#------------------------------------------------------------------------------
#$Date: 2024-04-05 01:37:39 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/27/7132727.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_7132727
loop_
_publ_author_name
'Li, Kai'
'Rajeshkumar, Thayalan'
'Zhao, Yue'
'Wang, Tianwei'
'Maron, Laurent'
'Zhu, Congqing'
_publ_section_title
;
 Temperature induced single-crystal to single-crystal transformation of
 uranium azide complexes.
;
_journal_issue                   21
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2966
_journal_page_last               2969
_journal_paper_doi               10.1039/d4cc00546e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C20 H48 N10 P2 U'
_chemical_formula_sum            'C20 H48 N10 P2 U'
_chemical_formula_weight         728.65
_chemical_name_systematic        5
_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             2024-01-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-31 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.838(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8845(5)
_cell_length_b                   10.6539(6)
_cell_length_c                   14.7678(9)
_cell_measurement_reflns_used    6037
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.86
_cell_volume                     1503.32(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.476
_diffrn_reflns_theta_min         2.853
_exptl_absorpt_coefficient_mu    5.531
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1022 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.7606.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0237
_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)+(0.0192P)²+1.2936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2149
_reflns_number_total             2771
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc00546e2.cif
_cod_data_source_block           lk-1_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7132717--7132729.cif.'
_cod_original_cell_volume        1503.31(15)
_cod_database_code               7132727
_shelx_shelxl_version_number     2014/7
_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   0.471
_shelx_estimated_absorpt_t_min   0.436
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C),
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
U1 U 0.5000 0.5000 0.5000 0.02464(8) Uani 1 2 d S . P . .
P1 P 0.65046(12) 0.27485(10) 0.45310(9) 0.0318(3) Uani 1 1 d . . . . .
N1 N 0.2502(4) 0.3891(3) 0.4842(3) 0.0352(9) Uani 1 1 d . . . . .
N2 N 0.4848(4) 0.2988(3) 0.4475(3) 0.0341(9) Uani 1 1 d . . . . .
N4 N 0.4784(4) 0.6124(3) 0.2771(3) 0.0392(9) Uani 1 1 d . . . . .
N3 N 0.4554(4) 0.5676(3) 0.3453(3) 0.0405(9) Uani 1 1 d . . . . .
C2 C 0.1778(5) 0.4216(4) 0.5572(4) 0.0457(13) Uani 1 1 d . . . . .
H2A H 0.2379 0.4001 0.6190 0.069 Uiso 1 1 calc R U . . .
H2B H 0.0900 0.3745 0.5463 0.069 Uiso 1 1 calc R U . . .
H2C H 0.1577 0.5118 0.5547 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7110(5) 0.1360(4) 0.5269(3) 0.0355(10) Uani 1 1 d . . . . .
H5 H 0.6536 0.0624 0.4974 0.043 Uiso 1 1 calc R U . . .
C4 C 0.3669(5) 0.2135(4) 0.4271(4) 0.0427(12) Uani 1 1 d . . . . .
H4A H 0.3996 0.1262 0.4413 0.051 Uiso 1 1 calc R U . . .
H4B H 0.3167 0.2187 0.3600 0.051 Uiso 1 1 calc R U . . .
C6 C 0.6919(6) 0.1522(4) 0.6251(4) 0.0495(13) Uani 1 1 d . . . . .
H6A H 0.7434 0.2266 0.6542 0.074 Uiso 1 1 calc R U . . .
H6B H 0.7277 0.0779 0.6627 0.074 Uiso 1 1 calc R U . . .
H6C H 0.5922 0.1627 0.6217 0.074 Uiso 1 1 calc R U . . .
C3 C 0.2708(5) 0.2509(4) 0.4871(4) 0.0418(12) Uani 1 1 d . . . . .
H3A H 0.1793 0.2085 0.4641 0.050 Uiso 1 1 calc R U . . .
