Temperature induced single-crystal to single-crystal transformation of uranium azide complexes.
Li, Kai; Rajeshkumar, Thayalan; Zhao, Yue; Wang, Tianwei; Maron, Laurent; Zhu, Congqing; Chemical communications (Cambridge, England) 60 (2024) 2966–2969; doi:10.1039/d4cc00546e

data_7132723
_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         'C40 H96 N20 P4 U2'
_chemical_formula_sum            'C40 H96 N20 P4 U2'
_chemical_formula_weight         1457.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-12
_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                 110.786(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.279(2)
_cell_length_b                   10.4213(10)
_cell_length_c                   25.477(3)
_cell_measurement_reflns_used    6811
_cell_measurement_temperature    333.00
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.54
_cell_volume                     6274.8(11)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      333.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28222
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         2.184
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.301
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1467
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1159 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.5608.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.852
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7206
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+11.7175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4498
_reflns_number_total             7206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00546e2.cif
_cod_data_source_block           lk2023122608_0m
_cod_depositor_comments
'Adding full bibliography for 7132717--7132729.cif.'
_cod_original_cell_volume        6274.9(11)
_cod_database_code               7132723
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.546
_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. Restrained distances
 C17-C16
 2.3 with sigma of 0.02
 C7A-C5A \\sim C7-C5 \\sim C6A-C5A \\sim C6-C5
 with sigma of 0.02
 P1-C5A \\sim P1-C5
 with sigma of 0.02
 C17-C15 \\sim C17A-C15A \\sim C16-C15 \\sim C16A-C15A
 with sigma of 0.02
 P2-C15 \\sim P2-C15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C15 \\sim C16 \\sim C17 \\sim C6A \\sim C7A \\sim
C15A \\sim C16A \\sim C17A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=
 Sof(H7AB)=Sof(H7AC)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(H7C)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C18(H18), C5(H5), C15(H15), C5A(H5A), C15A(H15A)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C13(H13A,H13B), C14(H14A,H14B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C16A(H16D,H16E,H16F),
 C17A(H17D,H17E,H17F)
;
_shelx_res_checksum              22626
_shelx_hkl_checksum              3134
_olex2_submission_special_instructions 'No special instructions were received'