Consecutive N<sub>2</sub> loss from a uranium diphosphazide complex.
Dickie, Tara K. K.; MacNeil, Connor S.; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 578–582; doi:10.1039/c9dt04517a

data_7703340
_publ_section_title
;
 Consecutive N<sub>2</sub> loss from a uranium diphosphazide complex.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              578
_journal_page_last               582
_journal_paper_doi               10.1039/c9dt04517a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H32 Cl2 N6 O2 P2 U'
_chemical_formula_sum            'C42 H32 Cl2 N6 O2 P2 U'
_chemical_formula_weight         1023.60
_chemical_name_systematic        Phosphazide-UCl2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-19 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                103.8451(5)
_cell_angle_beta                 95.7658(6)
_cell_angle_gamma                102.8388(6)
_cell_formula_units_Z            2
_cell_length_a                   10.72961(8)
_cell_length_b                   11.58355(6)
_cell_length_c                   19.45445(11)
_cell_measurement_reflns_used    74553
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.9290
_cell_measurement_theta_min      4.0340
_cell_volume                     2258.64(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   -108.00 -34.00   0.50    0.50    --  -38.50 -24.00 112.14  148
  2  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00-120.00  150
  3  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00  60.00  176
  4  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00 -60.00  176
  5  \w   -108.00 -33.00   0.50    0.50    --  -38.50 -19.00-180.00  150
  6  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00   0.00  176
  7  \w    -90.00  -2.00   0.50    0.50    --  -38.50 125.00   0.00  176
  8  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00-180.00  176
  9  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00-120.00  176
 10  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00 120.00  176
 11  \w     23.00 101.00   0.50    0.50    --   50.22-125.00-120.00  156
 12  \w     27.00 115.00   0.50    0.50    --   50.22  77.00 -30.00  176
 13  \w     27.00 115.00   0.50    0.50    --   50.22  77.00 -90.00  176
 14  \w     27.00 115.00   0.50    0.50    --   50.22  77.00-180.00  176
 15  \w     27.00 115.00   0.50    0.50    --   50.22  77.00  90.00  176
 16  \w     27.00 115.00   0.50    0.50    --   50.22  77.00   0.00  176
 17  \w     23.00 101.00   0.50    0.50    --   50.22-125.00  60.00  156
 18  \w     27.00 115.00   0.50    0.50    --   50.22  77.00  30.00  176
 19  \w     27.00 115.00   0.50    0.50    --   50.22  77.00  60.00  176
 20  \w     27.00 115.00   0.50    0.50    --   50.22  77.00 120.00  176
 21  \w     27.00 115.00   0.50    0.50    --   50.22  77.00 150.00  176
 22  \w     27.00 115.00   0.50    0.50    --   50.22  77.00-150.00  176
 23  \w     27.00 115.00   0.50    0.50    --   50.22  77.00 -60.00  176
 24  \w     27.00 115.00   0.50    0.50    --   50.22  77.00-120.00  176
 25  \w     88.00 176.00   0.50    1.38    --  111.00  77.00 -60.00  176
 26  \w     98.00 174.00   0.50    1.38    --  111.00  61.00 -30.00  152
 27  \w     41.00 116.00   0.50    1.38    --  111.00-111.00 -30.00  150
 28  \w     98.00 174.00   0.50    1.38    --  111.00  61.00   0.00  152
 29  \w     88.00 176.00   0.50    1.38    --  111.00  77.00-120.00  176
 30  \w     88.00 176.00   0.50    1.38    --  111.00  77.00 -30.00  176
 31  \w     41.00 116.00   0.50    1.38    --  111.00-111.00 -60.00  150
 32  \w     41.00 116.00   0.50    1.38    --  111.00-111.00-150.00  150
 33  \w     48.00 124.00   0.50    1.38    --  111.00 -61.00 -60.00  152
 34  \w     88.00 176.00   0.50    1.38    --  111.00  77.00  90.00  176
 35  \w     88.00 176.00   0.50    1.38    --  111.00  77.00-150.00  176
 36  \w     88.00 176.00   0.50    1.38    --  111.00  77.00 120.00  176
 37  \w     88.00 176.00   0.50    1.38    --  111.00  77.00   0.00  176
 38  \w     42.00 109.00   0.50    1.38    --  111.00 -94.00-120.00  134
