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_7706597
_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         'C2 Cl N2 O2 P'
_chemical_formula_sum            'C2 Cl N2 O2 P'
_chemical_formula_weight         150.46
_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             2020-01-07
_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                   7.2241(17)
_cell_length_b                   12.227(3)
_cell_length_c                   6.3593(10)
_cell_measurement_reflns_used    1660
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1363
_cell_measurement_theta_min      3.2688
_cell_volume                     561.7(2)
_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
;
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 0.994
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
  1 omega   -4.00   22.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000 -180.0000 104

  2 omega   -7.00   21.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000   60.0000 112

  3 omega  -11.00   64.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9787   77.0000 -150.0000 300

  4 omega  -41.00   49.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000   60.0000 360

  5 omega  -25.00   42.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000 -180.0000 268

  6 omega  -48.00  -27.00   0.2500   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5412   77.0000  -60.0000 84
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0792733000
_diffrn_orient_matrix_UB_12      -0.0335013000
_diffrn_orient_matrix_UB_13      0.0130654000
_diffrn_orient_matrix_UB_21      -0.0580040000
_diffrn_orient_matrix_UB_22      -0.0442050000
_diffrn_orient_matrix_UB_23      0.0294215000
_diffrn_orient_matrix_UB_31      -0.0061975000
_diffrn_orient_matrix_UB_32      -0.0162902000
_diffrn_orient_matrix_UB_33      -0.1069139000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2888
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.840
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.737
_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    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.4715
_exptl_crystal_size_mid          0.3683
_exptl_crystal_size_min          0.3333
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0549P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                599
_reflns_number_total             704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00261a2.cif
_cod_data_source_block           exp_2547
_cod_depositor_comments
'Adding full bibliography for 7706596--7706597.cif.'
_cod_database_code               7706597
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C2 N2 O2 P1 Cl1'
_chemical_oxdiff_usercomment     PCl(NCO)2
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63563
_shelx_hkl_checksum              6993
_olex2_submission_special_instructions 'No special instructions were received'