#------------------------------------------------------------------------------
#$Date: 2021-10-06 18:38:01 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269716 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/78/7707884.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_7707884
loop_
_publ_author_name
'Wang, Shichun'
'Heng, Yi'
'Li, Tongyu'
'Hou, Guohua'
'Zi, Guofu'
'Walter, Marc D.'
_publ_section_title
;
 Synthesis and reactivity of the uranium phosphinidene metallocene
 [η⁵-1,3-(Me₃Si)₂C₅H₃]₂U(P-2,4,6-ⁱPr₃C₆H₂)(OPMe₃):
 influence of the coordinated Lewis base.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12502
_journal_page_last               12516
_journal_paper_doi               10.1039/d1dt02149d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C25 H51 Cl O P Si4 U'
_chemical_formula_sum            'C25 H51 Cl O P Si4 U'
_chemical_formula_weight         784.46
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.176(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5325(3)
_cell_length_b                   12.6083(3)
_cell_length_c                   30.1952(7)
_cell_measurement_reflns_used    11836
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.5930
_cell_measurement_theta_min      2.8940
_cell_volume                     4006.94(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00 -57.00   0.50    0.56    --  -47.70 134.00 -26.00   50
  2  ω   -116.00 -91.00   0.50    0.56    --  -47.70-135.00  86.00   50
  3  ω    -99.00 -74.00   0.50    0.56    --  -47.70-134.00 -94.00   50
  4  ω     24.00  93.00   0.50    0.56    --   47.70-134.00 -94.00  138
  5  ω     71.00  96.00   0.50    0.56    --   47.70 134.00 -26.00   50
  6  ω     37.00  62.00   0.50    0.56    --   47.70-135.00  86.00   50
  7  ω   -144.00 -95.00   0.50    1.00    -- -102.00-135.00  86.00   98
  8  ω   -101.00 -76.00   0.50    1.00    -- -102.00 135.00 152.00   50
  9  ω   -123.00 -77.00   0.50    1.00    -- -102.00 134.00 -26.00   92
 10  ω     54.00  79.00   0.50    1.00    --  104.75-135.00  86.00   50
 11  ω     99.00 124.00   0.50    1.00    --  104.75 135.00 152.00   50
 12  ω     54.00  79.00   0.50    1.00    --  104.75-134.00 -94.00   50
 13  ω   -119.00 -73.00   0.50    0.56    --  -47.70-125.00-150.00   92
 14  ω    -24.00  58.00   0.50    0.56    --   47.70 -37.00 -60.00  164
 15  ω     36.00  75.00   0.50    0.56    --   47.70  37.00  90.00   78
 16  ω     81.00 118.00   0.50    0.56    --   47.70  37.00  90.00   74
 17  ω   -115.00 -52.00   0.50    1.00    -- -102.00 125.00-150.00  126
 18  ω   -175.00 -88.00   0.50    1.00    -- -102.00 -15.00  60.00  174
 19  ω     47.00 108.00   0.50    1.00    --  104.75 -94.00  60.00  122
 20  ω     64.00  99.00   0.50    1.00    --  104.75 -94.00-180.00   70
 21  ω    121.00 176.00   0.50    1.00    --  104.75  45.00 -30.00  110
 22  ω     41.00 114.00   0.50    1.00    --  104.75 -45.00-150.00  146
 23  ω     34.00 118.00   0.50    1.00    --  104.75 -30.00  30.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1252483000
_diffrn_orient_matrix_UB_12      0.0611450000
_diffrn_orient_matrix_UB_13      0.0082130000
_diffrn_orient_matrix_UB_21      0.0722306000
_diffrn_orient_matrix_UB_22      -0.1057743000
_diffrn_orient_matrix_UB_23      0.0054786000
_diffrn_orient_matrix_UB_31      0.0228533000
_diffrn_orient_matrix_UB_32      -0.0012261000
_diffrn_orient_matrix_UB_33      -0.0500922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28157
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.707
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0422P)²+12.6932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7202
_reflns_number_total             8002
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02149d2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7707884--7707891.cif.'