H3B H 0.3117 0.2239 0.5526 0.050 Uiso 1 1 calc R U . . .
C1 C 0.1621(5) 0.4293(5) 0.3925(4) 0.0488(13) Uani 1 1 d . . . . .
H1A H 0.1417 0.5191 0.3946 0.073 Uiso 1 1 calc R U . . .
H1B H 0.0743 0.3818 0.3779 0.073 Uiso 1 1 calc R U . . .
H1C H 0.2118 0.4138 0.3441 0.073 Uiso 1 1 calc R U . . .
C8 C 0.6709(5) 0.2211(4) 0.3376(3) 0.0407(11) Uani 1 1 d . . . . .
H8 H 0.7731 0.2073 0.3445 0.049 Uiso 1 1 calc R U . . .
C10 C 0.6239(6) 0.3248(5) 0.2649(4) 0.0572(15) Uani 1 1 d . . . . .
H10A H 0.5252 0.3444 0.2590 0.086 Uiso 1 1 calc R U . . .
H10B H 0.6357 0.2964 0.2043 0.086 Uiso 1 1 calc R U . . .
H10C H 0.6808 0.4000 0.2849 0.086 Uiso 1 1 calc R U . . .
N5 N 0.4998(6) 0.6551(5) 0.2111(4) 0.0776(17) Uani 1 1 d . . . . .
C7 C 0.8654(5) 0.1078(5) 0.5308(4) 0.0601(15) Uani 1 1 d . . . . .
H7A H 0.8738 0.0863 0.4679 0.090 Uiso 1 1 calc R U . . .
H7B H 0.8980 0.0371 0.5733 0.090 Uiso 1 1 calc R U . . .
H7C H 0.9225 0.1820 0.5536 0.090 Uiso 1 1 calc R U . . .
C9 C 0.5964(7) 0.0978(5) 0.3029(4) 0.0629(16) Uani 1 1 d . . . . .
H9A H 0.6311 0.0315 0.3491 0.094 Uiso 1 1 calc R U . . .
H9B H 0.6148 0.0746 0.2430 0.094 Uiso 1 1 calc R U . . .
H9C H 0.4954 0.1081 0.2946 0.094 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 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
P1 U1 P1 180.0 3_666 . ?
N1 U1 P1 97.31(8) . . ?
N1 U1 P1 97.30(8) 3_666 3_666 ?
N1 U1 P1 82.70(8) . 3_666 ?
N1 U1 P1 82.69(8) 3_666 . ?
N1 U1 N1 180.0 3_666 . ?
N2 U1 P1 32.73(9) . . ?
N2 U1 P1 147.27(9) 3_666 . ?
N2 U1 P1 147.27(9) . 3_666 ?
N2 U1 P1 32.73(9) 3_666 3_666 ?
N2 U1 N1 64.99(11) . . ?
N2 U1 N1 115.01(11) . 3_666 ?
N2 U1 N1 64.99(11) 3_666 3_666 ?
N2 U1 N1 115.01(11) 3_666 . ?
N2 U1 N2 180.0 . 3_666 ?
N2 U1 N3 88.73(13) . . ?
N2 U1 N3 88.73(13) 3_666 3_666 ?
N2 U1 N3 91.27(13) . 3_666 ?
N2 U1 N3 91.27(13) 3_666 . ?
N3 U1 P1 89.93(9) 3_666 . ?
N3 U1 P1 90.07(9) 3_666 3_666 ?
N3 U1 P1 90.07(9) . . ?
N3 U1 P1 89.93(9) . 3_666 ?
N3 U1 N1 83.56(13) 3_666 . ?
N3 U1 N1 83.56(13) . 3_666 ?
N3 U1 N1 96.44(13) 3_666 3_666 ?
N3 U1 N1 96.44(13) . . ?
N3 U1 N3 180.0 3_666 . ?
N2 P1 U1 48.53(12) . . ?
N2 P1 C5 108.87(19) . . ?
