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_1557110
_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 N5 U, C4 H10 O2'
_chemical_formula_sum            'C73 H92 N5 O2 U'
_chemical_formula_weight         1309.54
_chemical_name_systematic        UImNHC
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-09
_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                103.573(2)
_cell_angle_beta                 95.666(3)
_cell_angle_gamma                116.252(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2857(9)
_cell_length_b                   13.9411(8)
_cell_length_c                   20.5686(15)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.24
_cell_volume                     3230.4(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.941
_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  0.0894
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66213
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.531
_diffrn_reflns_theta_min         2.094
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.561
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1295 before and 0.0695 after correction. The Ratio of minimum to maximum transmission is 0.8141. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1346
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.796
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         18595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0427P)^2^+3.3021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14867
_reflns_number_total             18595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05992j2.cif
_cod_data_source_block           uimnhc
_cod_depositor_comments
;Adding full bibliography for 1557110--1557114.cif.

 Adding full bibliography for 1557110--1557114.cif.
;
_cod_database_code               1557110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.413
_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:
 C2(H2), C10(H10), C33(H33), C40(H40), C48(H48), C55(H55), C60(H60), C67(H67)
2.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C17(H17), 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)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), 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), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              31677
_olex2_submission_original_sample_id UImNHC
_olex2_submission_special_instructions 'No special instructions were received'