#------------------------------------------------------------------------------
#$Date: 2020-01-22 03:49:08 +0100 (Wed 22 de Jan de 2020) $
#$Revision: 247074 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/33/7703339.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_7703339
loop_
_publ_author_name
'Dickie, Tara K. K.'
'MacNeil, Connor S.'
'Hayes, Paul G.'
_publ_section_title
;
 Consecutive N₂ loss from a uranium diphosphazide complex.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              578
_journal_page_last               582
_journal_paper_doi               10.1039/c9dt04517a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H33 Cl3 N4 O2 P2 U, 2(C6 H6)'
_chemical_formula_sum            'C54 H45 Cl3 N4 O2 P2 U'
_chemical_formula_weight         1188.26
_chemical_name_systematic        P(N3)-P=N
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-19 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9425(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.79440(10)
_cell_length_b                   17.44271(12)
_cell_length_c                   20.42070(16)
_cell_measurement_reflns_used    43167
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      79.3350
_cell_measurement_theta_min      4.0660
_cell_volume                     4895.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00  31.00   0.50    0.50    --  -38.50   0.00 150.00  278
  2  ω    -42.00  28.00   0.50    0.50    --  -38.50  38.00   0.00  140
  3  ω     45.00 115.00   0.50    0.50    --   48.81  38.00  60.00  140
  4  ω    -14.00  61.00   0.50    0.50    --   48.81 -57.00 -90.00  150
  5  ω     57.00 151.00   0.50    0.50    --  111.00 178.00  90.00  188
  6  ω     47.00 117.00   0.50    0.50    --  111.00 -50.00  30.00  140
  7  ω     45.00 115.00   0.50    0.50    --  111.00 -38.00  90.00  140
  8  ω    101.00 178.00   0.50    0.50    --  111.00  12.00-120.00  154
  9  ω     57.00 151.00   0.50    0.50    --  111.00 178.00 120.00  188
 10  ω     41.00 116.00   0.50    0.50    --  111.00-111.00-120.00  150
 11  ω     41.00 115.00   0.50    0.50    --  111.00 -25.00  60.00  148
 12  ω    105.00 175.00   0.50    0.50    --  111.00  50.00-150.00  140
 13  ω     41.00 116.00   0.50    0.50    --  111.00-111.00 -90.00  150
 14  ω     46.00 134.00   0.50    0.50    --  111.00 -77.00  60.00  176
 15  ω     45.00 115.00   0.50    0.50    --  111.00 -38.00 -90.00  140
 16  ω     41.00 121.00   0.50    0.50    --  111.00 -12.00  30.00  160
 17  ω     47.00 125.00   0.50    0.50    --  111.00-133.00  46.00  156
 18  ω     59.00 150.00   0.50    0.50    --  111.00 178.00  60.00  182
 19  ω     47.00 112.00   0.50    0.50    --  111.00 -38.00   0.00  130
 20  ω    130.00 156.00   0.50    0.50    --  111.00  50.00   0.00   52
 21  ω     69.00 106.00   0.50    0.50    --  111.00 -50.00-150.00   74
 22  ω     44.00 106.00   0.50    0.50    --  111.00 -25.00   0.00  124
 23  ω     46.00 130.00   0.50    0.50    --  111.00 -77.00-150.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1071794000
_diffrn_orient_matrix_UB_12      0.0142390000
_diffrn_orient_matrix_UB_13      0.0124789000
_diffrn_orient_matrix_UB_21      0.0278973000
_diffrn_orient_matrix_UB_22      -0.0017529000
_diffrn_orient_matrix_UB_23      0.0746919000
_diffrn_orient_matrix_UB_31      0.0178801000
_diffrn_orient_matrix_UB_32      0.0870751000
_diffrn_orient_matrix_UB_33      -0.0005460000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.691
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_preparation       'Staudinger with prolonged heating'
_exptl_crystal_recrystallization_method benzene
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         10592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0453P)²+10.7943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10248
_reflns_number_total             10592
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph17013
_cod_database_code               7703339
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H37 N4 O2 P2 Cl2 U1'
_chemical_oxdiff_usercomment     'mixed ligand; orange cube habit'
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C61(H61),
 C62(H62), C63(H63), C71(H71), C72(H72), C73(H73)
;
_olex2_exptl_crystal_mounting_method 'MitiGen loop'
_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 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.787
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.6715(2) 0.46282(18) 0.48133(16) 0.0146(6) Uani 1 1 d .
C2 C 0.6082(3) 0.4254(2) 0.52073(18) 0.0194(7) Uani 1 1 d .