_cod_database_code               7707884
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1Si1U1P1O1
_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   0.343
_shelx_estimated_absorpt_t_min   0.234
_diffrn_oxdiff_digest_frames
;
019e4d2a0031bc14aaa9ee276727eec02b021024ecb
;
_diffrn_oxdiff_digest_hkl
;
01e61a82261f21aed5794364d0c3a121ae88ca
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17B) = Uanis(C18A) = Uanis(C18B) = Uanis(C19A) =
Uanis(C19B)
3. Others
 Fixed Sof: C17A(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18A(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19A(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C17B(0.5)
 H17D(0.5) H17E(0.5) H17F(0.5) C18B(0.5) H18D(0.5) H18E(0.5) H18F(0.5)
 C19B(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20A(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22A(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C20B(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C21B(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
 Si3A(0.5) Si4A(0.5) Si3B(0.5) Si4B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C),
 C19A(H19A,H19B,H19C), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,
 H19E,H19F), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C),
 C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_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 3.121
_oxdiff_exptl_absorpt_empirical_full_min 0.690
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6964(6) 0.5210(4) 0.31737(19) 0.0352(12) Uani 1 1 d . . . . .
C2 C 0.6597(5) 0.6229(4) 0.33175(17) 0.0320(11) Uani 1 1 d . . . . .
H2 H 0.6325 0.6775 0.3130 0.038 Uiso 1 1 calc R . . . .
C3 C 0.6697(5) 0.6306(4) 0.37852(17) 0.0337(11) Uani 1 1 d . . . . .
C4 C 0.7168(5) 0.5304(5) 0.39369(18) 0.0349(11) Uani 1 1 d . . . . .
H4 H 0.7354 0.5121 0.4231 0.042 Uiso 1 1 calc R . . . .
C5 C 0.7305(5) 0.4640(5) 0.35666(18) 0.0373(12) Uani 1 1 d . . . . .
H5 H 0.7576 0.3938 0.3578 0.045 Uiso 1 1 calc R . . . .
C6 C 0.7243(7) 0.3307(5) 0.2557(2) 0.0501(16) Uani 1 1 d . . . . .
H6A H 0.7921 0.3028 0.2744 0.075 Uiso 1 1 calc GR . . . .
H6B H 0.7363 0.3095 0.2256 0.075 Uiso 1 1 calc GR . . . .
H6C H 0.6446 0.3037 0.2653 0.075 Uiso 1 1 calc GR . . . .
C7 C 0.6040(7) 0.5360(5) 0.2197(2) 0.0478(15) Uani 1 1 d . . . . .
H7A H 0.5224 0.5051 0.2247 0.072 Uiso 1 1 calc GR . . . .
H7B H 0.6276 0.5213 0.1900 0.072 Uiso 1 1 calc GR . . . .
H7C H 0.5998 0.6113 0.2241 0.072 Uiso 1 1 calc GR . . . .
C8 C 0.8847(7) 0.5257(6) 0.2442(2) 0.0567(18) Uani 1 1 d . . . . .
H8A H 0.8874 0.6017 0.2457 0.085 Uiso 1 1 calc GR . . . .
H8B H 0.9014 0.5033 0.2146 0.085 Uiso 1 1 calc GR . . . .
H8C H 0.9479 0.4965 0.2644 0.085 Uiso 1 1 calc GR . . . .
C9 C 0.7171(11) 0.8648(5) 0.3821(2) 0.080(3) Uani 1 1 d . . . . .
H9A H 0.8017 0.8473 0.3739 0.120 Uiso 1 1 calc GR . . . .
H9B H 0.7195 0.9266 0.4007 0.120 Uiso 1 1 calc GR . . . .
H9C H 0.6653 0.8789 0.3559 0.120 Uiso 1 1 calc GR . . . .
