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_1552196
_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         'C74 H162 N O28 Si6 U2, C16 H36 N'
_chemical_formula_sum            'C90 H198 N2 O28 Si6 U2'
_chemical_formula_weight         2401.09
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-05
_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                90
_cell_angle_beta                 96.8053(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9403(2)
_cell_length_b                   40.0672(5)
_cell_length_c                   17.9903(2)
_cell_measurement_reflns_used    45603
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.7920
_cell_measurement_theta_min      2.8300
_cell_volume                     12124.9(2)
_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 (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 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_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   -106.00 -79.00   0.50    2.00    --  -40.66 -57.00 -60.00   54
  2  \w    -70.00 -33.00   0.50    2.00    --  -40.66  77.00-150.00   74
  3  \w    -70.00  35.00   0.50    2.00    --  -40.66  77.00 -30.00  210
  4  \w    -69.00  23.00   0.50    2.00    --  -40.66  77.00  90.00  184
  5  \w   -108.00 -19.00   0.50    2.00    --  -40.66 -38.00-180.00  178
  6  \w      9.00  34.00   0.50    2.00    --  -40.66  77.00-150.00   50
  7  \w     36.00 136.00   0.50    8.00    --  107.65 -30.00 150.00  200
  8  \w     98.00 159.00   0.50    8.00    --  107.65 125.00 120.00  122
  9  \w     94.00 138.00   0.50    8.00    --  107.65 125.00-120.00   88
 10  \w     94.00 174.00   0.50    8.00    --  107.65 125.00-150.00  160
 11  \w     47.00 118.00   0.50    8.00    --  107.65-125.00-180.00  142
 12  \w     47.00 139.00   0.50    8.00    --  107.65 -77.00-180.00  184
 13  \w     97.00 126.00   0.50    8.00    --  107.65 125.00-180.00   58
 14  \w     89.00 114.00   0.50    8.00    --  107.65-125.00 -60.00   50
 15  \w    105.00 171.00   0.50    8.00    --  107.65  45.00-180.00  132
 16  \w     63.00 116.00   0.50    8.00    --  107.65-125.00  30.00  106
 17  \w     85.00 178.00   0.50    8.00    --  107.65  77.00 -60.00  186
 18  \w     80.00 109.00   0.50    8.00    --  107.65 -94.00   0.00   58
 19  \w     53.00 101.00   0.50    8.00    --  107.65 -45.00 -30.00   96
;
_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      0.0556858000
_diffrn_orient_matrix_UB_12      0.0160033000
_diffrn_orient_matrix_UB_13      0.0641091000
_diffrn_orient_matrix_UB_21      0.0706206000
_diffrn_orient_matrix_UB_22      -0.0197692000
_diffrn_orient_matrix_UB_23      -0.0243527000
_diffrn_orient_matrix_UB_31      0.0175325000
_diffrn_orient_matrix_UB_32      0.0287974000
_diffrn_orient_matrix_UB_33      -0.0523217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            78966
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.245
_diffrn_reflns_theta_min         2.708
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.541
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_correction_T_min  0.207
_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            'clear light blue'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       prism
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.196
_refine_diff_density_max         6.335
_refine_diff_density_min         -6.619
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         24134
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0826P)^2^+201.0061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.1906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22290
_reflns_number_total             24134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           lb541
_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_original_cell_volume        12124.9(3)
_cod_database_code               1552196
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C90 H198 N2 O28 Si6 U2'
_reflns_odcompleteness_completeness 99.42
_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
 C83A-C81 = C84A-C81 = C82A-C81 = C83B-C81 = C84B-C81 = C82B-C81
 1.54 with sigma of 0.02
 C83A-C84A \\sim C84A-C82A \\sim C82A-C83A \\sim C83B-C84B \\sim C84B-C82B
\\sim C82B-C83B
 with sigma of 0.02
 Si4-O83A \\sim Si4-O83B \\sim Si4-O84A \\sim Si4-O84B \\sim Si4-O82A \\sim
Si4-O82B
 with sigma of 0.02
 C83A-C84A \\sim C82A-C84A \\sim C82A-C83A \\sim C83B-C84B \\sim C82B-C84B
\\sim C82B-C83B
 with sigma of 0.02
 O83A-C85 \\sim C85-O83B \\sim O84A-C89 \\sim C89-O84B \\sim O82A-C81 \\sim
C81-O82B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\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
C81 \\sim C82A \\sim C83A \\sim C84A \\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 C121 \\sim C122 \\sim C123 \\sim C124 \\sim C129 \\sim
C130 \\sim C131 \\sim C132 \\sim C82B \\sim C83B \\sim C84B \\sim O42 \\sim O81
\\sim O82A \\sim O83A \\sim O84A \\sim O101 \\sim O104 \\sim O82B \\sim O83B
\\sim O84B \\sim O102: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Sof(O82B)=Sof(O83B)=Sof(O84B)=Sof(C82B)=Sof(H82D)=Sof(H82E)=Sof(H82F)=
 Sof(C83B)=Sof(H83D)=Sof(H83E)=Sof(H83F)=Sof(C84B)=Sof(H84D)=Sof(H84E)=
 Sof(H84F)=1-FVAR(1)
 Sof(O82A)=Sof(O83A)=Sof(O84A)=Sof(C82A)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C83A)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C84A)=Sof(H84A)=Sof(H84B)=
 Sof(H84C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C141(H14A,H14B), C142(H14C,H14D), C143(H14E,H14F), C145(H14J,H14K), C146(H14L,
 H14M), C147(H14N,H14O), C149(H14S,H14T), C150(H15A,H15B), C151(H15C,H15D),
 C153(H15H,H15I), C154(H15J,H15K), C155(H15L,H15M)
5.b Me refined with riding coordinates:
 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), C82A(H82A,H82B,H82C), C83A(H83A,H83B,H83C),
 C84A(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(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I), C106(H10J,
 H10K,H10L), C107(H10M,H10N,H10O), C108(H10P,H10Q,H10R), C110(H11A,H11B,H11C),
 C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C122(H12A,H12B,H12C), C123(H12D,
 H12E,H12F), C124(H12G,H12H,H12I), C126(H12J,H12K,H12L), C127(H12M,H12N,H12O),
 C128(H12P,H12Q,H12R), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,
 H13H,H13I), C144(H14G,H14H,H14I), C148(H14P,H14Q,H14R), C152(H15E,H15F,H15G),
 C156(H15N,H15O,H15P), C82B(H82D,H82E,H82F), C83B(H83D,H83E,H83F), C84B(H84D,
 H84E,H84F)
;
_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 2.255
_oxdiff_exptl_absorpt_empirical_full_min 0.636