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_1557112
_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         'C72 H89 N6 P U, C4 H10 O'
_chemical_formula_sum            'C76 H99 N6 O P U'
_chemical_formula_weight         1381.61
_chemical_name_systematic        UImNHCNPMe3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-02
_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                 110.09(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.884(5)
_cell_length_b                   13.889(3)
_cell_length_c                   21.315(4)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.735
_cell_measurement_theta_min      2.405
_cell_volume                     7197(3)
_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      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Venture D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            119106
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.670
_diffrn_reflns_theta_min         2.196
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1136 before and 0.0767 after correction.
The Ratio of minimum to maximum transmission is 0.8483.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       needle
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         18514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0168P)^2^+6.0190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15005
_reflns_number_total             18514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05992j2.cif
_cod_data_source_block           uimnhcnpme3
_cod_depositor_comments
;Adding full bibliography for 1557110--1557114.cif.

 Adding full bibliography for 1557110--1557114.cif.
;
_cod_database_code               1557112
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.606
_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. Others
 Sof(C72B)=Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(1)
 Sof(C72A)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(1)
 Fixed Sof: H67(0.5) H67A(0.5) C68A(0.5) H68A(0.5) H68B(0.5) H68C(0.5)
 C68B(0.5) H68D(0.5) H68E(0.5) H68F(0.5) C69A(0.5) H69A(0.5) H69B(0.5)
 H69C(0.5) C69B(0.5) H69D(0.5) H69E(0.5) H69F(0.5)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C33(H33), C40(H40), C48(H48), C55(H55), C60(H60), C67(H67),
 C67(H67A)
3.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C75(H75A,H75B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C23(H23), 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)
3.d 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), 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), C68A(H68A,H68B,H68C),
 C68B(H68D,H68E,H68F), C69A(H69A,H69B,H69C), C69B(H69D,H69E,H69F), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C72A(H72A,H72B,H72C), C72B(H72D,H72E,H72F),
 C73(H73A,H73B,H73C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              96585
_olex2_submission_special_instructions 'No special instructions were received'