H2 H 0.5854 0.3767 0.5090 0.023 Uiso 1 1 calc R
C3 C 0.5793(3) 0.4598(2) 0.57673(17) 0.0205(7) Uani 1 1 d .
H3 H 0.5368 0.4347 0.6025 0.025 Uiso 1 1 calc R
C4 C 0.6143(3) 0.5325(2) 0.59432(17) 0.0197(7) Uani 1 1 d .
H4 H 0.5956 0.5558 0.6322 0.024 Uiso 1 1 calc R
C5 C 0.6769(3) 0.57024(19) 0.55554(19) 0.0211(7) Uani 1 1 d .
H5 H 0.7006 0.6185 0.5679 0.025 Uiso 1 1 calc R
C6 C 0.7046(3) 0.53627(18) 0.49814(16) 0.0161(6) Uani 1 1 d .
C7 C 0.7535(3) 0.18687(19) 0.42203(16) 0.0167(6) Uani 1 1 d .
C8 C 0.6998(3) 0.1472(2) 0.46604(18) 0.0211(7) Uani 1 1 d .
H8 H 0.6328 0.1418 0.4577 0.025 Uiso 1 1 calc R
C9 C 0.7480(3) 0.1158(2) 0.52269(18) 0.0256(8) Uani 1 1 d .
H9 H 0.7129 0.0894 0.5524 0.031 Uiso 1 1 calc R
C10 C 0.8476(3) 0.1236(2) 0.5348(2) 0.0297(9) Uani 1 1 d .
H10 H 0.8793 0.1023 0.5726 0.036 Uiso 1 1 calc R
C11 C 0.9013(3) 0.1634(3) 0.4905(2) 0.0328(9) Uani 1 1 d .
H11 H 0.9683 0.1686 0.4987 0.039 Uiso 1 1 calc R
C12 C 0.8535(3) 0.1952(2) 0.43446(19) 0.0253(8) Uani 1 1 d .
H12 H 0.8886 0.2222 0.4051 0.030 Uiso 1 1 calc R
C13 C 0.7426(2) 0.2073(2) 0.27851(16) 0.0163(7) Uani 1 1 d .
C14 C 0.7404(2) 0.2557(2) 0.22361(16) 0.0154(6) Uani 1 1 d .
C15 C 0.7606(3) 0.2255(2) 0.16293(17) 0.0180(7) Uani 1 1 d .
H15 H 0.7605 0.2573 0.1264 0.022 Uiso 1 1 calc R
C16 C 0.7809(3) 0.1479(2) 0.15709(18) 0.0220(7) Uani 1 1 d .
H16 H 0.7924 0.1281 0.1162 0.026 Uiso 1 1 calc R
C17 C 0.7843(3) 0.0993(2) 0.21106(19) 0.0223(7) Uani 1 1 d .
H17 H 0.7987 0.0476 0.2065 0.027 Uiso 1 1 calc R
C18 C 0.7660(3) 0.12879(19) 0.27198(18) 0.0197(7) Uani 1 1 d .
H18 H 0.7692 0.0969 0.3086 0.024 Uiso 1 1 calc R
C19 C 0.5673(3) 0.21812(19) 0.34601(16) 0.0163(6) Uani 1 1 d .
C20 C 0.5332(3) 0.1483(2) 0.3193(2) 0.0250(8) Uani 1 1 d .
H20 H 0.5773 0.1122 0.3063 0.030 Uiso 1 1 calc R
C21 C 0.4343(3) 0.1325(2) 0.3119(2) 0.0282(8) Uani 1 1 d .
H21 H 0.4123 0.0858 0.2945 0.034 Uiso 1 1 calc R
C22 C 0.3685(3) 0.1866(2) 0.3307(2) 0.0247(8) Uani 1 1 d .
H22 H 0.3022 0.1762 0.3258 0.030 Uiso 1 1 calc R
C23 C 0.4013(3) 0.2557(2) 0.35655(19) 0.0259(8) Uani 1 1 d .
H23 H 0.3568 0.2919 0.3688 0.031 Uiso 1 1 calc R
C24 C 0.5007(3) 0.2721(2) 0.36462(18) 0.0203(7) Uani 1 1 d .
H24 H 0.5222 0.3188 0.3823 0.024 Uiso 1 1 calc R
C25 C 0.8574(2) 0.60599(19) 0.32547(16) 0.0152(6) Uani 1 1 d .
C26 C 0.8506(3) 0.66636(19) 0.37063(16) 0.0161(6) Uani 1 1 d .
C27 C 0.9097(3) 0.7316(2) 0.36688(18) 0.0197(7) Uani 1 1 d .
