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_1550617
_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_absolute_configuration rmad
_chemical_formula_moiety         'C73 H162 K2 N2 O24 S2 Si6 U2, 1[C7H8]'
_chemical_formula_sum            'C73 H162 K2 N2 O24 S2 Si6 U2'
_chemical_formula_weight         2238.96
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-22
_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                 92.450(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9065(4)
_cell_length_b                   18.2338(7)
_cell_length_c                   22.1810(9)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      74.1360
_cell_measurement_theta_min      3.9810
_cell_volume                     5619.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_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    -70.00 -11.00   1.00   10.00    --  -39.91 125.00 -30.00   59
  2  \w   -114.00 -32.00   1.00   10.00    --  -39.91 -38.00-180.00   82
  3  \w   -108.00   0.00   1.00   10.00    --  -39.91 -19.00-120.00  108
  4  \w     36.00  91.00   1.00   10.00    --   39.91-125.00 -30.00   55
  5  \w     26.00  81.00   1.00   10.00    --   39.91  77.00  60.00   55
  6  \w      4.00  77.00   1.00   10.00    --   39.91 -99.00 150.00   73
  7  \w     97.00 124.00   1.00   40.00    --  108.90  77.00 150.00   27
  8  \w     62.00 114.00   1.00   40.00    --  108.90-118.00  83.00   52
  9  \w     48.00 140.00   1.00   40.00    --  108.90 -77.00-120.00   92
 10  \w     33.00 137.00   1.00   40.00    --  108.90 -30.00-150.00  104
 11  \w     59.00 117.00   1.00   40.00    --  108.90-125.00 -90.00   58
 12  \w     43.00 133.00   1.00   40.00    --  108.90 -45.00   0.00   90
 13  \w     93.00 118.00   1.00   40.00    --  108.90-125.00   0.00   25
 14  \w     66.00 126.00   1.00   40.00    --  108.90 -45.00 120.00   60
 15  \w     91.00 118.00   1.00   40.00    --  108.90-125.00-180.00   27
 16  \w    143.00 178.00   1.00   40.00    --  108.90  77.00 150.00   35
 17  \w     96.00 147.00   1.00   40.00    --  108.90 125.00 -90.00   51
 18  \w     22.00 171.00   1.00   40.00    --  108.90   0.00 -60.00  149
 19  \w     70.00 141.00   1.00   40.00    --  108.90 -77.00  60.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0197704000
_diffrn_orient_matrix_UB_12      0.0668800000
_diffrn_orient_matrix_UB_13      -0.0410982000
_diffrn_orient_matrix_UB_21      0.0093314000
_diffrn_orient_matrix_UB_22      0.0509660000
_diffrn_orient_matrix_UB_23      0.0553630000
_diffrn_orient_matrix_UB_31      0.1087069000
_diffrn_orient_matrix_UB_32      0.0078266000
_diffrn_orient_matrix_UB_33      -0.0091477000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.1419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38004
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.836
_diffrn_reflns_theta_min         3.139
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.139
_exptl_absorpt_correction_T_max  0.743
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model/Empirical absorption correction using
 spherical harmonics as implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.045
_refine_diff_density_max         3.583
_refine_diff_density_min         -4.163
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.267(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         20460
_refine_ls_number_restraints     1736
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+12.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.836
_reflns_Friedel_fraction_max     0.767
_reflns_number_gt                13621
_reflns_number_total             20460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05721d2.cif
_cod_data_source_block           lb528bis
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               1550617
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C73 H162 N2 O24 Si6 S2 K2 U2'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.733(12)
 0.267(12)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C21-C22 = C21-C24 = C21-C23 = C3-C1 = C4-C1 = C2-C1 = C27-C25 = C26-C25 = C25-
 C28 = C10-C9 = C12-C9 = C11-C9 = C42-C41 = C41-C44 = C41-C43 = C50-C49 = C49-
 C51 = C52-C49 = C5-C8 = C5-C6 = C5-C7 = C32-C29 = C30-C29 = C31-C29 = C45-C46 =
  C45-C48 = C45-C47 = C63-C61 = C64-C61 = C62-C61 = C85-C86 = C87-C85 = C85-C88
 = C69-C70 = C72-C69 = C69-C71 = C91-C89 = C92-C89 = C90-C89 = C83-C81 = C81-
 C82 = C84-C81 = C105-C107 = C105-C106 = C105-C108 = C104-C101 = C103-C101 =
 C102-C101 = C109-C112 = C109-C110 = C111-C109 = C67-C65 = C65-C66 = C65-C68
 1.54 with sigma of 0.01
 U1-N2B \\sim U1-N2A \\sim U2-N2B \\sim U2-N2A
 with sigma of 0.02
 C42-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 C86-C87 \\sim C87-C88 \\sim C88-C86
 with sigma of 0.02
 C111-C112 \\sim C112-C110 \\sim C110-C111
 with sigma of 0.02
 C103-C102 \\sim C102-C104 \\sim C104-C103
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
S1 \\sim S2A \\sim S2B \\sim O1 \\sim O2 \\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 N2A \\sim N2B \\sim C1 \\sim C1A
\\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim
C10 \\sim C11 \\sim C12 \\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:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
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(S2B)=Sof(N2B)=1-FVAR(1)
 Sof(S2A)=Sof(N2A)=FVAR(1)
 Fixed X: U1(0.2528) U2(0.296639)
 Fixed Y: U1(0.42244) U2(0.2953)
 Fixed Z: U1(0.807509) U2(0.69015)
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), 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), 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(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C106(H10M,
 H10N,H10O), C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C110(H11D,H11E,H11F),
 C111(H11G,H11H,H11I), C112(H11J,H11K,H11L)
;
_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 11.236
_oxdiff_exptl_absorpt_empirical_full_min 0.154