C10 C 0.7349(7) 0.7355(6) 0.46746(19) 0.0540(17) Uani 1 1 d . . . . .
H10A H 0.6941 0.6813 0.4842 0.081 Uiso 1 1 calc GR . . . .
H10B H 0.7333 0.8012 0.4835 0.081 Uiso 1 1 calc GR . . . .
H10C H 0.8213 0.7154 0.4629 0.081 Uiso 1 1 calc GR . . . .
C11 C 0.4786(7) 0.7818(7) 0.4220(3) 0.076(3) Uani 1 1 d . . . . .
H11A H 0.4317 0.7817 0.3941 0.114 Uiso 1 1 calc GR . . . .
H11B H 0.4718 0.8503 0.4356 0.114 Uiso 1 1 calc GR . . . .
H11C H 0.4444 0.7289 0.4410 0.114 Uiso 1 1 calc GR . . . .
C12 C 0.4625(5) 0.3185(5) 0.4213(2) 0.0390(13) Uani 1 1 d . . . . .
C13 C 0.3369(6) 0.3320(5) 0.40521(17) 0.0401(13) Uani 1 1 d . . . . .
H13 H 0.2925 0.2840 0.3871 0.048 Uiso 1 1 calc R . . . .
C14 C 0.2878(7) 0.4286(6) 0.4205(2) 0.0552(19) Uani 1 1 d . . . . .
C15 C 0.3841(10) 0.4744(5) 0.4470(2) 0.066(2) Uani 1 1 d . . . . .
H15 H 0.3790 0.5392 0.4616 0.079 Uiso 1 1 calc R . . . .
C16 C 0.4894(7) 0.4075(6) 0.44803(19) 0.056(2) Uani 1 1 d . . . . .
H16 H 0.5653 0.4197 0.4639 0.068 Uiso 1 1 calc R . . . .
C17A C 0.5594(15) 0.1110(13) 0.4603(5) 0.0490(14) Uani 0.5 1 d . . P A 1
H17A H 0.6230 0.1479 0.4779 0.074 Uiso 0.5 1 calc GR . P A 1
H17B H 0.5874 0.0399 0.4549 0.074 Uiso 0.5 1 calc GR . P A 1
H17C H 0.4815 0.1092 0.4758 0.074 Uiso 0.5 1 calc GR . P A 1
C18A C 0.4203(14) 0.1015(10) 0.3693(4) 0.0490(14) Uani 0.5 1 d . . P A 1
H18A H 0.3398 0.0958 0.3829 0.074 Uiso 0.5 1 calc GR . P A 1
H18B H 0.4550 0.0319 0.3652 0.074 Uiso 0.5 1 calc GR . P A 1
H18C H 0.4090 0.1358 0.3410 0.074 Uiso 0.5 1 calc GR . P A 1
C19A C 0.6855(14) 0.1898(11) 0.3783(4) 0.0490(14) Uani 0.5 1 d . . P A 1
H19A H 0.6729 0.2235 0.3499 0.074 Uiso 0.5 1 calc GR . P A 1
H19B H 0.7185 0.1196 0.3742 0.074 Uiso 0.5 1 calc GR . P A 1
H19C H 0.7446 0.2305 0.3963 0.074 Uiso 0.5 1 calc GR . P A 1
C17B C 0.5114(15) 0.0960(13) 0.4550(5) 0.0490(14) Uani 0.5 1 d . . P B 2
H17D H 0.4882 0.1185 0.4839 0.074 Uiso 0.5 1 calc GR . P B 2
H17E H 0.5728 0.0399 0.4577 0.074 Uiso 0.5 1 calc GR . P B 2
H17F H 0.4373 0.0709 0.4387 0.074 Uiso 0.5 1 calc GR . P B 2
C18B C 0.6034(15) 0.1676(11) 0.3655(4) 0.0490(14) Uani 0.5 1 d . . P B 2
H18D H 0.5232 0.1448 0.3527 0.074 Uiso 0.5 1 calc GR . P B 2