H27 H 0.9046 0.7715 0.3966 0.024 Uiso 1 1 calc R
C28 C 0.9752(3) 0.7372(2) 0.31973(18) 0.0208(7) Uani 1 1 d .
H28 H 1.0131 0.7809 0.3169 0.025 Uiso 1 1 calc R
C29 C 0.9839(2) 0.6764(2) 0.27639(17) 0.0181(7) Uani 1 1 d .
H29 H 1.0290 0.6792 0.2452 0.022 Uiso 1 1 calc R
C30 C 0.9261(3) 0.6116(2) 0.27929(16) 0.0170(6) Uani 1 1 d .
H30 H 0.9331 0.5714 0.2501 0.020 Uiso 1 1 calc R
C31 C 0.8100(2) 0.72447(19) 0.50076(16) 0.0152(6) Uani 1 1 d .
C32 C 0.8685(3) 0.6952(2) 0.55461(18) 0.0197(7) Uani 1 1 d .
H32 H 0.8862 0.6437 0.5560 0.024 Uiso 1 1 calc R
C33 C 0.8994(3) 0.7438(2) 0.60561(18) 0.0222(7) Uani 1 1 d .
H33 H 0.9359 0.7244 0.6423 0.027 Uiso 1 1 calc R
C34 C 0.8766(3) 0.8213(2) 0.60271(18) 0.0227(7) Uani 1 1 d .
H34 H 0.8989 0.8535 0.6370 0.027 Uiso 1 1 calc R
C35 C 0.8207(3) 0.8508(2) 0.54890(18) 0.0204(7) Uani 1 1 d .
H35 H 0.8060 0.9028 0.5469 0.024 Uiso 1 1 calc R
C36 C 0.7865(2) 0.80238(19) 0.49781(16) 0.0163(6) Uani 1 1 d .
H36 H 0.7482 0.8218 0.4619 0.020 Uiso 1 1 calc R
C37 C 0.6524(3) 0.7015(2) 0.40367(18) 0.0195(7) Uani 1 1 d .
C38 C 0.5798(3) 0.7129(2) 0.4470(2) 0.0244(8) Uani 1 1 d .
H38 H 0.5892 0.6952 0.4900 0.029 Uiso 1 1 calc R
C39 C 0.4951(3) 0.7501(2) 0.4259(2) 0.0280(8) Uani 1 1 d .
H39 H 0.4466 0.7565 0.4544 0.034 Uiso 1 1 calc R
C40 C 0.4814(3) 0.7784(3) 0.3621(2) 0.0319(9) Uani 1 1 d .
H40 H 0.4248 0.8049 0.3484 0.038 Uiso 1 1 calc R
C41 C 0.5520(3) 0.7668(3) 0.3191(2) 0.0403(11) Uani 1 1 d .
H41 H 0.5425 0.7851 0.2762 0.048 Uiso 1 1 calc R
C42 C 0.6373(3) 0.7279(3) 0.3396(2) 0.0323(9) Uani 1 1 d .
H42 H 0.6843 0.7197 0.3103 0.039 Uiso 1 1 calc R
Cl1 Cl 0.55518(6) 0.45875(5) 0.27867(4) 0.02283(17) Uani 1 1 d .
Cl2 Cl 0.76830(6) 0.50284(4) 0.16879(4) 0.01897(15) Uani 1 1 d .
Cl3 Cl 0.92606(6) 0.38209(5) 0.29434(4) 0.02481(17) Uani 1 1 d .
N1 N 0.7179(2) 0.33055(16) 0.36170(14) 0.0159(5) Uani 1 1 d .
N2 N 0.6929(2) 0.35748(16) 0.42040(14) 0.0154(5) Uani 1 1 d .
N3 N 0.7036(2) 0.42989(15) 0.42284(14) 0.0141(6) Uani 1 1 d .
N4 N 0.7695(3) 0.57354(17) 0.45806(17) 0.0203(6) Uani 1 1 d .
O1 O 0.71741(18) 0.32961(12) 0.22821(11) 0.0152(4) Uani 1 1 d .
O2 O 0.79986(18) 0.54362(13) 0.32688(11) 0.0154(4) Uani 1 1 d .
P1 P 0.69574(6) 0.23804(4) 0.35291(4) 0.01359(15) Uani 1 1 d .
P2 P 0.76846(6) 0.66309(5) 0.43344(4) 0.01478(16) Uani 1 1 d .
U1 U 0.74532(2) 0.43440(2) 0.28252(2) 0.01167(5) Uani 1 1 d .
C51 C 0.9112(4) 0.9424(3) 0.3314(3) 0.0411(11) Uani 1 1 d .
