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_1557113
_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 N6 U, 2(C3 H7)'
_chemical_formula_sum            'C75 H96 N6 U'
_chemical_formula_weight         1319.60
_chemical_name_systematic        UImNHCN
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-10
_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                90
_cell_angle_beta                 94.521(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7113(8)
_cell_length_b                   12.9790(6)
_cell_length_c                   36.7480(17)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.01
_cell_volume                     6994.8(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            104088
_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         27.565
_diffrn_reflns_theta_min         2.722
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1163 before and 0.0611 after correction. The Ratio of minimum to maximum transmission is 0.7279. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear blackish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.435
_refine_diff_density_min         -2.658
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         16096
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0669
_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^)+41.0102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13716
_reflns_number_total             16096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05992j2.cif
_cod_data_source_block           uimnhcnh
_cod_depositor_comments
;Adding full bibliography for 1557110--1557114.cif.

 Adding full bibliography for 1557110--1557114.cif.
;
_cod_database_code               1557113
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.509
_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. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C6(H6A), C13(H13), C18(H18), C25(H25), C34(H34), C37(H37), C60(H60)
3.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C74(H74A,H74B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C30(H30), C31(H31), C32(H32), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47),
  C48(H48), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56),
 C63(H63), C64(H64), C65(H65)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              14698
_olex2_submission_special_instructions 'No special instructions were received'