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_7703337
_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 H4 N6'
_chemical_formula_sum            'C6 H4 N6'
_chemical_formula_weight         160.15
_chemical_name_systematic        1,2-diazidobenzene
_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   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                90
_cell_angle_beta                 95.700(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7390(4)
_cell_length_b                   20.3245(11)
_cell_length_c                   5.2307(3)
_cell_measurement_reflns_used    3724
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.5150
_cell_measurement_theta_min      4.3150
_cell_volume                     712.89(7)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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    -44.00  31.00   0.50    2.20    --  -38.50  19.00  90.00  150
  2  \w    -50.00  25.00   0.50    2.20    --  -38.50  57.00-180.00  150
  3  \w     46.00 116.00   0.50    2.20    --   49.97  38.00-120.00  140
  4  \w     46.00 116.00   0.50    2.20    --   49.97  38.00 -60.00  140
  5  \w     23.00 101.00   0.50    2.20    --   49.97-125.00   0.00  156
  6  \w     42.00 109.00   0.50    8.81    --  111.00 -94.00-120.00  134
  7  \w     41.00 116.00   0.50    8.81    --  111.00-111.00  90.00  150
  8  \w    103.00 178.00   0.50    8.81    --  111.00  15.00   0.00  150
  9  \w     43.00 115.00   0.50    8.81    --  111.00 -30.00  60.00  144
 10  \w     46.00 116.00   0.50    8.81    --  111.00 -45.00   0.00  140
 11  \w     42.00 109.00   0.50    8.81    --  111.00 -94.00 -90.00  134
 12  \w     48.00 124.00   0.50    8.81    --  111.00 -61.00-150.00  152
 13  \w    107.00 178.00   0.50    8.81    --  111.00  30.00  30.00  142
 14  \w     42.00 109.00   0.50    8.81    --  111.00 -94.00   0.00  134
 15  \w     43.00 115.00   0.50    8.81    --  111.00 -30.00-120.00  144
 16  \w     41.00 116.00   0.50    8.81    --  111.00-111.00 -30.00  150
 17  \w     42.00 119.00   0.50    8.81    --  111.00 -15.00-180.00  154
 18  \w     48.00 124.00   0.50    8.81    --  111.00 -61.00 -60.00  152
 19  \w     27.00 115.00   0.50    2.20    --   49.97  77.00 120.00  176
 20  \w     27.00 115.00   0.50    2.20    --   49.97  77.00 -60.00  176
 21  \w     38.00 113.00   0.50    2.20    --   49.97  57.00-180.00  150
 22  \w     27.00 115.00   0.50    2.20    --   49.97  77.00  30.00  176
 23  \w    107.00 132.00   0.50    8.81    --  111.00  30.00 150.00   50
 24  \w    103.00 178.00   0.50    8.81    --  111.00  15.00-120.00  150
;
_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      0.0764465000
_diffrn_orient_matrix_UB_12      -0.0560379000
_diffrn_orient_matrix_UB_13      -0.1627978000
_diffrn_orient_matrix_UB_21      0.0301423000
_diffrn_orient_matrix_UB_22      0.0493424000
_diffrn_orient_matrix_UB_23      -0.2163203000
_diffrn_orient_matrix_UB_31      0.2144624000
_diffrn_orient_matrix_UB_32      0.0130892000
_diffrn_orient_matrix_UB_33      0.1197851000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7702
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.300
_diffrn_reflns_theta_min         6.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22542
_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    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_preparation       'diazotization of 1,2-azidoaniline'
_exptl_crystal_recrystallization_method 'from melt'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1010P)^2^+0.1190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1537
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1296
_reflns_number_total             1543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph17008a
_cod_original_cell_volume        712.88(7)
_cod_database_code               7703337
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 H4 N6'
_reflns_odcompleteness_completeness 99.68
_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:
 C3(H3), C4(H4), C5(H5), C6(H6)
;
_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 2.900
_oxdiff_exptl_absorpt_empirical_full_min 0.375