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_7703339
_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 H33 Cl3 N4 O2 P2 U, 2(C6 H6)'
_chemical_formula_sum            'C54 H45 Cl3 N4 O2 P2 U'
_chemical_formula_weight         1188.26
_chemical_name_systematic        P(N3)-P=N
_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'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 94.9425(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.79440(10)
_cell_length_b                   17.44271(12)
_cell_length_c                   20.42070(16)
_cell_measurement_reflns_used    43167
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      79.3350
_cell_measurement_theta_min      4.0660
_cell_volume                     4895.19(6)
_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      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_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   -108.00  31.00   0.50    0.50    --  -38.50   0.00 150.00  278
  2  \w    -42.00  28.00   0.50    0.50    --  -38.50  38.00   0.00  140
  3  \w     45.00 115.00   0.50    0.50    --   48.81  38.00  60.00  140
  4  \w    -14.00  61.00   0.50    0.50    --   48.81 -57.00 -90.00  150
  5  \w     57.00 151.00   0.50    0.50    --  111.00 178.00  90.00  188
  6  \w     47.00 117.00   0.50    0.50    --  111.00 -50.00  30.00  140
  7  \w     45.00 115.00   0.50    0.50    --  111.00 -38.00  90.00  140
  8  \w    101.00 178.00   0.50    0.50    --  111.00  12.00-120.00  154
  9  \w     57.00 151.00   0.50    0.50    --  111.00 178.00 120.00  188
 10  \w     41.00 116.00   0.50    0.50    --  111.00-111.00-120.00  150
 11  \w     41.00 115.00   0.50    0.50    --  111.00 -25.00  60.00  148
 12  \w    105.00 175.00   0.50    0.50    --  111.00  50.00-150.00  140
 13  \w     41.00 116.00   0.50    0.50    --  111.00-111.00 -90.00  150
 14  \w     46.00 134.00   0.50    0.50    --  111.00 -77.00  60.00  176
 15  \w     45.00 115.00   0.50    0.50    --  111.00 -38.00 -90.00  140
 16  \w     41.00 121.00   0.50    0.50    --  111.00 -12.00  30.00  160
 17  \w     47.00 125.00   0.50    0.50    --  111.00-133.00  46.00  156
 18  \w     59.00 150.00   0.50    0.50    --  111.00 178.00  60.00  182
 19  \w     47.00 112.00   0.50    0.50    --  111.00 -38.00   0.00  130
 20  \w    130.00 156.00   0.50    0.50    --  111.00  50.00   0.00   52
 21  \w     69.00 106.00   0.50    0.50    --  111.00 -50.00-150.00   74
 22  \w     44.00 106.00   0.50    0.50    --  111.00 -25.00   0.00  124
 23  \w     46.00 130.00   0.50    0.50    --  111.00 -77.00-150.00  168
;
_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      -0.1071794000
_diffrn_orient_matrix_UB_12      0.0142390000
_diffrn_orient_matrix_UB_13      0.0124789000
_diffrn_orient_matrix_UB_21      0.0278973000
_diffrn_orient_matrix_UB_22      -0.0017529000
_diffrn_orient_matrix_UB_23      0.0746919000
_diffrn_orient_matrix_UB_31      0.0178801000
_diffrn_orient_matrix_UB_32      0.0870751000
_diffrn_orient_matrix_UB_33      -0.0005460000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.691
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58943
_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    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_preparation       'Staudinger with prolonged heating'
_exptl_crystal_recrystallization_method benzene
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.801
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         10592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+10.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10248
_reflns_number_total             10592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph17013
_cod_database_code               7703339
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H37 N4 O2 P2 Cl2 U1'
_chemical_oxdiff_usercomment     'mixed ligand; orange cube habit'
_reflns_odcompleteness_completeness 99.96
_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), C8(H8), 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), 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),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C61(H61),
 C62(H62), C63(H63), C71(H71), C72(H72), C73(H73)
;
_olex2_exptl_crystal_mounting_method 'MitiGen loop'
_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 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.787