H18E H 0.6628 0.1098 0.3652 0.074 Uiso 0.5 1 calc GR . P B 2
H18F H 0.6352 0.2257 0.3486 0.074 Uiso 0.5 1 calc GR . P B 2
C19B C 0.7354(13) 0.2516(10) 0.4517(4) 0.0490(14) Uani 0.5 1 d . . P B 2
H19D H 0.7695 0.3110 0.4362 0.074 Uiso 0.5 1 calc GR . P B 2
H19E H 0.7940 0.1934 0.4510 0.074 Uiso 0.5 1 calc GR . P B 2
H19F H 0.7220 0.2712 0.4818 0.074 Uiso 0.5 1 calc GR . P B 2
C20A C 0.0708(12) 0.4174(13) 0.3436(4) 0.047(3) Uani 0.5 1 d . . P C 1
H20A H 0.1315 0.4536 0.3261 0.071 Uiso 0.5 1 calc GR . P C 1
H20B H -0.0132 0.4417 0.3354 0.071 Uiso 0.5 1 calc GR . P C 1
H20C H 0.0764 0.3424 0.3384 0.071 Uiso 0.5 1 calc GR . P C 1
C21A C 0.0030(11) 0.3605(10) 0.4382(4) 0.041(3) Uani 0.5 1 d . . P C 1
H21A H 0.0042 0.2889 0.4274 0.062 Uiso 0.5 1 calc GR . P C 1
H21B H -0.0826 0.3869 0.4365 0.062 Uiso 0.5 1 calc GR . P C 1
H21C H 0.0346 0.3619 0.4684 0.062 Uiso 0.5 1 calc GR . P C 1
C22A C 0.0767(14) 0.5889(11) 0.4170(4) 0.050(3) Uani 0.5 1 d . . P C 1
H22A H 0.0782 0.5981 0.4486 0.075 Uiso 0.5 1 calc GR . P C 1
H22B H -0.0047 0.6102 0.4046 0.075 Uiso 0.5 1 calc GR . P C 1
H22C H 0.1419 0.6316 0.4046 0.075 Uiso 0.5 1 calc GR . P C 1
C20B C 0.0636(12) 0.4782(14) 0.3651(4) 0.051(4) Uani 0.5 1 d . . P D 2
H20D H 0.1145 0.5096 0.3429 0.076 Uiso 0.5 1 calc GR . P D 2
H20E H -0.0197 0.5092 0.3636 0.076 Uiso 0.5 1 calc GR . P D 2
H20F H 0.0570 0.4032 0.3600 0.076 Uiso 0.5 1 calc GR . P D 2
C21B C 0.0402(12) 0.4391(14) 0.4639(4) 0.054(4) Uani 0.5 1 d . . P D 2
H21D H 0.0423 0.3635 0.4602 0.081 Uiso 0.5 1 calc GR . P D 2
H21E H -0.0458 0.4637 0.4601 0.081 Uiso 0.5 1 calc GR . P D 2
H21F H 0.0728 0.4572 0.4930 0.081 Uiso 0.5 1 calc GR . P D 2
C22B C 0.1514(14) 0.6467(12) 0.4351(5) 0.056(4) Uani 0.5 1 d . . P D 2
H22D H 0.1820 0.6553 0.4652 0.084 Uiso 0.5 1 calc GR . P D 2
H22E H 0.0690 0.6787 0.4314 0.084 Uiso 0.5 1 calc GR . P D 2
H22F H 0.2091 0.6803 0.4156 0.084 Uiso 0.5 1 calc GR . P D 2
C23 C 0.2378(7) 0.6197(5) 0.2511(2) 0.0522(16) Uani 1 1 d . . . . .
H23A H 0.1762 0.5659 0.2571 0.078 Uiso 1 1 calc GR . . . .
H23B H 0.3140 0.5869 0.2412 0.078 Uiso 1 1 calc GR . . . .
H23C H 0.2041 0.6663 0.2284 0.078 Uiso 1 1 calc GR . . . .
