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_1552190
_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         'C72 H164 N O24 Si6 U2, C16H36 N, C7 H8'
_chemical_formula_sum            'C95 H208 N2 O24 Si6 U2'
_chemical_formula_weight         2407.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-30 deposited with the CCDC.    2019-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.74703(14)
_cell_length_b                   32.4889(3)
_cell_length_c                   27.4987(3)
_cell_measurement_reflns_used    33567
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.9030
_cell_measurement_theta_min      4.1750
_cell_volume                     12127.7(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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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    -69.00  29.00   1.00    3.98    --  -43.01  57.00-120.00   98
  2  \w   -117.00 -80.00   1.00    3.98    --  -43.01 -99.00-150.00   37
  3  \w   -114.00 -20.00   1.00    3.98    --  -43.01 -57.00  90.00   94
  4  \w     20.00  56.00   1.00    3.98    --   43.01  37.00   0.00   36
  5  \w     42.00  67.00   1.00    3.98    --   43.01-125.00 -90.00   25
  6  \w      1.00  76.00   1.00    3.98    --   43.01 -99.00  30.00   75
  7  \w     35.00 102.00   1.00   15.92    --  109.26 -94.00-180.00   67
  8  \w     28.00  54.00   1.00   15.92    --  109.26 -94.00-150.00   26
  9  \w     75.00 138.00   1.00   15.92    --  109.26 -61.00 -60.00   63
 10  \w     36.00 112.00   1.00   15.92    --  109.26 -45.00  30.00   76
 11  \w     39.00 124.00   1.00   15.92    --  109.26 -30.00-120.00   85
 12  \w     83.00 169.00   1.00   15.92    --  109.26  30.00 -90.00   86
 13  \w     33.00  60.00   1.00   15.92    --  109.26-111.00  60.00   27
 14  \w     78.00 113.00   1.00   15.92    --  109.26-111.00  60.00   35
 15  \w     66.00 109.00   1.00   15.92    --  109.26 -94.00  90.00   43
 16  \w     84.00 113.00   1.00   15.92    --  109.26-111.00 -90.00   29
 17  \w     53.00 107.00   1.00   15.92    --  109.26-111.00   0.00   54
 18  \w    101.00 127.00   1.00   15.92    --  109.26 111.00-150.00   26
 19  \w     45.00 127.00   1.00   15.92    --  109.26 -61.00-180.00   82
 20  \w     57.00 178.00   1.00   15.92    --  109.26  15.00-150.00  121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            89384
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.461
_diffrn_reflns_theta_min         3.528
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.514
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics as
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.007
_refine_diff_density_max         1.877
_refine_diff_density_min         -2.482
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1394
_refine_ls_number_reflns         24736
_refine_ls_number_restraints     482
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0308P)^2^+20.3689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21791
_reflns_number_total             24736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           lb453
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Analytical' changed to
'analytical' 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               1552190
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_shelx_res_checksum              49099