Facile N-functionalization and strong magnetic communication in a diuranium(v) bis-nitride complex
Barluzzi, Luciano; Chatelain, Lucile; Fadaei-Tirani, Farzaneh; Zivkovic, Ivica; Mazzanti, Marinella; Chemical Science  (2019) –; doi:10.1039/C8SC05721D

data_1550618
_publ_section_title
;
 Facile N-functionalization and strong magnetic communication in a
 diuranium(v) bis-nitride complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05721D
_journal_year                    2019
_chemical_formula_moiety         'C74 H162 K2 N2 O26 Si6 U2, C7 H8'
_chemical_formula_sum            'C81 H170 K2 N2 O26 Si6 U2'
_chemical_formula_weight         2310.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.321(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9927(15)
_cell_length_b                   18.2874(12)
_cell_length_c                   22.208(2)
_cell_measurement_reflns_used    186
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     5673.3(9)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67143
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_min         2.278
_exptl_absorpt_coefficient_mu    3.049
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0945 before and 0.0782 after correction.
The Ratio of minimum to maximum transmission is 0.7606.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.148(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         20671
_refine_ls_number_restraints     1858
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0373P)^2^+20.4152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                17177
_reflns_number_total             20671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05721d2.cif
_cod_data_source_block           lb208
_cod_original_cell_volume        5673.2(9)
_cod_database_code               1550618
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.852(8)
 0.148(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C2A
 1.18 with sigma of 0.01
 O1B-C2A
 1.2 with sigma of 0.01
 C110-C109 = C112-C109 = C111-C109
 1.54 with sigma of 0.02
 C207-C201
 1.54 with sigma of 0.02
 N2-O1B
 2.41 with sigma of 0.005
 N1-C1A \\sim O1A-C1A
 with sigma of 0.02
 C9-C10A \\sim C9-C11A \\sim C9-C12A \\sim C9-C10B \\sim C9-C11B \\sim C9-C12B
 with sigma of 0.02
 C10A-C12A \\sim C12A-C11A \\sim C11A-C10A \\sim C11B-C10B \\sim C10B-C12B
\\sim C12B-C11B
 with sigma of 0.02
 C110-C111 \\sim C111-C112 \\sim C112-C110
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10A \\sim C10B \\sim C11A \\sim C11B \\sim C12A \\sim
C12B \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27
\\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51
\\sim C52 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67
\\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C81 \\sim C82 \\sim C83
\\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91
\\sim C92 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106
\\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111 \\sim C112 \\sim C201
\\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim O1
\\sim O1A \\sim O1B \\sim O2 \\sim O2A \\sim O3 \\sim O4 \\sim O21 \\sim O22
\\sim O23 \\sim O24 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O61 \\sim O62
\\sim O63 \\sim O64 \\sim O81 \\sim O82 \\sim O83 \\sim O84 \\sim O101 \\sim
O102 \\sim O103 \\sim O104 \\sim N1 \\sim N2: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O63) \\sim Ueq, Uanis(O62) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(O103)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11B)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: O1A(0.5) O1B(0.5)
7.a Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F),
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C12A(H12A,H12B,H12C), C12B(H12D,
 H12E,H12F), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,
 H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C),
 C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C104(H10M,H10N,H10O), C106(H10P,
 H10Q,H10R), C107(H10S,H10T,H10U), C108(H10V,H10W,H10X), C110(H11G,H11H,H11I),
 C111(H11J,H11K,H11L), C112(H11M,H11N,H11O), C207(H20A,H20B,H20C)
7.b Aromatic/amide H refined with riding coordinates:
 C202(H202), C203(H203), C204(H204), C205(H205), C206(H206)
7.c Fitted hexagon refined as free rotating group:
 C201(C202,C203,C204,C205,C206)
;
_olex2_submission_special_instructions 'No special instructions were received'