C24 C 0.1280(8) 0.7459(7) 0.3180(2) 0.070(2) Uani 1 1 d . . . . .
H24A H 0.0868 0.7843 0.2941 0.106 Uiso 1 1 calc GR . . . .
H24B H 0.1441 0.7928 0.3426 0.106 Uiso 1 1 calc GR . . . .
H24C H 0.0742 0.6889 0.3269 0.106 Uiso 1 1 calc GR . . . .
C25 C 0.3723(8) 0.8013(6) 0.2850(3) 0.071(2) Uani 1 1 d . . . . .
H25A H 0.4528 0.7743 0.2763 0.107 Uiso 1 1 calc GR . . . .
H25B H 0.3851 0.8483 0.3098 0.107 Uiso 1 1 calc GR . . . .
H25C H 0.3323 0.8392 0.2607 0.107 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.39791(14) 0.36967(11) 0.29238(4) 0.0409(3) Uani 1 1 d . . . . .
O1 O 0.3384(3) 0.6260(3) 0.33585(12) 0.0350(8) Uani 1 1 d . . . . .
P1 P 0.27320(14) 0.69372(12) 0.30037(5) 0.0366(3) Uani 1 1 d . . . . .
Si1 Si 0.72416(16) 0.47826(13) 0.25930(5) 0.0375(3) Uani 1 1 d . . . . .
Si2 Si 0.64897(16) 0.75185(12) 0.41271(5) 0.0356(3) Uani 1 1 d . . . . .
Si3A Si 0.5324(4) 0.1817(3) 0.40581(12) 0.0366(7) Uani 0.5 1 d . . P A 1
Si4A Si 0.1053(3) 0.4454(3) 0.40360(11) 0.0361(7) Uani 0.5 1 d . . P C 1
Si3B Si 0.5821(3) 0.2116(2) 0.42453(11) 0.0308(6) Uani 0.5 1 d . . P B 2
Si4B Si 0.1400(3) 0.5029(3) 0.42163(12) 0.0412(8) Uani 0.5 1 d . . P D 2
U1 U 0.47196(2) 0.48870(2) 0.36264(2) 0.02585(7) Uani 1 1 d . . . . .
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'
Cl Cl 0.3639 0.7018 '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'
P P 0.2955 0.4335 '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_
_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
C2 C1 C5 105.4(5) . . ?
C2 C1 Si1 127.2(4) . . ?
C2 C1 U1 74.7(3) . . ?
C5 C1 Si1 126.5(4) . . ?
C5 C1 U1 73.2(3) . . ?
Si1 C1 U1 125.5(3) . . ?
C1 C2 H2 124.5 . . ?
C1 C2 C3 111.0(5) . . ?
C1 C2 U1 76.0(3) . . ?
C3 C2 H2 124.5 . . ?
C3 C2 U1 74.7(3) . . ?
U1 C2 H2 116.6 . . ?
C2 C3 C4 105.7(5) . . ?
C2 C3 Si2 127.1(4) . . ?
C2 C3 U1 75.9(3) . . ?
C4 C3 Si2 126.6(4) . . ?
C4 C3 U1 74.6(3) . . ?
Si2 C3 U1 121.5(3) . . ?
C3 C4 H4 125.8 . . ?
C3 C4 U1 75.6(3) . . ?
C5 C4 C3 108.4(5) . . ?
C5 C4 H4 125.8 . . ?
C5 C4 U1 74.9(3) . . ?
U1 C4 H4 115.9 . . ?
C1 C5 H5 125.3 . . ?
C1 C5 U1 77.2(3) . . ?
C4 C5 C1 109.4(5) . . ?
C4 C5 H5 125.3 . . ?
C4 C5 U1 75.5(3) . . ?
U1 C5 H5 114.1 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
C13 C12 C16 105.6(6) . . ?
C13 C12 Si3A 112.7(5) . . ?
C13 C12 Si3B 137.7(5) . . ?
