Synthesis and characterization of phosphorous(III) diisocyanate and triisocyanate.
Hu, Dandan; Lu, Bo; Song, Chao; Zhu, Bifeng; Wang, Lina; Bernhardt, Eduard; Zeng, Xiaoqing; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3299–3307; doi:10.1039/d1dt00261a

data_7706596
_publ_section_title
;
 Synthesis and characterization of phosphorous(III) diisocyanate and
 triisocyanate.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3299
_journal_page_last               3307
_journal_paper_doi               10.1039/d1dt00261a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C3 N3 O3 P'
_chemical_formula_sum            'C3 N3 O3 P'
_chemical_formula_weight         157.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-09
_audit_creation_method
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Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-01-14 deposited with the CCDC.	2021-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2574(4)
_cell_length_b                   11.2605(6)
_cell_length_c                   7.1530(4)
_cell_measurement_reflns_used    3606
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.6692
_cell_measurement_theta_min      3.3328
_cell_volume                     584.56(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.2705
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
  1 omega   25.00   67.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000  -90.0000 168

  2 omega   22.00   68.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000   30.0000 184

  3 omega    7.00   66.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -       26.2288  -99.0000  150.0000 236

  4 omega  -82.00  -54.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913 -178.0000    0.0000 112

  5 omega  -34.00   34.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913   57.0000   60.0000 272

  6 omega  -97.00   -6.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913  -57.0000 -180.0000 364

  7 omega -101.00   16.00   0.2500    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7913  -19.0000 -120.0000 468
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0724617000
_diffrn_orient_matrix_UB_12      0.0398548000
_diffrn_orient_matrix_UB_13      -0.0224646000
_diffrn_orient_matrix_UB_21      -0.0419810000
_diffrn_orient_matrix_UB_22      0.0116885000
_diffrn_orient_matrix_UB_23      -0.0875806000
_diffrn_orient_matrix_UB_31      -0.0504103000
_diffrn_orient_matrix_UB_32      0.0474136000
_diffrn_orient_matrix_UB_33      0.0405213000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5868
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.746
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.411
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.5673
_exptl_crystal_size_mid          0.4878
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0351P)^2^+0.1721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                981
_reflns_number_total             1050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00261a2.cif
_cod_data_source_block           exp_2516
_cod_depositor_comments
'Adding full bibliography for 7706596--7706597.cif.'
_cod_database_code               7706596
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C3 N3 O3 P1'
_chemical_oxdiff_usercomment     'P(NCO)3 100K'
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.800
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              35400
_shelx_hkl_checksum              24253
_olex2_submission_special_instructions 'No special instructions were received'