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_1550619
_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         'C72 H164 K2 N2 O24 Si6 U2, C7 H8'
_chemical_formula_sum            'C79 H172 K2 N2 O24 Si6 U2'
_chemical_formula_weight         2256.98
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-07 deposited with the CCDC.
2019-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.840(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4207(4)
_cell_length_b                   17.5321(5)
_cell_length_c                   21.9098(6)
_cell_measurement_reflns_used    22809
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      32.1700
_cell_measurement_theta_min      3.6940
_cell_volume                     5536.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  89.00   1.00    9.29    --   18.87  77.00 -30.00  101
  2  \w     22.00  49.00   1.00    9.29    --   18.87  77.00   0.00   27
  3  \w    -56.00  43.00   1.00    9.29    --   18.87 -37.00-180.00   99
  4  \w     35.00  60.00   1.00    9.29    --   18.87-178.00 -90.00   25
  5  \w    -56.00  24.00   1.00    9.29    --   18.87 -37.00  90.00   80
  6  \w    -84.00   5.00   1.00    9.29    --  -18.25 -77.00  60.00   89
  7  \w   -105.00 -67.00   1.00    9.29    --  -18.25 178.00  90.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0007382000
_diffrn_orient_matrix_UB_12      -0.0118031000
_diffrn_orient_matrix_UB_13      -0.0309773000
_diffrn_orient_matrix_UB_21      0.0048868000
_diffrn_orient_matrix_UB_22      -0.0385064000
_diffrn_orient_matrix_UB_23      0.0094465000
_diffrn_orient_matrix_UB_31      -0.0489825000
_diffrn_orient_matrix_UB_32      -0.0036864000
_diffrn_orient_matrix_UB_33      0.0003835000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73741
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.845
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.11577
_exptl_absorpt_correction_T_min  0.08301
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense brown'
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       prism
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.756
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.354
_exptl_crystal_size_rad          0.2513
_refine_diff_density_max         2.543
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         19069
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0382P)^2^+0.8953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13881
_reflns_number_total             19069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05721d2.cif
_cod_data_source_block           lb239
_cod_database_code               1550619
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H169 N2 O24 Si6 K2 U2'
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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
 C61-C67
 1.5 with sigma of 0.01
 C42A-C41 \\sim C43A-C41 \\sim C44A-C41 \\sim C42B-C41 \\sim C43B-C41 \\sim
C44B-C41
 with sigma of 0.02
 C42A-C43A \\sim C43A-C44A \\sim C44A-C42A \\sim C42B-C43B \\sim C43B-C44B
\\sim C44B-C42B
 with sigma of 0.02
 C66-C67 \\sim C67-C62
 with sigma of 0.01
3. Restrained planarity
 C61, C62, C63, C64, C65, C66, C67
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C41 \\sim C42A \\sim C42B \\sim C43A \\sim C43B \\sim C44A \\sim C44B: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43B)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43A)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Fixed Sof: C61(0.5) C66(0.5) H66(0.5) C65(0.5) H65(0.5) C64(0.5) H64(0.5)
 C63(0.5) H63(0.5) C62(0.5) H62(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C66(H66), C65(H65), C64(H64), C63(H63), C62(H62)
6.b Fitted hexagon refined as free rotating group:
 C61(C66,C65,C64,C63,C62)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), 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), C42A(H42A,H42B,H42C),
 C42B(H42D,H42E,H42F), C43A(H43A,H43B,H43C), C43B(H43D,H43E,H43F), C44A(H44A,
 H44B,H44C), C44B(H44D,H44E,H44F), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C67(H67A,H67B,H67C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 8.059
_oxdiff_exptl_absorpt_empirical_full_min 0.538