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_1552195
_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         'C36 H108 N7 Si12 U2, 2(C7 H8)'
_chemical_formula_sum            'C50 H124 N7 Si12 U2'
_chemical_formula_weight         1636.69
_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             2019-02-15
_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                 110.2211(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.65806(12)
_cell_length_b                   31.4333(2)
_cell_length_c                   17.60034(19)
_cell_measurement_reflns_used    41543
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.5820
_cell_measurement_theta_min      3.4970
_cell_volume                     7609.56(13)
_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      139.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -57.00  39.00   1.00    3.00    --  -40.66  19.00-120.00   96
  2  \w   -115.00 -16.00   1.00    3.00    --  -40.66 -38.00  60.00   99
  3  \w     27.00  54.00   1.00    3.00    --   40.66-125.00-120.00   27
  4  \w     28.00  97.00   1.00    3.00    --   40.66-125.00 -90.00   69
  5  \w    -31.00  69.00   1.00    3.00    --   40.66 -57.00 -60.00  100
  6  \w     28.00  84.00   1.00    3.00    --   40.66-125.00  90.00   56
  7  \w     74.00 113.00   1.00   12.00    --  112.00-111.00 150.00   39
  8  \w     36.00  62.00   1.00   12.00    --  112.00-111.00 150.00   26
  9  \w     41.00 136.00   1.00   12.00    --  112.00 -61.00 150.00   95
 10  \w     36.00  70.00   1.00   12.00    --  112.00 -77.00  30.00   34
 11  \w     84.00 116.00   1.00   12.00    --  112.00  30.00-120.00   32
 12  \w    116.00 143.00   1.00   12.00    --  112.00 111.00 120.00   27
 13  \w     55.00  82.00   1.00   12.00    --  112.00-111.00-120.00   27
 14  \w     85.00 111.00   1.00   12.00    --  112.00-111.00-120.00   26
 15  \w     48.00 113.00   1.00   12.00    --  112.00-111.00 -30.00   65
 16  \w     84.00 178.00   1.00   12.00    --  112.00  30.00-180.00   94
 17  \w     59.00 113.00   1.00   12.00    --  112.00-111.00  90.00   54
 18  \w     44.00  88.00   1.00   12.00    --  112.00 -61.00  90.00   44
 19  \w     68.00 113.00   1.00   12.00    --  112.00-111.00 -60.00   45
 20  \w     46.00  72.00   1.00   12.00    --  112.00-111.00-150.00   26
 21  \w     76.00 113.00   1.00   12.00    --  112.00-111.00-150.00   37
 22  \w     59.00  89.00   1.00   12.00    --  112.00-111.00 120.00   30
 23  \w    108.00 137.00   1.00   12.00    --  112.00 111.00-180.00   29
 24  \w    112.00 177.00   1.00   12.00    --  112.00 111.00  90.00   65
 25  \w     65.00  94.00   1.00   12.00    --  112.00  15.00 -30.00   29
 26  \w    101.00 155.00   1.00   12.00    --  112.00  15.00 -30.00   54
 27  \w     55.00  80.00   1.00   12.00    --  112.00 -61.00 120.00   25
 28  \w    115.00 140.00   1.00   12.00    --  112.00 -61.00 120.00   25
 29  \w     70.00 113.00   1.00   12.00    --  112.00-111.00  30.00   43
 30  \w     43.00  91.00   1.00   12.00    --  112.00 -94.00 -30.00   48
 31  \w    116.00 143.00   1.00   12.00    --  112.00 -77.00  60.00   27
 32  \w     30.00  71.00   1.00   12.00    --  112.00 -94.00  30.00   41
 33  \w    116.00 178.00   1.00   12.00    --  112.00  15.00  90.00   62
 34  \w     62.00  88.00   1.00   12.00    --  112.00  15.00  90.00   26
 35  \w     36.00 109.00   1.00   12.00    --  112.00 -30.00-180.00   73
 36  \w    106.00 131.00   1.00   12.00    --  112.00 -61.00  90.00   25
 37  \w     37.00 106.00   1.00   12.00    --  112.00 -30.00   0.00   69
 38  \w     37.00  67.00   1.00   12.00    --  112.00 -94.00   0.00   30
;
