Nitrogen activation and cleavage by a multimetallic uranium complex.
Keener, Megan; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Zivkovic, Ivica; Mazzanti, Marinella; Chemical science 13 (2022) 8025–8035; doi:10.1039/d2sc02997a

data_1567206
_publ_section_title
;
 Nitrogen activation and cleavage by a multimetallic uranium complex.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8025
_journal_page_last               8035
_journal_paper_doi               10.1039/d2sc02997a
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C48 H126 K N5 O8 Si10 U2, 0.3(C4 H10 O)'
_chemical_formula_sum            'C49.2 H129 K N5 O8.3 Si10 U2'
_chemical_formula_weight         1719.83
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9855(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.81649(7)
_cell_length_b                   23.44652(10)
_cell_length_c                   27.38157(13)
_cell_measurement_reflns_used    41708
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5810
_cell_measurement_theta_min      3.5590
_cell_volume                     8077.44(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -77.00   5.00   1.00    2.00    --  -40.91 106.00  69.00   82
  2  \w     26.00  53.00   1.00    2.00    --   40.91-106.00 -29.00   27
  3  \w    104.00 166.00   1.00    8.00    --  105.15 106.00  69.00   62
  4  \w     64.00 108.00   1.00    8.00    --  105.15-106.00 -29.00   44
  5  \w    -65.00  17.00   1.00    2.00    --  -40.91  38.00  90.00   82
  6  \w   -115.00 -17.00   1.00    2.00    --  -40.91 -38.00 -90.00   98
  7  \w     32.00  95.00   1.00    2.00    --   40.91-125.00 -60.00   63
  8  \w     17.00  97.00   1.00    2.00    --   40.91  57.00-150.00   80
  9  \w     34.00 103.00   1.00    8.00    --  105.15 -94.00   0.00   69
 10  \w    110.00 151.00   1.00    8.00    --  105.15  77.00  30.00   41
 11  \w     77.00 163.00   1.00    8.00    --  105.15  61.00 120.00   86
 12  \w    124.00 177.00   1.00    8.00    --  105.15 111.00  30.00   53
 13  \w     28.00 103.00   1.00    8.00    --  105.15 -94.00  90.00   75
 14  \w     47.00  81.00   1.00    8.00    --  105.15 -94.00-180.00   34
 15  \w     60.00 109.00   1.00    8.00    --  105.15-111.00 150.00   49
 16  \w    104.00 155.00   1.00    8.00    --  105.15  77.00-120.00   51
 17  \w    128.00 164.00   1.00    8.00    --  105.15  61.00 150.00   36
 18  \w     60.00 107.00   1.00    8.00    --  105.15-111.00-120.00   47
 19  \w    111.00 178.00   1.00    8.00    --  105.15 111.00 150.00   67
 20  \w     85.00 125.00   1.00    8.00    --  105.15 178.00 -30.00   40
 21  \w    106.00 148.00   1.00    8.00    --  105.15 111.00-180.00   42
 22  \w     36.00 133.00   1.00    8.00    --  105.15 -30.00  90.00   97
;
_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      0.0638708000
_diffrn_orient_matrix_UB_12      -0.0134846000
_diffrn_orient_matrix_UB_13      0.0522815000
_diffrn_orient_matrix_UB_21      -0.1043888000
_diffrn_orient_matrix_UB_22      -0.0108110000
_diffrn_orient_matrix_UB_23      0.0186171000
_diffrn_orient_matrix_UB_31      0.0042200000
_diffrn_orient_matrix_UB_32      -0.0634038000
_diffrn_orient_matrix_UB_33      -0.0142507000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            63014
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.672
_diffrn_reflns_theta_min         3.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.420
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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 intense orange'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       prism
_exptl_crystal_F_000             3474
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         15884
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.8747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15444
_reflns_number_total             15884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02997a2.cif
_cod_data_source_block           mk-73
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1567201--1567212.cif.
;
_cod_original_formula_sum        'C49.20 H129 K N5 O8.30 Si10 U2'
_cod_database_code               1567206
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C49.20 H129 K N5 O8.30 Si10 U2'
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.069
_reflns_odcompleteness_completeness 99.97
_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
 O9-C51
 1.41 with sigma of 0.02
 C49-C50
 1.5 with sigma of 0.02
 O9-C49
 1.42 with sigma of 0.02
 C52-C51
 1.48 with sigma of 0.02
 O9-C52 = O9-C50
 2.37 with sigma of 0.04
 C6B-C7B \\sim C7B-C8B \\sim C8B-C6B
 with sigma of 0.02
 C6A-C7A \\sim C7A-C8A \\sim C8A-C6A
 with sigma of 0.02
 C6A-C5 \\sim C6B-C5 \\sim C7A-C5 \\sim C7B-C5 \\sim C8A-C5 \\sim C8B-C5
 with sigma of 0.02
 Si7-C37B \\sim Si7-C37A \\sim Si7-C39A \\sim Si7-C39B
 with sigma of 0.02
 C37A-C39A \\sim C37B-C39B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6A \\sim C6B \\sim C7A \\sim C7B \\sim C8A \\sim C8B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Si7 \\sim C37A \\sim C37B \\sim C38 \\sim C39A \\sim C39B: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=1-FVAR(1)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=FVAR(1)
 Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C39B)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=1-FVAR(2)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=FVAR(2)
 Fixed Sof: O9(0.3) C49(0.3) H49A(0.3) H49B(0.3) C50(0.3) H50A(0.3) H50B(0.3)
 H50C(0.3) C51(0.3) H51A(0.3) H51B(0.3) C52(0.3) H52A(0.3) H52B(0.3) H52C(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C51(H51A,H51B)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6A(H6AA,H6AB,H6AC),
 C6B(H6BA,H6BB,H6BC), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC), C8A(H8AA,H8AB,
 H8AC), C8B(H8BA,H8BB,H8BC), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), 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), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C38(H38A,H38B,H38C), C39A(H39A,
 H39B,H39C), C39B(H39D,H39E,H39F), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              26266
_shelx_hkl_checksum              44182
_olex2_date_sample_data_collection 2020-12-18
_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 2.060
_oxdiff_exptl_absorpt_empirical_full_min 0.640