H51 H 0.9779 0.9451 0.3280 0.049 Uiso 1 1 calc R
C52 C 0.8709(4) 0.9692(3) 0.3878(3) 0.0443(12) Uani 1 1 d .
H52 H 0.9111 0.9892 0.4225 0.053 Uiso 1 1 calc R
C53 C 0.7718(4) 0.9659(2) 0.3921(3) 0.0431(12) Uani 1 1 d .
H53 H 0.7457 0.9840 0.4296 0.052 Uiso 1 1 calc R
C54 C 0.7112(4) 0.9364(3) 0.3414(3) 0.0414(12) Uani 1 1 d .
H54 H 0.6444 0.9345 0.3443 0.050 Uiso 1 1 calc R
C55 C 0.7511(4) 0.9093(3) 0.2857(2) 0.0428(12) Uani 1 1 d .
H55 H 0.7107 0.8891 0.2511 0.051 Uiso 1 1 calc R
C56 C 0.8503(4) 0.9121(3) 0.2811(3) 0.0408(11) Uani 1 1 d .
H56 H 0.8762 0.8933 0.2438 0.049 Uiso 1 1 calc R
C61 C 0.4530(3) 0.0607(2) 0.5271(2) 0.0260(8) Uani 1 1 d .
H61 H 0.4216 0.1016 0.5453 0.031 Uiso 1 1 calc R
C62 C 0.4310(3) 0.0417(3) 0.4620(2) 0.0314(9) Uani 1 1 d .
H62 H 0.3845 0.0696 0.4364 0.038 Uiso 1 1 calc R
C63 C 0.4784(3) -0.0191(3) 0.4349(2) 0.0332(9) Uani 1 1 d .
H63 H 0.4639 -0.0318 0.3909 0.040 Uiso 1 1 calc R
C71 C 0.9539(3) 0.4414(3) 0.5303(3) 0.0356(10) Uani 1 1 d .
H71 H 0.9229 0.4018 0.5507 0.043 Uiso 1 1 calc R
C72 C 0.9960(3) 0.5009(3) 0.5677(2) 0.0313(9) Uani 1 1 d .
H72 H 0.9928 0.5012 0.6130 0.038 Uiso 1 1 calc R
C73 C 1.0425(3) 0.5594(3) 0.5378(2) 0.0321(9) Uani 1 1 d .
H73 H 1.0712 0.5992 0.5628 0.038 Uiso 1 1 calc R
H4A H 0.783(4) 0.546(3) 0.432(3) 0.032(14) Uiso 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'
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'
P P 0.2955 0.4335 '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
C2 C1 N3 123.2(3) . .
C6 C1 C2 119.7(3) . .
C6 C1 N3 117.2(3) . .
C1 C2 H2 119.6 . .
C3 C2 C1 120.9(3) . .
C3 C2 H2 119.6 . .
C2 C3 H3 120.3 . .
C2 C3 C4 119.4(3) . .
C4 C3 H3 120.3 . .
C3 C4 H4 119.9 . .
C5 C4 C3 120.3(3) . .
C5 C4 H4 119.9 . .
C4 C5 H5 119.8 . .
C4 C5 C6 120.4(3) . .
C6 C5 H5 119.8 . .
C1 C6 C5 119.3(3) . .
C1 C6 N4 119.2(3) . .
C5 C6 N4 121.4(3) . .
C8 C7 P1 121.8(3) . .
C12 C7 C8 120.5(3) . .
C12 C7 P1 117.3(3) . .
C7 C8 H8 120.4 . .
C7 C8 C9 119.2(4) . .
C9 C8 H8 120.4 . .
C8 C9 H9 119.9 . .
C10 C9 C8 120.3(4) . .
C10 C9 H9 119.9 . .
C9 C10 H10 119.8 . .
C9 C10 C11 120.4(4) . .
C11 C10 H10 119.8 . .
C10 C11 H11 120.3 . .
C12 C11 C10 119.4(4) . .
C12 C11 H11 120.3 . .
C7 C12 H12 119.9 . .
C11 C12 C7 120.2(4) . .
C11 C12 H12 119.9 . .
C14 C13 C18 119.8(3) . .
C14 C13 P1 121.0(3) . .
C18 C13 P1 118.3(3) . .
C15 C14 C13 119.3(3) . .
O1 C14 C13 121.0(3) . .
O1 C14 C15 119.7(3) . .
C14 C15 H15 120.0 . .
C16 C15 C14 120.1(3) . .
C16 C15 H15 120.0 . .
C15 C16 H16 119.3 . .
C17 C16 C15 121.3(3) . .
C17 C16 H16 119.3 . .
C16 C17 H17 120.4 . .
