Intra- and intermolecular interception of a photochemically generated terminal uranium nitride
Yadav, Munendra; Metta-Magaña, Alejandro; Fortier, Skye; Chemical Science 11 (2020) 2381–2387; doi:10.1039/C9SC05992J

data_1557111
_publ_section_title
;
 Intra- and intermolecular interception of a photochemically generated
 terminal uranium nitride
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              2381
_journal_page_last               2387
_journal_paper_doi               10.1039/C9SC05992J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C69 H82 N8 U, 2(C3 H3)'
_chemical_formula_sum            'C75 H88 N8 U'
_chemical_formula_weight         1339.56
_chemical_name_systematic        UImNHCazide
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-10 deposited with the CCDC.	2020-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                78.109(2)
_cell_angle_beta                 76.264(2)
_cell_angle_gamma                68.201(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1219(4)
_cell_length_b                   13.5561(5)
_cell_length_c                   20.3099(7)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.41
_cell_volume                     3230.5(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0981
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.716
_diffrn_reflns_theta_max         24.716
_diffrn_reflns_theta_min         1.915
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.561
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1192 before and 0.0749 after correction. The Ratio of minimum to maximum transmission is 0.8722. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         2.678
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         10999
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+13.6666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9762
_reflns_number_total             10999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05992j2.cif
_cod_data_source_block           uimnhcazide
_cod_depositor_comments
;Adding full bibliography for 1557110--1557114.cif.

 Adding full bibliography for 1557110--1557114.cif.
;
_cod_database_code               1557111
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 U1-N6 \\sim U1-N6A
 with sigma of 0.02
 N6-N7 \\sim N6A-N7A
 with sigma of 0.02
 N7-N8 \\sim N7A-N8A
 with sigma of 0.02
 U1-N7 \\sim U1-N7A
 with sigma of 0.04
 N6-N8 \\sim N6A-N8A
 with sigma of 0.04
 C39-C40 \\sim C39-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C40-C42 \\sim C40A-C42A
 with sigma of 0.02
 C39-C41 \\sim C39-C41A
 with sigma of 0.04
 C39-C42 \\sim C39-C42A
 with sigma of 0.04
 C41-C42 \\sim C41A-C42A
 with sigma of 0.04
3. Others
 Sof(N6A)=Sof(N7A)=Sof(N8A)=1-FVAR(1)
 Sof(N6)=Sof(N7)=Sof(N8)=FVAR(1)
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42A)=
 Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C33(H33), C40(H40), C40A(H40A), C48(H48), C55(H55),
 C60(H60), C67(H67)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C36(H36),
  C37(H37), C38(H38), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53),
 C63(H63), C64(H64), C65(H65), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C41A(H41D,H41E,
 H41F), C42(H42A,H42B,H42C), C42A(H42D,H42E,H42F), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              62055
_olex2_submission_special_instructions 'No special instructions were received'