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_7132718
_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 N10 P4 U2'
_chemical_formula_sum            'C40 H98 N10 P4 U2'
_chemical_formula_weight         1319.22
_chemical_name_systematic        4
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-24 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.853(6)
_cell_angle_beta                 79.684(6)
_cell_angle_gamma                69.571(5)
_cell_formula_units_Z            2
_cell_length_a                   10.769(3)
_cell_length_b                   13.579(3)
_cell_length_c                   20.817(5)
_cell_measurement_reflns_used    5500
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.47
_cell_volume                     2800.2(12)
_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      296.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15512
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.831
_exptl_absorpt_coefficient_mu    5.925
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0878 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.7492.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.390
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6581
_reflns_number_total             9727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00546e2.cif
_cod_data_source_block           lk-1_a
_cod_depositor_comments
'Adding full bibliography for 7132717--7132729.cif.'
_cod_original_cell_volume        2800.3(12)
_cod_database_code               7132718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.451
_shelx_estimated_absorpt_t_min   0.415
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C18(H18), C8(H8), C25(H25), C5(H5), C15(H15), C35(H35), C28(H28), C38(H38)
1.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C33(H33A,H33B), C4(H4A,H4B), C13(H13A,H13B), C24(H24A,H24B),
 C23(H23A,H23B), C14(H14A,H14B), C34(H34A,H34B)
1.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C29(H29A,H29B,H29C), C22(H22A,H22B,
 H22C), C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C30(H30A,
 H30B,H30C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C19(H19A,H19B,H19C),
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C),
  C10(H10A,H10B,H10C), C36(H36A,H36B,H36C), C17(H17A,H17B,H17C), C7(H7A,H7B,
 H7C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C40(H40A,H40B,H40C), C26(H26A,H26B,
 H26C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              25630
_shelx_hkl_checksum              85332
_olex2_submission_special_instructions 'No special instructions were received'