C16 C17 C18 119.3(3) . .
C18 C17 H17 120.4 . .
C13 C18 H18 119.9 . .
C17 C18 C13 120.2(3) . .
C17 C18 H18 119.9 . .
C20 C19 P1 119.6(3) . .
C24 C19 C20 119.2(3) . .
C24 C19 P1 121.2(3) . .
C19 C20 H20 119.7 . .
C21 C20 C19 120.6(3) . .
C21 C20 H20 119.7 . .
C20 C21 H21 120.1 . .
C22 C21 C20 119.7(3) . .
C22 C21 H21 120.1 . .
C21 C22 H22 120.0 . .
C23 C22 C21 120.0(4) . .
C23 C22 H22 120.0 . .
C22 C23 H23 119.6 . .
C22 C23 C24 120.8(4) . .
C24 C23 H23 119.6 . .
C19 C24 C23 119.6(3) . .
C19 C24 H24 120.2 . .
C23 C24 H24 120.2 . .
C30 C25 C26 118.5(3) . .
O2 C25 C26 121.1(3) . .
O2 C25 C30 120.4(3) . .
C25 C26 P2 122.0(3) . .
C27 C26 C25 119.8(3) . .
C27 C26 P2 118.2(3) . .
C26 C27 H27 119.6 . .
C28 C27 C26 120.9(3) . .
C28 C27 H27 119.6 . .
C27 C28 H28 120.4 . .
C27 C28 C29 119.2(3) . .
C29 C28 H28 120.4 . .
C28 C29 H29 119.6 . .
C30 C29 C28 120.8(3) . .
C30 C29 H29 119.6 . .
C25 C30 H30 119.6 . .
C29 C30 C25 120.8(3) . .
C29 C30 H30 119.6 . .
C32 C31 P2 120.5(3) . .
C36 C31 C32 120.2(3) . .
C36 C31 P2 119.3(3) . .
C31 C32 H32 120.4 . .
C33 C32 C31 119.1(3) . .
C33 C32 H32 120.4 . .
C32 C33 H33 119.6 . .
C32 C33 C34 120.8(3) . .
C34 C33 H33 119.6 . .
C33 C34 H34 119.9 . .
C35 C34 C33 120.3(3) . .
C35 C34 H34 119.9 . .
C34 C35 H35 120.0 . .
C34 C35 C36 119.9(3) . .
C36 C35 H35 120.0 . .
C31 C36 H36 120.2 . .
C35 C36 C31 119.7(3) . .
C35 C36 H36 120.2 . .
C38 C37 P2 120.2(3) . .
C42 C37 C38 119.4(4) . .
C42 C37 P2 120.1(3) . .
C37 C38 H38 119.9 . .
C39 C38 C37 120.1(4) . .
C39 C38 H38 119.9 . .
C38 C39 H39 119.9 . .
C38 C39 C40 120.3(4) . .
C40 C39 H39 119.9 . .
C39 C40 H40 120.1 . .
C41 C40 C39 119.8(4) . .
C41 C40 H40 120.1 . .
C40 C41 H41 119.9 . .
C40 C41 C42 120.3(4) . .
C42 C41 H41 119.9 . .
C37 C42 C41 120.0(4) . .
C37 C42 H42 120.0 . .
C41 C42 H42 120.0 . .
N2 N1 P1 112.0(2) . .
N2 N1 U1 112.78(19) . .
P1 N1 U1 132.95(15) . .
N3 N2 N1 109.9(3) . .
C1 N3 U1 153.4(2) . .
N2 N3 C1 112.8(3) . .
N2 N3 U1 91.15(19) . .
C6 N4 P2 128.5(3) . .
C6 N4 H4A 109(4) . .
P2 N4 H4A 112(4) . .
C14 O1 U1 145.4(2) . .
C25 O2 U1 150.0(2) . .
C7 P1 C19 109.44(16) . .
C13 P1 C7 110.53(16) . .
C13 P1 C19 107.56(16) . .
N1 P1 C7 109.55(15) . .
N1 P1 C13 108.02(16) . .
N1 P1 C19 111.70(15) . .
C26 P2 C31 110.51(16) . .
C26 P2 C37 110.37(17) . .
C37 P2 C31 104.68(15) . .
N4 P2 C26 105.16(16) . .
N4 P2 C31 109.81(17) . .
N4 P2 C37 116.35(17) . .
Cl1 U1 Cl2 95.42(3) . .
Cl1 U1 N3 76.09(6) . .
Cl2 U1 N3 154.57(5) . .
Cl3 U1 Cl1 168.44(3) . .
Cl3 U1 Cl2 93.00(3) . .