_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      -0.0748111000
_diffrn_orient_matrix_UB_12      -0.0215122000
_diffrn_orient_matrix_UB_13      -0.0741885000
_diffrn_orient_matrix_UB_21      -0.0095757000
_diffrn_orient_matrix_UB_22      -0.0371084000
_diffrn_orient_matrix_UB_23      0.0538856000
_diffrn_orient_matrix_UB_31      -0.0828136000
_diffrn_orient_matrix_UB_32      0.0237039000
_diffrn_orient_matrix_UB_33      0.0171598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80831
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.184
_diffrn_reflns_theta_min         2.812
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.952
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20756
_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 dark green'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       needle
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.962
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         15824
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+41.1699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14974
_reflns_number_total             15824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           ctp280
_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               1552195
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C50 H124 N7 Si12 U2'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C86B-C81B = C77B-C71B = C81A-C87A = C71A-C77A
 1.5 with sigma of 0.02
 C20-C86B \\sim C86B-C82B \\sim C82A-C87A \\sim C87A-C86A \\sim C76A-C77A \\sim
C77A-C72A \\sim C72B-
 C77B \\sim C77B-C76B
 with sigma of 0.02
3. Restrained planarity
 C20, C81B, C82B, C83B, C84B, C85B, C86B
 with sigma of 0.1
 C81A, C82A, C83A, C84A, C85A, C86A, C87A
 with sigma of 0.1
 C71A, C72A, C73A, C74A, C75A, C76A, C77A
 with sigma of 0.1
 C71B, C72B, C73B, C74B, C75B, C76B, C77B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C71A \\sim C76A \\sim C75A \\sim C74A \\sim C73A \\sim C72A \\sim C71B \\sim
C72B \\sim C73B \\sim C74B \\sim C75B \\sim C76B \\sim C81A \\sim C86A \\sim
C85A \\sim C84A \\sim C83A \\sim C82A \\sim C81B \\sim C20 \\sim C85B \\sim
C84B \\sim C83B \\sim C82B \\sim C87A \\sim C86B \\sim C77B \\sim C77A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C81B)=Sof(C82B)=Sof(H82B)=Sof(C83B)=Sof(H83B)=Sof(C84B)=Sof(H84B)=
 Sof(C85B)=Sof(H85B)=Sof(C20)=Sof(H20)=Sof(C86B)=Sof(H86A)=Sof(H86B)=Sof(H86C)=
 1-FVAR(1)
 Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(H84A)=
 Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86D)=Sof(C87A)=Sof(H87A)=Sof(H87B)=
 Sof(H87C)=FVAR(1)
 Sof(C71B)=Sof(C76B)=Sof(H76B)=Sof(C75B)=Sof(H75B)=Sof(C74B)=Sof(H74B)=
 Sof(C73B)=Sof(H73B)=Sof(C72B)=Sof(H72B)=Sof(C77B)=Sof(H77D)=Sof(H77E)=
 Sof(H77F)=1-FVAR(2)
 Sof(C71A)=Sof(C76A)=Sof(H76A)=Sof(C75A)=Sof(H75A)=Sof(C74A)=Sof(H74A)=
 Sof(C73A)=Sof(H73A)=Sof(C72A)=Sof(H72A)=Sof(C77A)=Sof(H77A)=Sof(H77B)=
 Sof(H77C)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C82B(H82B), C83B(H83B), C84B(H84B), C85B(H85B), C20(H20), C76A(H76A),
 C75A(H75A), C74A(H74A), C73A(H73A), C72A(H72A), C76B(H76B), C75B(H75B),
 C74B(H74B), C73B(H73B), C72B(H72B), C82A(H82A), C83A(H83A), C84A(H84A),
 C85A(H85A), C86A(H86D)
6.b Fitted hexagon refined as free rotating group:
 C81B(C82B,C83B,C84B,C85B,C20), C71A(C76A,C75A,C74A,C73A,C72A), C71B(C76B,C75B,
 C74B,C73B,C72B), C81A(C82A,C83A,C84A,C85A,C86A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), 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), C86B(H86A,H86B,H86C), C77A(H77A,H77B,
 H77C), C77B(H77D,H77E,H77F), C87A(H87A,H87B,H87C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.032
_oxdiff_exptl_absorpt_empirical_full_min 0.683