N2 P1 C8 110.1(2) . . ?
C5 P1 U1 127.66(15) . . ?
C5 P1 C8 101.6(2) . . ?
C8 P1 U1 129.48(15) . . ?
C2 N1 U1 116.0(3) . . ?
C2 N1 C3 107.4(3) . . ?
C3 N1 U1 108.4(2) . . ?
C1 N1 U1 105.3(3) . . ?
C1 N1 C2 108.6(4) . . ?
C1 N1 C3 111.1(4) . . ?
P1 N2 U1 98.75(16) . . ?
C4 N2 U1 130.0(3) . . ?
C4 N2 P1 130.8(3) . . ?
N5 N4 N3 179.5(6) . . ?
N4 N3 U1 158.0(4) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C5 H5 108.0 . . ?
C6 C5 P1 111.8(3) . . ?
C6 C5 H5 108.0 . . ?
C6 C5 C7 110.5(4) . . ?
C7 C5 P1 110.3(3) . . ?
C7 C5 H5 108.0 . . ?
N2 C4 H4A 110.1 . . ?
N2 C4 H4B 110.1 . . ?
N2 C4 C3 107.8(4) . . ?
H4A C4 H4B 108.5 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C3 C4 110.3(4) . . ?
N1 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C8 H8 107.2 . . ?
C10 C8 P1 109.7(3) . . ?
C10 C8 H8 107.2 . . ?
C10 C8 C9 110.7(4) . . ?
C9 C8 P1 114.6(3) . . ?
C9 C8 H8 107.2 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 P1 2.9955(11) . ?
U1 P1 2.9955(11) 3_666 ?
U1 N1 2.694(3) . ?
U1 N1 2.694(3) 3_666 ?
U1 N2 2.271(3) . ?
U1 N2 2.271(3) 3_666 ?
U1 N3 2.328(4) . ?
U1 N3 2.327(4) 3_666 ?
P1 N2 1.639(4) . ?
P1 C5 1.844(4) . ?
P1 C8 1.859(4) . ?
N1 C2 1.479(5) . ?
N1 C3 1.485(5) . ?
N1 C1 1.474(6) . ?
N2 C4 1.447(5) . ?
N4 N3 1.188(5) . ?
N4 N5 1.143(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C5 H5 1.0000 . ?
C5 C6 1.520(6) . ?
C5 C7 1.542(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.509(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C8 H8 1.0000 . ?
C8 C10 1.526(6) . ?
C8 C9 1.529(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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 P1 N2 C4 -173.0(5) . . . . ?
U1 P1 C5 C6 -7.0(4) . . . . ?
U1 P1 C5 C7 -130.4(3) . . . . ?
U1 P1 C8 C10 12.0(5) . . . . ?
U1 P1 C8 C9 -113.2(4) . . . . ?
U1 N1 C3 C4 -43.6(4) . . . . ?
U1 N2 C4 C3 -27.0(6) . . . . ?
P1 N2 C4 C3 144.0(4) . . . . ?
N2 P1 C5 C6 -58.6(4) . . . . ?
N2 P1 C5 C7 178.0(3) . . . . ?
N2 P1 C8 C10 64.3(4) . . . . ?
N2 P1 C8 C9 -60.9(4) . . . . ?
N2 C4 C3 N1 45.6(5) . . . . ?
C2 N1 C3 C4 -169.7(4) . . . . ?
C5 P1 N2 U1 124.03(18) . . . . ?
C5 P1 N2 C4 -49.0(5) . . . . ?
C5 P1 C8 C10 179.5(4) . . . . ?
C5 P1 C8 C9 54.3(4) . . . . ?
C1 N1 C3 C4 71.6(5) . . . . ?
C8 P1 N2 U1 -125.45(18) . . . . ?
C8 P1 N2 C4 61.5(5) . . . . ?
C8 P1 C5 C6 -174.8(3) . . . . ?
C8 P1 C5 C7 61.8(4) . . . . ?
