4(15) . . ?
C40 O4 K1 114.8(11) . . ?
C40 O4 C41 110.6(17) . . ?
C41 O4 K1 116.8(13) . . ?
C44 O5 K1 116.9(11) . . ?
C44 O5 C45 113.4(13) . . ?
C45 O5 K1 118.3(10) . . ?
C46 O6 K1 113.1(10) . . ?
C47 O6 K1 121.7(11) . . ?
C47 O6 C46 110.3(13) . . ?
C31 N6 K1 109.0(12) . . ?
C31 N6 C37 108.8(16) . . ?
C37 N6 K1 107.4(10) . . ?
C43 N6 K1 109.0(10) . . ?
C43 N6 C31 113.3(17) . . ?
C43 N6 C37 109.1(15) . . ?
C36 N7 K1 110.4(14) . . ?
C36 N7 C42 111.5(19) . . ?
C36 N7 C48 108.5(17) . . ?
C42 N7 K1 105.6(13) . . ?
C42 N7 C48 113.2(19) . . ?
C48 N7 K1 107.6(11) . . ?
N6 C31 C32 109.9(18) . . ?
O1 C32 C31 113.8(19) . . ?
O1 C33 C34 109(2) . . ?
O2 C34 C33 112(2) . . ?
O2 C35 C36 109.5(19) . . ?
N7 C36 C35 113.5(19) . . ?
N6 C37 C38 115.2(17) . . ?
O3 C38 C37 111.3(16) . . ?
O3 C39 C40 108.5(16) . . ?
O4 C40 C39 110.3(18) . . ?
O4 C41 C42 107(2) . . ?
N7 C42 C41 116.6(18) . . ?
N6 C43 C44 114.2(15) . . ?
O5 C44 C43 109.9(14) . . ?
O5 C45 C46 109.9(14) . . ?
O6 C46 C45 109.1(15) . . ?
O6 C47 C48 109.1(15) . . ?
N7 C48 C47 115.1(18) . . ?
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
U1 Si3 3.417(5) . ?
U1 N1 2.271(14) . ?
U1 N2 2.229(13) . ?
U1 N3 2.342(13) . ?
U1 N4 2.318(13) . ?
U1 N5 2.366(12) . ?
Si1 N3 1.752(11) . ?
Si1 C13 1.863(13) . ?
Si1 C14 1.862(13) . ?
Si1 C15 1.879(13) . ?
Si2 N3 1.722(11) . ?
Si2 C16 1.876(13) . ?
Si2 C17 1.880(13) . ?
Si2 C18 1.876(13) . ?
Si3 N4 1.754(11) . ?
Si3 C19 1.872(13) . ?
Si3 C20 1.876(13) . ?
Si3 C21 1.849(14) . ?
Si4 N4 1.745(11) . ?
Si4 C22 1.866(12) . ?
Si4 C23 1.878(13) . ?
Si4 C24 1.878(13) . ?
Si5 N5 1.722(11) . ?
Si5 C25 1.881(13) . ?
Si5 C26 1.872(13) . ?
Si5 C27 1.868(13) . ?
Si6 N5 1.728(11) . ?
Si6 C28 1.864(13) . ?
Si6 C29 1.875(14) . ?
Si6 C30 1.873(14) . ?
N1 N2 1.431(19) . ?
N1 C1 1.407(13) . ?
N2 C7 1.385(14) . ?
C1 C6 1.3900 . ?
C1 C2 1.3900 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C7 C12 1.3900 . ?
C7 C8 1.3900 . ?
C12 C11 1.3900 . ?
C11 C10 1.3900 . ?
C10 C9 1.3900 . ?
C9 C8 1.3900 . ?
K1 O1 2.815(16) . ?
K1 O2 2.842(16) . ?
K1 O3 2.836(14) . ?
K1 O4 2.822(16) . ?
K1 O5 2.772(13) . ?
K1 O6 2.814(13) . ?
K1 N6 3.046(16) . ?
K1 N7 3.066(18) . ?
O1 C32 1.417(15) . ?
O1 C33 1.415(15) . ?
O2 C34 1.422(15) . ?
O2 C35 1.411(16) . ?
O3 C38 1.416(15) . ?
O3 C39 1.414(15) . ?
O4 C40 1.412(15) . ?
O4 C41 1.414(15) . ?
O5 C44 1.413(14) . ?
O5 C45 1.417(14) . ?
O6 C46 1.413(14) . ?
O6 C47 1.412(14) . ?
N6 C31 1.453(15) . ?
N6 C37 1.463(16) . ?
N6 C43 1.453(16) . ?
N7 C36 1.457(16) . ?
N7 C42 1.463(16) . ?