C13 C12 U1 75.0(3) . . ?
C16 C12 Si3A 141.2(5) . . ?
C16 C12 Si3B 115.6(5) . . ?
C16 C12 U1 74.9(3) . . ?
Si3A C12 U1 120.5(3) . . ?
Si3B C12 U1 123.7(3) . . ?
C12 C13 H13 124.9 . . ?
C12 C13 C14 110.2(6) . . ?
C12 C13 U1 75.8(3) . . ?
C14 C13 H13 124.9 . . ?
C14 C13 U1 74.8(4) . . ?
U1 C13 H13 116.4 . . ?
C13 C14 Si4A 111.9(6) . . ?
C13 C14 Si4B 141.1(7) . . ?
C13 C14 U1 75.8(3) . . ?
C15 C14 C13 106.2(6) . . ?
C15 C14 Si4A 141.4(6) . . ?
C15 C14 Si4B 112.3(6) . . ?
C15 C14 U1 74.7(4) . . ?
Si4A C14 U1 120.4(3) . . ?
Si4B C14 U1 119.5(3) . . ?
C14 C15 H15 125.6 . . ?
C14 C15 U1 76.0(4) . . ?
C16 C15 C14 108.8(6) . . ?
C16 C15 H15 125.6 . . ?
C16 C15 U1 76.4(4) . . ?
U1 C15 H15 114.2 . . ?
C12 C16 H16 125.4 . . ?
C12 C16 U1 75.9(3) . . ?
C15 C16 C12 109.2(6) . . ?
C15 C16 H16 125.4 . . ?
C15 C16 U1 74.4(3) . . ?
U1 C16 H16 116.3 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
Si3A C17A H17A 109.5 . . ?
Si3A C17A H17B 109.5 . . ?
Si3A C17A H17C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
Si3A C18A H18A 109.5 . . ?
Si3A C18A H18B 109.5 . . ?
Si3A C18A H18C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
Si3A C19A H19A 109.5 . . ?
Si3A C19A H19B 109.5 . . ?
Si3A C19A H19C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
Si3B C17B H17D 109.5 . . ?
Si3B C17B H17E 109.5 . . ?
Si3B C17B H17F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
Si3B C18B H18D 109.5 . . ?
Si3B C18B H18E 109.5 . . ?
Si3B C18B H18F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
Si3B C19B H19D 109.5 . . ?
Si3B C19B H19E 109.5 . . ?
Si3B C19B H19F 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
Si4A C20A H20A 109.5 . . ?
Si4A C20A H20B 109.5 . . ?
Si4A C20A H20C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
Si4A C21A H21A 109.5 . . ?
Si4A C21A H21B 109.5 . . ?
Si4A C21A H21C 109.5 . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
Si4A C22A H22A 109.5 . . ?
Si4A C22A H22B 109.5 . . ?
Si4A C22A H22C 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
Si4B C20B H20D 109.5 . . ?
Si4B C20B H20E 109.5 . . ?
Si4B C20B H20F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
Si4B C21B H21D 109.5 . . ?
Si4B C21B H21E 109.5 . . ?
Si4B C21B H21F 109.5 . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
Si4B C22B H22D 109.5 . . ?
Si4B C22B H22E 109.5 . . ?
Si4B C22B H22F 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
P1 C23 H23A 109.5 . . ?
P1 C23 H23B 109.5 . . ?
P1 C23 H23C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P1 C24 H24A 109.5 . . ?
P1 C24 H24B 109.5 . . ?
P1 C24 H24C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
P1 C25 H25A 109.5 . . ?
P1 C25 H25B 109.5 . . ?
P1 C25 H25C 109.5 . . ?
P1 O1 U1 155.1(2) . . ?
C24 P1 C23 106.9(4) . . ?
C24 P1 C25 108.5(4) . . ?
C25 P1 C23 106.7(4) . . ?
O1 P1 C23 111.7(3) . . ?
O1 P1 C24 111.8(3) . . ?