Cl3 U1 N3 99.33(6) . .
N1 U1 Cl1 86.01(7) . .
N1 U1 Cl2 159.36(7) . .
N1 U1 Cl3 83.33(7) . .
N1 U1 N3 45.47(8) . .
O1 U1 Cl1 89.32(7) . .
O1 U1 Cl2 87.75(6) . .
O1 U1 Cl3 83.09(7) . .
O1 U1 N1 71.66(9) . .
O1 U1 N3 115.65(8) . .
O1 U1 O2 168.50(9) . .
O2 U1 Cl1 100.07(7) . .
O2 U1 Cl2 84.78(6) . .
O2 U1 Cl3 88.57(7) . .
O2 U1 N1 115.32(9) . .
O2 U1 N3 73.46(8) . .
C52 C51 H51 120.6 . .
C56 C51 H51 120.6 . .
C56 C51 C52 118.8(5) . .
C51 C52 H52 119.9 . .
C53 C52 C51 120.3(5) . .
C53 C52 H52 119.9 . .
C52 C53 H53 119.7 . .
C54 C53 C52 120.7(5) . .
C54 C53 H53 119.7 . .
C53 C54 H54 120.5 . .
C53 C54 C55 119.1(5) . .
C55 C54 H54 120.5 . .
C54 C55 H55 119.7 . .
C56 C55 C54 120.5(5) . .
C56 C55 H55 119.7 . .
C51 C56 C55 120.6(5) . .
C51 C56 H56 119.7 . .
C55 C56 H56 119.7 . .
C62 C61 H61 120.0 . .
C62 C61 C63 120.1(4) . 3_656
C63 C61 H61 120.0 3_656 .
C61 C62 H62 120.1 . .
C61 C62 C63 119.8(4) . .
C63 C62 H62 120.1 . .
C61 C63 C62 120.1(4) 3_656 .
C61 C63 H63 120.0 3_656 .
C62 C63 H63 120.0 . .
C72 C71 H71 119.8 . .
C72 C71 C73 120.5(4) . 3_766
C73 C71 H71 119.8 3_766 .
C71 C72 H72 120.0 . .
C73 C72 C71 120.0(4) . .
C73 C72 H72 120.0 . .
C71 C73 H73 120.2 3_766 .
C72 C73 C71 119.5(4) . 3_766
C72 C73 H73 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.398(5) .
C1 C6 1.393(5) .
C1 N3 1.430(4) .
C2 H2 0.9300 .
C2 C3 1.380(5) .
C3 H3 0.9300 .
C3 C4 1.392(5) .
C4 H4 0.9300 .
C4 C5 1.388(5) .
C5 H5 0.9300 .
C5 C6 1.396(5) .
C6 N4 1.422(4) .
C7 C8 1.396(5) .
C7 C12 1.389(5) .
C7 P1 1.797(4) .
C8 H8 0.9300 .
C8 C9 1.396(5) .
C9 H9 0.9300 .
C9 C10 1.382(6) .
C10 H10 0.9300 .
C10 C11 1.401(6) .
C11 H11 0.9300 .
C11 C12 1.386(6) .
C12 H12 0.9300 .
C13 C14 1.402(5) .
C13 C18 1.416(5) .
C13 P1 1.784(3) .
C14 C15 1.397(5) .
C14 O1 1.332(4) .
C15 H15 0.9300 .
C15 C16 1.389(5) .
C16 H16 0.9300 .
C16 C17 1.387(5) .
C17 H17 0.9300 .
C17 C18 1.389(5) .
C18 H18 0.9300 .
C19 C20 1.400(5) .
C19 C24 1.391(5) .
C19 P1 1.799(4) .
C20 H20 0.9300 .
C20 C21 1.387(5) .
C21 H21 0.9300 .
C21 C22 1.386(6) .
C22 H22 0.9300 .
C22 C23 1.377(5) .
C23 H23 0.9300 .
C23 C24 1.395(5) .
C24 H24 0.9300 .
C25 C26 1.408(5) .
C25 C30 1.396(5) .
C25 O2 1.349(4) .
C26 C27 1.406(5) .
C26 P2 1.784(3) .
C27 H27 0.9300 .
C27 C28 1.380(5) .
C28 H28 0.9300 .
C28 C29 1.393(5) .
C29 H29 0.9300 .
C29 C30 1.387(5) .
C30 H30 0.9300 .
C31 C32 1.403(5) .
C31 C36 1.397(5) .
C31 P2 1.797(3) .
C32 H32 0.9300 .
C32 C33 1.382(5) .
C33 H33 0.9300 .
C33 C34 1.387(5) .
