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_1552194
_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         'C31 H89 N5 O2 Si10 U2'
_chemical_formula_sum            'C31 H89 N5 O2 Si10 U2'
_chemical_formula_weight         1321.03
_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             2019-02-08
_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                91.085(4)
_cell_angle_beta                 92.236(4)
_cell_angle_gamma                91.691(4)
_cell_formula_units_Z            4
_cell_length_a                   14.4014(6)
_cell_length_b                   19.5701(8)
_cell_length_c                   20.1516(9)
_cell_measurement_reflns_used    11625
_cell_measurement_temperature    139.99(11)
_cell_measurement_theta_max      31.0670
_cell_measurement_theta_min      3.0960
_cell_volume                     5671.5(4)
_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      139.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -10.00  96.00   1.00   95.00    --   19.91  77.00-120.00  106
  2  \w    -56.00  44.00   1.00   95.00    --   19.91 -77.00  30.00  100
  3  \w    -51.00  44.00   1.00   95.00    --   19.91 -38.00  90.00   95
  4  \w    -27.00   0.00   1.00   95.00    --  -20.22 -38.00  30.00   27
  5  \w    -64.00  10.00   1.00   95.00    --  -20.22 -77.00 -60.00   74
  6  \w    -10.00  15.00   1.00   95.00    --  -20.22  57.00   0.00   25
  7  \w   -107.00 -70.00   1.00   95.00    --  -20.22 178.00   0.00   37
;
_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      0.0317509000
_diffrn_orient_matrix_UB_12      -0.0089225000
_diffrn_orient_matrix_UB_13      -0.0245349000
_diffrn_orient_matrix_UB_21      0.0224353000
_diffrn_orient_matrix_UB_22      -0.0220149000
_diffrn_orient_matrix_UB_23      0.0226833000
_diffrn_orient_matrix_UB_31      -0.0303356000
_diffrn_orient_matrix_UB_32      -0.0274052000
_diffrn_orient_matrix_UB_33      -0.0111718000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22606
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.483
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.944
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.388
_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            'clear pale orange'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.993
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         22606
_refine_ls_number_restraints     1010
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0855
_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^)+(0.0900P)^2^+184.0828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16496
_reflns_number_total             22606
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.8917\% 
 around [-0.03 1.00 -0.02] (reciprocal) or [-0.01 1.00 0.00] (direct)
;
_cod_data_source_file            c9sc02149c2.cif
_cod_data_source_block           ctp290_2_twin1_hklf5
_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               1552194
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C31 H89 N5 O2 Si10 U2'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6313(15)
 0.3687(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C21)
Uanis(N1) = Uanis(N3)
Uanis(C75) = Uanis(C76)
Uanis(N7) = Uanis(N8)
Uanis(C25) = Uanis(C26)
Uanis(O2) = Uanis(O1)
Uanis(O4) = Uanis(O3)
4. 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
5.a Me refined with riding coordinates:
 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), 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), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C81(H81A,
 H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C85(H85A,H85B,H85C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,
 H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,
 H10K,H10L), C105(H10M,H10N,H10O), C106(H10P,H10Q,H10R)
5.b X=CH2 refined with riding coordinates:
 C37(H37A,H37B), C87(H87A,H87B)
;
_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 1.952
_oxdiff_exptl_absorpt_empirical_full_min 0.585
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2