O1 P1 C25 111.0(3) . . ?
C6 Si1 C1 110.1(3) . . ?
C6 Si1 C8 107.6(3) . . ?
C7 Si1 C1 111.4(3) . . ?
C7 Si1 C6 110.9(3) . . ?
C7 Si1 C8 108.6(3) . . ?
C8 Si1 C1 108.2(3) . . ?
C3 Si2 C10 109.7(3) . . ?
C3 Si2 C11 112.5(3) . . ?
C9 Si2 C3 107.3(3) . . ?
C9 Si2 C10 110.0(4) . . ?
C9 Si2 C11 108.1(5) . . ?
C10 Si2 C11 109.1(4) . . ?
C17A Si3A C12 104.8(6) . . ?
C18A Si3A C12 112.6(5) . . ?
C18A Si3A C17A 109.2(6) . . ?
C19A Si3A C12 114.0(5) . . ?
C19A Si3A C17A 108.3(7) . . ?
C19A Si3A C18A 107.8(6) . . ?
C20A Si4A C14 112.4(5) . . ?
C20A Si4A C22A 111.3(7) . . ?
C21A Si4A C14 111.7(4) . . ?
C21A Si4A C20A 109.8(6) . . ?
C21A Si4A C22A 109.3(6) . . ?
C22A Si4A C14 102.1(5) . . ?
C12 Si3B C17B 107.9(6) . . ?
C12 Si3B C18B 105.7(5) . . ?
C12 Si3B C19B 113.9(5) . . ?
C18B Si3B C17B 107.2(7) . . ?
C19B Si3B C17B 110.4(6) . . ?
C19B Si3B C18B 111.4(6) . . ?
C14 Si4B C20B 103.5(6) . . ?
C14 Si4B C21B 107.2(5) . . ?
C14 Si4B C22B 117.3(6) . . ?
C21B Si4B C20B 108.4(6) . . ?
C22B Si4B C20B 112.4(7) . . ?
C22B Si4B C21B 107.7(7) . . ?
C2 U1 C1 29.29(15) . . ?
C3 U1 C1 49.40(15) . . ?
C3 U1 C2 29.48(15) . . ?
C3 U1 C12 115.54(17) . . ?
C3 U1 C13 140.63(16) . . ?
C3 U1 C16 93.14(17) . . ?
C4 U1 C1 49.01(16) . . ?
C4 U1 C2 48.17(16) . . ?
C4 U1 C3 29.86(16) . . ?
C4 U1 C12 89.20(17) . . ?
C4 U1 C13 117.81(17) . . ?
C4 U1 C14 120.44(19) . . ?
C4 U1 C16 74.15(18) . . ?
C5 U1 C1 29.61(17) . . ?
C5 U1 C2 48.03(17) . . ?
C5 U1 C3 49.17(17) . . ?
C5 U1 C4 29.60(16) . . ?
C5 U1 C12 90.80(17) . . ?
C5 U1 C13 118.36(18) . . ?
C5 U1 C14 136.87(18) . . ?
C5 U1 C16 89.3(2) . . ?
C12 U1 C1 118.21(17) . . ?
C12 U1 C2 136.24(17) . . ?
C13 U1 C1 141.68(18) . . ?
C13 U1 C2 165.44(17) . . ?
C13 U1 C12 29.21(17) . . ?
C14 U1 C1 166.43(18) . . ?
C14 U1 C2 154.3(2) . . ?
C14 U1 C3 127.5(2) . . ?
C14 U1 C12 49.04(17) . . ?
C14 U1 C13 29.41(19) . . ?
C14 U1 C16 48.3(2) . . ?
C15 U1 C1 141.3(2) . . ?
C15 U1 C2 128.1(2) . . ?
C15 U1 C3 99.1(2) . . ?
C15 U1 C4 92.3(2) . . ?
C15 U1 C5 115.0(2) . . ?
C15 U1 C12 48.62(19) . . ?
