Tuning the structure, reactivity and magnetic communication of nitride-bridged uranium complexes with the ancillary ligands
Palumbo, Chad T.; Barluzzi, Luciano; Scopelliti, Rosario; Zivkovic, Ivica; Fabrizio, Alberto; Corminboeuf, Clémence; Mazzanti, Marinella; Chemical Science  (2019) –; doi:10.1039/C9SC02149C

data_1552191
_publ_section_title
;
 Tuning the structure, reactivity and magnetic communication of
 nitride-bridged uranium complexes with the ancillary ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02149C
_journal_year                    2019
_chemical_formula_moiety         'C42 H117 N6 O4 Si11 U2, C12 H30 Na O6'
_chemical_formula_sum            'C54 H147 N6 Na O10 Si11 U2'
_chemical_formula_weight         1848.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-30 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                88.488(2)
_cell_angle_beta                 87.105(2)
_cell_angle_gamma                82.328(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1641(4)
_cell_length_b                   15.3150(4)
_cell_length_c                   19.3228(6)
_cell_measurement_reflns_used    14972
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.4110
_cell_measurement_theta_min      3.6280
_cell_volume                     4440.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.960
_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   -108.00 -17.00   1.00    5.00    --  -43.01 -57.00  60.00   91
  2  \w   -124.00 -80.00   1.00    5.00    --  -43.01 -99.00-180.00   44
  3  \w    -90.00 -30.00   1.00    5.00    --  -43.01 125.00 -90.00   60
  4  \w    -67.00  29.00   1.00    5.00    --  -43.01  57.00-150.00   96
  5  \w   -124.00 -97.00   1.00    5.00    --  -43.01 -99.00-150.00   27
  6  \w   -123.00 -95.00   1.00    5.00    --  -43.01 -99.00 120.00   28
  7  \w     27.00  52.00   1.00    5.00    --   43.01-125.00  30.00   25
  8  \w    105.00 178.00   1.00   20.00    --  105.68  77.00 -30.00   73
  9  \w     90.00 120.00   1.00   20.00    --  105.68 -45.00-180.00   30
 10  \w     45.00  76.00   1.00   20.00    --  105.68 -45.00-180.00   31
 11  \w     34.00 130.00   1.00   20.00    --  105.68 -45.00 -90.00   96
 12  \w     34.00  63.00   1.00   20.00    --  105.68 -61.00  30.00   29
 13  \w     80.00 118.00   1.00   20.00    --  105.68-125.00-150.00   38
 14  \w     59.00  86.00   1.00   20.00    --  105.68 -94.00 120.00   27
 15  \w     45.00 132.00   1.00   20.00    --  105.68 -45.00  30.00   87
 16  \w     72.00 109.00   1.00   20.00    --  105.68 -94.00 -60.00   37
 17  \w     32.00 101.00   1.00   20.00    --  105.68 -94.00 -90.00   69
 18  \w     59.00 107.00   1.00   20.00    --  105.68 -94.00  30.00   48
 19  \w     33.00 108.00   1.00   20.00    --  105.68 -94.00-180.00   75
 20  \w     19.00 172.00   1.00   20.00    --  105.68   0.00 150.00  153
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0506558000
_diffrn_orient_matrix_UB_12      -0.0302436000
_diffrn_orient_matrix_UB_13      -0.0602415000
_diffrn_orient_matrix_UB_21      0.0149568000
_diffrn_orient_matrix_UB_22      0.0844995000
_diffrn_orient_matrix_UB_23      -0.0414619000
_diffrn_orient_matrix_UB_31      0.0879905000
_diffrn_orient_matrix_UB_32      -0.0474499000
_diffrn_orient_matrix_UB_33      -0.0320486000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32284
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.524
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.018
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         17171
_refine_ls_number_restraints     341
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0511P)^2^+10.3375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14852
_reflns_number_total             17171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           ctp293
_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               1552191
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H147 N6 Na O10 Si11 U2'
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Na1-O10A \\sim Na1-O10B \\sim Na1-O9A \\sim Na1-O9B
 with sigma of 0.02
 C80A-C81A \\sim C80B-C81B
 with sigma of 0.02
 O9A-C79A \\sim O9B-C79B \\sim O10A-C82A \\sim O10B-C82B
 with sigma of 0.02
 O9A-C80A \\sim O9B-C80B \\sim O10A-C81A \\sim O10B-C81B
 with sigma of 0.02
 O7A-C75A \\sim O7B-C75B \\sim O8B-C78B
 with sigma of 0.02
 Na1-O7A \\sim Na1-O7B \\sim Na1-O8A \\sim Na1-O8B
 with sigma of 0.02
 C76A-C77A \\sim C77B-C76B
 with sigma of 0.02
 O7A-C76A \\sim O7B-C76B \\sim O8A-C77A \\sim O8B-C77B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7A \\sim O7B \\sim O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B
\\sim C75A \\sim C75B \\sim C76A \\sim C76B \\sim C77A \\sim C77B \\sim C78A
\\sim C78B \\sim C79A \\sim C79B \\sim C80A \\sim C80B \\sim C81A \\sim C81B
\\sim C82A \\sim C82B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(O9B)=Sof(O10B)=Sof(C79B)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C80B)=
 Sof(H80C)=Sof(H80D)=Sof(C81B)=Sof(H81C)=Sof(H81D)=Sof(C82B)=Sof(H82D)=
 Sof(H82E)=Sof(H82F)=1-FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(C79A)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C80A)=
 Sof(H80A)=Sof(H80B)=Sof(C81A)=Sof(H81A)=Sof(H81B)=Sof(C82A)=Sof(H82A)=
 Sof(H82B)=Sof(H82C)=FVAR(1)
 Sof(O7B)=Sof(O8B)=Sof(C75B)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76B)=Sof(H76C)=
 Sof(H76D)=Sof(C77B)=Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78D)=Sof(H78E)=
 Sof(H78F)=1-FVAR(2)
 Sof(O7A)=Sof(O8A)=Sof(C75A)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76A)=Sof(H76A)=
 Sof(H76B)=Sof(C77A)=Sof(H77A)=Sof(H77B)=Sof(C78A)=Sof(H78A)=Sof(H78B)=
 Sof(H78C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C73(H73A,H73B), C76A(H76A,H76B), C76B(H76C,H76D), C77A(H77A,
 H77B), C77B(H77C,H77D), C80A(H80A,H80B), C80B(H80C,H80D), C81A(H81A,H81B),
 C81B(H81C,H81D)
5.b 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), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C),
 C75A(H75A,H75B,H75C), C75B(H75D,H75E,H75F), C78A(H78A,H78B,H78C), C78B(H78D,
 H78E,H78F), C79A(H79A,H79B,H79C), C79B(H79D,H79E,H79F), C82A(H82A,H82B,H82C),
 C82B(H82D,H82E,H82F)
;
_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 6.628
_oxdiff_exptl_absorpt_empirical_full_min 0.510