N7 C48 1.465(16) . ?
C31 C32 1.497(18) . ?
C33 C34 1.493(19) . ?
C35 C36 1.490(18) . ?
C37 C38 1.496(17) . ?
C39 C40 1.491(17) . ?
C41 C42 1.496(18) . ?
C43 C44 1.502(16) . ?
C45 C46 1.497(16) . ?
C47 C48 1.502(17) . ?
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
U1 Si3 N4 Si4 178.1(14) . . . . ?
U1 N1 N2 C7 -149.3(13) . . . . ?
U1 N1 C1 C6 -107.4(13) . . . . ?
U1 N1 C1 C2 75.2(16) . . . . ?
U1 N2 C7 C12 -117.5(17) . . . . ?
U1 N2 C7 C8 66(2) . . . . ?
N1 N2 C7 C12 -9.0(18) . . . . ?
N1 N2 C7 C8 174.9(11) . . . . ?
N1 C1 C6 C5 -177.3(13) . . . . ?
N1 C1 C2 C3 177.4(13) . . . . ?
N2 N1 C1 C6 -14.9(18) . . . . ?
N2 N1 C1 C2 167.7(11) . . . . ?
N2 C7 C12 C11 -175.9(13) . . . . ?
N2 C7 C8 C9 176.3(12) . . . . ?
C1 N1 N2 U1 -133.1(14) . . . . ?
C1 N1 N2 C7 77.6(18) . . . . ?
C1 C6 C5 C4 0.0 . . . . ?
C6 C1 C2 C3 0.0 . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C5 C4 C3 C2 0.0 . . . . ?
C4 C3 C2 C1 0.0 . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C7 C12 C11 C10 0.0 . . . . ?
C12 C7 C8 C9 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C10 C9 C8 C7 0.0 . . . . ?
C8 C7 C12 C11 0.0 . . . . ?
C13 Si1 N3 U1 11.5(12) . . . . ?
C13 Si1 N3 Si2 -172.7(9) . . . . ?
C14 Si1 N3 U1 -109.3(8) . . . . ?
C14 Si1 N3 Si2 66.6(11) . . . . ?
C15 Si1 N3 U1 130.6(9) . . . . ?
C15 Si1 N3 Si2 -53.6(11) . . . . ?
C16 Si2 N3 U1 143.9(10) . . . . ?
C16 Si2 N3 Si1 -31.9(13) . . . . ?
C17 Si2 N3 U1 -94.2(12) . . . . ?
C17 Si2 N3 Si1 90.1(12) . . . . ?
C18 Si2 N3 U1 27.3(13) . . . . ?
C18 Si2 N3 Si1 -148.4(11) . . . . ?
C19 Si3 N4 U1 -122.5(11) . . . . ?
C19 Si3 N4 Si4 55.6(14) . . . . ?
C20 Si3 N4 U1 -1.4(11) . . . . ?
C20 Si3 N4 Si4 176.7(10) . . . . ?
C21 Si3 N4 U1 113.6(10) . . . . ?
C21 Si3 N4 Si4 -68.3(12) . . . . ?
C22 Si4 N4 U1 94.3(11) . . . . ?
C22 Si4 N4 Si3 -83.4(11) . . . . ?
C23 Si4 N4 U1 -25.7(14) . . . . ?
C23 Si4 N4 Si3 156.6(11) . . . . ?
C24 Si4 N4 U1 -144.7(10) . . . . ?
C24 Si4 N4 Si3 37.6(13) . . . . ?
C25 Si5 N5 U1 103.0(11) . . . . ?
C25 Si5 N5 Si6 -76.2(12) . . . . ?
C26 Si5 N5 U1 -19.8(12) . . . . ?
C26 Si5 N5 Si6 161.0(9) . . . . ?
C27 Si5 N5 U1 -135.3(11) . . . . ?
C27 Si5 N5 Si6 45.5(13) . . . . ?
C28 Si6 N5 U1 -8.7(12) . . . . ?
C28 Si6 N5 Si5 170.5(9) . . . . ?
C29 Si6 N5 U1 -128.3(11) . . . . ?
C29 Si6 N5 Si5 51.0(13) . . . . ?
C30 Si6 N5 U1 114.3(13) . . . . ?
C30 Si6 N5 Si5 -66.4(14) . . . . ?
K1 O1 C32 C31 44(3) . . . . ?
K1 O1 C33 C34 -53(2) . . . . ?
K1 O2 C34 C33 -44(3) . . . . ?
K1 O2 C35 C36 59(3) . . . . ?
K1 O3 C38 C37 48(2) . . . . ?
K1 O3 C39 C40 -48(2) . . . . ?
K1 O4 C40 C39 -48(2) . . . . ?
