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_7703336
_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         'C6 H6 N4'
_chemical_formula_sum            'C6 H6 N4'
_chemical_formula_weight         134.15
_chemical_name_systematic        1,2-azidoaniline
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3467(3)
_cell_length_b                   13.1849(3)
_cell_length_c                   4.90129(8)
_cell_measurement_reflns_used    5759
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.2310
_cell_measurement_theta_min      3.9960
_cell_volume                     1314.87(4)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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    -60.00  28.00   0.50    0.50    --    4.52 -77.00 150.00  176
  2  \w      1.00  71.00   0.50    0.50    --    4.52  38.00 -90.00  140
  3  \w    101.00 170.00   0.50    0.50    --  105.46  45.00  30.00  138
  4  \w    101.00 170.00   0.50    0.50    --  105.46  45.00 -90.00  138
  5  \w     37.00 109.00   0.50    0.50    --  105.46 -94.00 -30.00  144
  6  \w     37.00 109.00   0.50    0.50    --  105.46 -94.00 120.00  144
  7  \w     94.00 171.00   0.50    0.50    --  105.46 125.00-150.00  154
  8  \w     82.00 170.00   0.50    0.50    --  105.46  77.00 150.00  176
  9  \w    -69.00  19.00   0.50    0.50    --   -4.52 -77.00 -30.00  176
 10  \w    -71.00  -1.00   0.50    0.50    --   -4.52 -38.00  60.00  140
 11  \w     92.00 168.00   0.50    0.50    --  105.46  61.00  90.00  152
 12  \w    102.00 145.00   0.50    0.50    --  105.46  30.00-150.00   86
 13  \w     97.00 174.00   0.50    0.50    --  105.46  15.00   0.00  154
;
_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      0.0060324000
_diffrn_orient_matrix_UB_12      -0.0458293000
_diffrn_orient_matrix_UB_13      -0.2880034000
_diffrn_orient_matrix_UB_21      -0.0753477000
_diffrn_orient_matrix_UB_22      0.0016617000
_diffrn_orient_matrix_UB_23      -0.0291607000
_diffrn_orient_matrix_UB_31      0.0037966000
_diffrn_orient_matrix_UB_32      0.1074945000
_diffrn_orient_matrix_UB_33      -0.1226314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6939
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.446
_diffrn_reflns_theta_min         3.995
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82133
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_preparation       'see SI'
_exptl_crystal_recrystallization_method 'see SI'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1371
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0510P)^2^+0.4525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1319
_reflns_number_total             1371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph16051
_cod_database_code               7703336
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 H6 N4 '
_chemical_oxdiff_usercomment     'long red needles '
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.834
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim N3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3.a Rotating group:
 N1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C6(H6), C5(H5)
;
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.832