C34 H34 0.9300 .
C34 C35 1.386(5) .
C35 H35 0.9300 .
C35 C36 1.392(5) .
C36 H36 0.9300 .
C37 C38 1.406(5) .
C37 C42 1.385(6) .
C37 P2 1.793(4) .
C38 H38 0.9300 .
C38 C39 1.374(6) .
C39 H39 0.9300 .
C39 C40 1.391(6) .
C40 H40 0.9300 .
C40 C41 1.382(6) .
C41 H41 0.9300 .
C41 C42 1.391(6) .
C42 H42 0.9300 .
Cl1 U1 2.6516(8) .
Cl2 U1 2.6545(8) .
Cl3 U1 2.6463(8) .
N1 N2 1.359(4) .
N1 P1 1.649(3) .
N1 U1 2.479(3) .
N2 N3 1.272(4) .
N3 U1 2.972(3) .
N4 P2 1.641(3) .
N4 H4A 0.75(6) .
O1 U1 2.155(2) .
O2 U1 2.213(2) .
C51 H51 0.9300 .
C51 C52 1.403(8) .
C51 C56 1.374(8) .
C52 H52 0.9300 .
C52 C53 1.377(8) .
C53 H53 0.9300 .
C53 C54 1.374(8) .
C54 H54 0.9300 .
C54 C55 1.389(7) .
C55 H55 0.9300 .
C55 C56 1.380(7) .
C56 H56 0.9300 .
C61 H61 0.9300 .
C61 C62 1.377(6) .
C61 C63 1.378(6) 3_656
C62 H62 0.9300 .
C62 C63 1.387(6) .
C63 C61 1.378(6) 3_656
C63 H63 0.9300 .
C71 H71 0.9300 .
C71 C72 1.385(7) .
C71 C73 1.396(7) 3_766
C72 H72 0.9300 .
C72 C73 1.376(7) .
C73 C71 1.396(7) 3_766
C73 H73 0.9300 .
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_4
C1 C2 C3 C4 -0.5(6) . .
C1 C6 N4 P2 137.3(3) . .
C2 C1 C6 C5 2.4(5) . .
C2 C1 C6 N4 179.5(3) . .
C2 C1 N3 N2 -19.0(5) . .
C2 C1 N3 U1 134.0(4) . .
C2 C3 C4 C5 0.6(6) . .
C3 C4 C5 C6 0.8(6) . .
C4 C5 C6 C1 -2.3(6) . .
C4 C5 C6 N4 -179.3(4) . .
C5 C6 N4 P2 -45.7(5) . .
C6 C1 C2 C3 -1.1(5) . .
C6 C1 N3 N2 162.1(3) . .
C6 C1 N3 U1 -44.9(6) . .
C6 N4 P2 C26 -167.1(3) . .
C6 N4 P2 C31 73.9(4) . .
C6 N4 P2 C37 -44.7(4) . .
C7 C8 C9 C10 -0.3(6) . .
C8 C7 C12 C11 0.7(6) . .
C8 C7 P1 C13 -125.8(3) . .
C8 C7 P1 C19 -7.5(3) . .
C8 C7 P1 N1 115.3(3) . .
C8 C9 C10 C11 0.3(6) . .
C9 C10 C11 C12 0.2(7) . .
C10 C11 C12 C7 -0.6(7) . .
C12 C7 C8 C9 -0.2(5) . .
C12 C7 P1 C13 61.2(3) . .
C12 C7 P1 C19 179.5(3) . .
C12 C7 P1 N1 -57.7(3) . .
C13 C14 C15 C16 1.2(5) . .
C13 C14 O1 U1 49.6(5) . .
C14 C13 C18 C17 -1.7(5) . .
C14 C13 P1 C7 -154.4(3) . .
C14 C13 P1 C19 86.1(3) . .
C14 C13 P1 N1 -34.6(3) . .
C14 C15 C16 C17 -1.9(6) . .
C15 C14 O1 U1 -131.8(3) . .
C15 C16 C17 C18 0.7(6) . .
C16 C17 C18 C13 1.1(6) . .
C18 C13 C14 C15 0.6(5) . .
C18 C13 C14 O1 179.2(3) . .
C18 C13 P1 C7 36.7(3) . .
C18 C13 P1 C19 -82.8(3) . .
C18 C13 P1 N1 156.5(3) . .
C19 C20 C21 C22 0.6(6) . .
C20 C19 C24 C23 0.2(5) . .
C20 C19 P1 C7 -77.4(3) . .
C20 C19 P1 C13 42.7(3) . .
C20 C19 P1 N1 161.1(3) . .
