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_7703338
_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 N4 O2 P2 U'
_chemical_formula_sum            'C42 H32 Cl2 N4 O2 P2 U'
_chemical_formula_weight         995.58
_chemical_name_systematic        PN3PNUCl2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-11
_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            4
_cell_length_a                   20.8270(3)
_cell_length_b                   11.8420(2)
_cell_length_c                   15.7786(3)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100.3(8)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      2.16
_cell_volume                     3891.53(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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_temperature      100
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -50.00  25.00   0.50    2.33    --  -38.50  57.00-180.00  150
  2  \w   -105.00 -35.00   0.50    2.33    --  -38.50 -37.00  30.00  140
  3  \w    105.00 175.00   0.50    9.31    --  111.00  50.00-150.00  140
  4  \w     41.00 116.00   0.50    9.31    --  111.00-111.00  30.00  150
  5  \w    105.00 175.00   0.50    9.31    --  111.00  50.00 120.00  140
  6  \w     47.00 130.00   0.50    9.31    --  111.00 -72.00 128.00  166
  7  \w    108.00 178.00   0.50    9.31    --  111.00  37.00 150.00  140
  8  \w    105.00 175.00   0.50    9.31    --  111.00  50.00-120.00  140
  9  \w     26.00 114.00   0.50    2.33    --   49.06  77.00-150.00  176
 10  \w     38.00 112.00   0.50    2.33    --   49.06  55.00 117.00  148
 11  \w    101.00 178.00   0.50    9.31    --  111.00  12.00   0.00  154
 12  \w    107.00 149.00   0.50    9.31    --  111.00  25.00 -60.00   84
 13  \w     88.00 176.00   0.50    9.31    --  111.00  77.00  60.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20838
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        66.995
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_min         3.733
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    1.699
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_preparation       TD
_exptl_crystal_recrystallization_method benzene
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.762
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 2413 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.041(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6585
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0456P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.893
_reflns_Friedel_fraction_max     0.893
_reflns_number_gt                5991
_reflns_number_total             6585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04517a2.cif
_cod_data_source_block           ph17084b
_cod_database_code               7703338
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.333
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C13, C14, C15, C16, C17, C18
 with sigma of 0.1
 C9, C10, C11, C12, C7, C8
 with sigma of 0.1
 C23, C22, C21, C20, C19, C24
 with sigma of 0.1
 C26, C25, C30, C29, C28, C27
 with sigma of 0.1
 C37, C38, C39, C40, C41, C42
 with sigma of 0.1
 C31, C32, C33, C34, C35, C36
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C5(H5), C29(H29), C17(H17), C27(H27), C39(H39), C15(H15), C11(H11),
 C21(H21), C8(H8), C18(H18), C30(H30), C2(H2), C32(H32), C16(H16), C34(H34),
 C36(H36), C4(H4), C38(H38), C14(H14), C40(H40), C33(H33), C42(H42), C28(H28),
 C20(H20), C3(H3), C22(H22), C12(H12), C9(H9), C23(H23), C10(H10), C41(H41)
;
_olex2_exptl_crystal_mounting_method 'MiTiGen loop'
_olex2_submission_original_sample_id ph17084b
_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
;