 39  \w     41.00 116.00   0.50    1.38    --  111.00-111.00 150.00  150
 40  \w     98.00 174.00   0.50    1.38    --  111.00  61.00 150.00  152
 41  \w     88.00 176.00   0.50    1.38    --  111.00  77.00 150.00  176
 42  \w     43.00 115.00   0.50    1.38    --  111.00 -30.00  60.00  144
 43  \w     98.00 174.00   0.50    1.38    --  111.00  61.00 -90.00  152
 44  \w     88.00 176.00   0.50    1.38    --  111.00  77.00  60.00  176
 45  \w     98.00 174.00   0.50    1.38    --  111.00  61.00  30.00  152
 46  \w     88.00 176.00   0.50    1.38    --  111.00  77.00 -90.00  176
 47  \w     98.00 174.00   0.50    1.38    --  111.00  61.00-180.00  152
 48  \w     88.00 176.00   0.50    1.38    --  111.00  77.00-180.00  176
 49  \w     42.00 109.00   0.50    1.38    --  111.00 -94.00-150.00  134
 50  \w     98.00 174.00   0.50    1.38    --  111.00  61.00-150.00  152
 51  \w     41.00 116.00   0.50    1.38    --  111.00-111.00  90.00  150
 52  \w     98.00 174.00   0.50    1.38    --  111.00  61.00  60.00  152
 53  \w     98.00 174.00   0.50    1.38    --  111.00  61.00 -60.00  152
 54  \w     48.00 124.00   0.50    1.38    --  111.00 -61.00  90.00  152
 55  \w     88.00 176.00   0.50    1.38    --  111.00  77.00  30.00  176
 56  \w     42.00 109.00   0.50    1.38    --  111.00 -94.00 -30.00  134
 57  \w     42.00 109.00   0.50    1.38    --  111.00 -94.00  60.00  134
 58  \w     41.00 116.00   0.50    1.38    --  111.00-111.00  30.00  150
 59  \w     41.00 116.00   0.50    1.38    --  111.00-111.00 120.00  150
 60  \w     98.00 174.00   0.50    1.38    --  111.00  61.00  90.00  152
 61  \w     98.00 174.00   0.50    1.38    --  111.00  61.00-120.00  152
 62  \w     41.00 116.00   0.50    1.38    --  111.00-111.00 -90.00  150
 63  \w     98.00 174.00   0.50    1.38    --  111.00  61.00 120.00  152
 64  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00  90.00  176
 65  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00-150.00  176
 66  \w    -44.00  31.00   0.50    0.50    --  -38.50  19.00-150.00  150
 67  \w   -102.00 -27.00   0.50    0.50    --  -38.50 -57.00-120.00  150
 68  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00  30.00  140
 69  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00 -60.00  140
 70  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00  90.00  140
 71  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00 -90.00  140
 72  \w     47.00 117.00   0.50    0.50    --   50.22  38.00-120.00  140
 73  \w     39.00 113.00   0.50    0.50    --   50.22  57.00  60.00  148
 74  \w     47.00 117.00   0.50    0.50    --   50.22  38.00 120.00  140
 75  \w     47.00 117.00   0.50    0.50    --   50.22  38.00  60.00  140
 76  \w     47.00 117.00   0.50    0.50    --   50.22  38.00 -60.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1418376000
_diffrn_orient_matrix_UB_12      -0.0268347000
_diffrn_orient_matrix_UB_13      0.0125658000
_diffrn_orient_matrix_UB_21      0.0415312000
_diffrn_orient_matrix_UB_22      0.0907423000
_diffrn_orient_matrix_UB_23      0.0753041000
_diffrn_orient_matrix_UB_31      -0.0207365000
_diffrn_orient_matrix_UB_32      0.1054126000
_diffrn_orient_matrix_UB_33      -0.0316700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.192
_diffrn_reflns_theta_min         4.065
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.192
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_preparation       TD
_exptl_crystal_recrystallization_method TD
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0227P)^2^+5.2530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9635
_reflns_number_total             9778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph17009
_cod_database_code               7703340
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H37 Cl2 N6 O3 P2 U1'
_chemical_oxdiff_usercomment     'Block orange crystal'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42)
;
_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 2.051
_oxdiff_exptl_absorpt_empirical_full_min 0.771