C20 C21 C22 C23 0.0(6) . .
C21 C22 C23 C24 -0.4(6) . .
C22 C23 C24 C19 0.3(6) . .
C24 C19 C20 C21 -0.7(6) . .
C24 C19 P1 C7 104.9(3) . .
C24 C19 P1 C13 -134.9(3) . .
C24 C19 P1 N1 -16.6(3) . .
C25 C26 C27 C28 -0.5(5) . .
C25 C26 P2 C31 156.0(3) . .
C25 C26 P2 C37 -88.7(3) . .
C25 C26 P2 N4 37.6(3) . .
C26 C25 C30 C29 -2.2(5) . .
C26 C25 O2 U1 172.4(3) . .
C26 C27 C28 C29 -1.4(6) . .
C27 C26 P2 C31 -23.9(3) . .
C27 C26 P2 C37 91.4(3) . .
C27 C26 P2 N4 -142.4(3) . .
C27 C28 C29 C30 1.5(6) . .
C28 C29 C30 C25 0.3(5) . .
C30 C25 C26 C27 2.3(5) . .
C30 C25 C26 P2 -177.6(3) . .
C30 C25 O2 U1 -8.2(6) . .
C31 C32 C33 C34 -2.6(5) . .
C32 C31 C36 C35 -0.6(5) . .
C32 C31 P2 C26 -92.8(3) . .
C32 C31 P2 C37 148.3(3) . .
C32 C31 P2 N4 22.7(3) . .
C32 C33 C34 C35 1.2(6) . .
C33 C34 C35 C36 0.6(6) . .
C34 C35 C36 C31 -0.9(5) . .
C36 C31 C32 C33 2.3(5) . .
C36 C31 P2 C26 84.8(3) . .
C36 C31 P2 C37 -34.0(3) . .
C36 C31 P2 N4 -159.6(3) . .
C37 C38 C39 C40 -1.5(6) . .
C38 C37 C42 C41 1.4(6) . .
C38 C37 P2 C26 -172.6(3) . .
C38 C37 P2 C31 -53.7(3) . .
C38 C37 P2 N4 67.7(3) . .
C38 C39 C40 C41 2.0(7) . .
C39 C40 C41 C42 -0.9(7) . .
C40 C41 C42 C37 -0.9(8) . .
C42 C37 C38 C39 -0.3(6) . .
C42 C37 P2 C26 0.3(4) . .
C42 C37 P2 C31 119.3(3) . .
C42 C37 P2 N4 -119.3(3) . .
N1 N2 N3 C1 175.5(3) . .
N1 N2 N3 U1 7.2(3) . .
N2 N1 P1 C7 -53.7(3) . .
N2 N1 P1 C13 -174.1(2) . .
N2 N1 P1 C19 67.8(3) . .
N3 C1 C2 C3 -179.9(3) . .
N3 C1 C6 C5 -178.7(3) . .
N3 C1 C6 N4 -1.6(5) . .
O1 C14 C15 C16 -177.4(3) . .
O2 C25 C26 C27 -178.3(3) . .
O2 C25 C26 P2 1.7(5) . .
O2 C25 C30 C29 178.4(3) . .
P1 C7 C8 C9 -172.9(3) . .
P1 C7 C12 C11 173.7(3) . .
P1 C13 C14 C15 -168.2(3) . .
P1 C13 C14 O1 10.4(5) . .
P1 C13 C18 C17 167.4(3) . .
P1 C19 C20 C21 -178.4(3) . .
P1 C19 C24 C23 177.9(3) . .
P1 N1 N2 N3 -174.6(2) . .
P2 C26 C27 C28 179.4(3) . .
P2 C31 C32 C33 180.0(3) . .
P2 C31 C36 C35 -178.2(3) . .
P2 C37 C38 C39 172.7(3) . .
P2 C37 C42 C41 -171.6(4) . .
U1 N1 N2 N3 -9.4(3) . .
U1 N1 P1 C7 145.0(2) . .
U1 N1 P1 C13 24.5(3) . .
U1 N1 P1 C19 -93.6(2) . .
C51 C52 C53 C54 0.1(7) . .
C52 C51 C56 C55 1.1(7) . .
C52 C53 C54 C55 0.3(7) . .
C53 C54 C55 C56 -0.1(7) . .
C54 C55 C56 C51 -0.7(8) . .
C56 C51 C52 C53 -0.9(7) . .
C61 C62 C63 C61 0.4(7) . 3_656
C63 C61 C62 C63 -0.4(7) 3_656 .
C71 C72 C73 C71 0.5(7) . 3_766
C73 C71 C72 C73 -0.5(7) 3_766 .
