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_7132725
_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         '2(C40 H96 N20 P4 U2)'
_chemical_formula_sum            'C80 H192 N40 P8 U4'
_chemical_formula_weight         2914.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                 111.1580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.9458(11)
_cell_length_b                   10.2858(5)
_cell_length_c                   25.3172(12)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.16
_cell_volume                     6058.2(5)
_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      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       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55348
_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         27.573
_diffrn_reflns_theta_min         1.965
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.490
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0501
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.5279.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         13966
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0491
_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/[\s^2^(Fo^2^)+(0.0330P)^2^+15.5472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9616
_reflns_number_total             13966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00546e2.cif
_cod_data_source_block           lk2023122503_0m
_cod_depositor_comments
'Adding full bibliography for 7132717--7132729.cif.'
_cod_database_code               7132725
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.438
_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
 C28-C29A \\sim C28-C29
 with sigma of 0.02
 C28-C30A \\sim C28-C30
 with sigma of 0.02
 P3-C28 \\sim P3-C28A
 with sigma of 0.02
 C28-C29A \\sim C28A-C29A
 with sigma of 0.02
 C28-C30A \\sim C28A-C30A
 with sigma of 0.02
 C28-C29 \\sim C28A-C29
 with sigma of 0.02
 C28-C30 \\sim C28A-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C29A \\sim C30A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C28 \\sim C28A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C35(H35), C38(H38), C28(H28), C28A(H28A), C5(H5), C8(H8), C15(H15),
 C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C33(H33A,H33B), C34(H34A,H34B), C3(H3A,H3B),
 C4(H4A,H4B), C13(H13A,H13B), C14(H14A,H14B)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C1(H1A,H1B,
 H1C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              5577
_shelx_hkl_checksum              78316
_olex2_submission_special_instructions 'No special instructions were received'