C15 U1 C13 47.8(2) . . ?
C15 U1 C14 29.3(2) . . ?
C15 U1 C16 29.2(2) . . ?
C16 U1 C1 118.6(2) . . ?
C16 U1 C2 120.80(17) . . ?
C16 U1 C12 29.23(19) . . ?
C16 U1 C13 47.49(17) . . ?
Cl1 U1 C1 85.48(11) . . ?
Cl1 U1 C2 105.23(11) . . ?
Cl1 U1 C3 133.60(11) . . ?
Cl1 U1 C4 127.82(12) . . ?
Cl1 U1 C5 98.23(12) . . ?
Cl1 U1 C12 93.20(14) . . ?
Cl1 U1 C13 80.20(12) . . ?
Cl1 U1 C14 98.95(18) . . ?
Cl1 U1 C15 126.63(18) . . ?
Cl1 U1 C16 122.27(14) . . ?
O1 U1 C1 103.27(15) . . ?
O1 U1 C2 82.02(15) . . ?
O1 U1 C3 91.16(15) . . ?
O1 U1 C4 120.98(15) . . ?
O1 U1 C5 129.80(16) . . ?
O1 U1 C12 138.52(15) . . ?
O1 U1 C13 111.84(16) . . ?
O1 U1 C14 89.66(15) . . ?
O1 U1 C15 98.5(2) . . ?
O1 U1 C16 127.5(2) . . ?
O1 U1 Cl1 89.30(10) . . ?
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
C1 C2 1.414(7) . ?
C1 C5 1.421(8) . ?
C1 Si1 1.868(6) . ?
C1 U1 2.805(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.415(7) . ?
C2 U1 2.789(5) . ?
C3 C4 1.426(8) . ?
C3 Si2 1.862(6) . ?
C3 U1 2.774(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.409(8) . ?
C4 U1 2.761(5) . ?
C5 H5 0.9300 . ?
C5 U1 2.754(6) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 Si1 1.864(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 Si1 1.856(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 Si1 1.867(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 Si2 1.857(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 Si2 1.866(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 Si2 1.866(8) . ?
C12 C13 1.403(8) . ?
C12 C16 1.403(9) . ?
C12 Si3A 1.940(7) . ?
C12 Si3B 1.846(6) . ?
C12 U1 2.787(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.407(9) . ?
C13 U1 2.778(5) . ?
C14 C15 1.394(12) . ?
C14 Si4A 1.980(8) . ?
C14 Si4B 1.818(7) . ?
C14 U1 2.765(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(12) . ?
C15 U1 2.748(7) . ?
C16 H16 0.9300 . ?
C16 U1 2.774(5) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A Si3A 1.883(16) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A Si3A 1.880(14) . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
C19A Si3A 1.845(14) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B Si3B 1.891(16) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B Si3B 1.888(13) . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
C19B Si3B 1.852(14) . ?
C20A H20A 0.9600 . ?
C20A H20B 0.9600 . ?
C20A H20C 0.9600 . ?
C20A Si4A 1.868(13) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
C21A Si4A 1.867(12) . ?
C22A H22A 0.9600 . ?
C22A H22B 0.9600 . ?
C22A H22C 0.9600 . ?
C22A Si4A 1.881(14) . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?
C20B Si4B 1.886(13) . ?
C21B H21D 0.9600 . ?
C21B H21E 0.9600 . ?
C21B H21F 0.9600 . ?
C21B Si4B 1.865(13) . ?
C22B H22D 0.9600 . ?
C22B H22E 0.9600 . ?
C22B H22F 0.9600 . ?
C22B Si4B 1.862(16) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 P1 1.785(7) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 P1 1.765(7) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 P1 1.783(7) . ?
Cl1 U1 2.6899(12) . ?
O1 P1 1.514(4) . ?
O1 U1 2.354(3) . ?
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 0.000 0.000 0.500 330.5 66.9 ?
2 0.500 0.500 0.000 330.5 66.9 ?