K1 O4 C41 C42 54(2) . . . . ?
K1 O5 C44 C43 55.6(19) . . . . ?
K1 O5 C45 C46 -38(2) . . . . ?
K1 O6 C46 C45 -53.8(16) . . . . ?
K1 O6 C47 C48 43(2) . . . . ?
K1 N6 C31 C32 49(2) . . . . ?
K1 N6 C37 C38 43.6(18) . . . . ?
K1 N6 C43 C44 36.9(19) . . . . ?
K1 N7 C36 C35 36(3) . . . . ?
K1 N7 C42 C41 44(3) . . . . ?
K1 N7 C48 C47 47(2) . . . . ?
O1 C33 C34 O2 68(3) . . . . ?
O2 C35 C36 N7 -65(3) . . . . ?
O3 C39 C40 O4 65(3) . . . . ?
O4 C41 C42 N7 -68(3) . . . . ?
O5 C45 C46 O6 61(2) . . . . ?
O6 C47 C48 N7 -62(2) . . . . ?
N6 C31 C32 O1 -65(3) . . . . ?
N6 C37 C38 O3 -65(2) . . . . ?
N6 C43 C44 O5 -63(2) . . . . ?
C31 N6 C37 C38 -74(2) . . . . ?
C31 N6 C43 C44 158.4(17) . . . . ?
C32 O1 C33 C34 169(2) . . . . ?
C33 O1 C32 C31 180(2) . . . . ?
C34 O2 C35 C36 -170(2) . . . . ?
C35 O2 C34 C33 -177(2) . . . . ?
C36 N7 C42 C41 164(2) . . . . ?
C36 N7 C48 C47 -73(2) . . . . ?
C37 N6 C31 C32 165.5(18) . . . . ?
C37 N6 C43 C44 -80(2) . . . . ?
C38 O3 C39 C40 174.0(19) . . . . ?
C39 O3 C38 C37 -174.6(19) . . . . ?
C40 O4 C41 C42 -172.7(19) . . . . ?
C41 O4 C40 C39 176.8(19) . . . . ?
C42 N7 C36 C35 -81(3) . . . . ?
C42 N7 C48 C47 162.8(17) . . . . ?
C43 N6 C31 C32 -73(2) . . . . ?
C43 N6 C37 C38 161.7(16) . . . . ?
C44 O5 C45 C46 179.5(16) . . . . ?
C45 O5 C44 C43 -161.4(17) . . . . ?
C46 O6 C47 C48 179.6(17) . . . . ?
C47 O6 C46 C45 166.1(16) . . . . ?
C48 N7 C36 C35 154(2) . . . . ?
C48 N7 C42 C41 -73(3) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.658(3) 19215 7457 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.342(3) 0 7457 nmt 1.0005 0.0024 0.0024 -0.0162 -0.9754 0.0792 -0.6598
-0.0987 -1.0185
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
-0.1266 -4.2551 11.9753 -0.4342 -0.3702 0.8212
0.1266 4.2551 -11.9753 0.4342 0.3702 -0.8212
7.3665 -1.7526 -2.3456 0.6178 0.5291 0.5816
-7.3449 1.9694 1.7207 -0.5941 -0.5089 -0.6230
6.8473 0.0775 -6.9332 0.7430 0.6356 0.2096
4.1717 0.0825 8.2996 -0.2750 0.3201 0.9066
0.1967 10.5325 -0.2301 -0.6348 0.7428 -0.2128
2.0396 -10.1776 4.6608 0.4691 -0.5497 0.6912
-1.6671 -9.0640 -2.7838 0.6433 -0.7521 -0.1431
4.6307 -8.5456 -0.1546 0.7771 -0.1867 0.6011
2.8332 -7.4508 -6.2714 0.9721 -0.2328 0.0290
-3.8378 8.3432 3.6325 -0.9258 0.2220 -0.3060
-4.6565 1.2017 10.3208 -0.9084 -0.3771 0.1806
-6.9423 -3.7675 3.3682 -0.3107 -0.8779 -0.3644
6.3701 5.1090 -5.6486 0.3301 0.9333 0.1411
-3.1839 -9.4426 6.0889 0.0763 -0.9585 0.2746
4.9183 7.9810 -2.9622 -0.0784 0.9905 0.1129
-6.1836 5.7195 3.0398 -0.8461 -0.1579 -0.5091
-4.5713 3.8048 8.8616 -0.9822 -0.1826 0.0442
0.7753 -1.4906 11.7029 -0.5456 -0.1005 0.8320
-3.5108 -6.4252 10.4824 -0.3833 -0.8036 0.4553
-0.4527 -10.7774 3.7191 0.4351 -0.8011 0.4110
