Dichlorophosphanyl isocyanate - spectroscopy, conformation and molecular structure in the gas phase and the solid state.
Li, Dingqing; Schwabedissen, Jan; Stammler, Hans-Georg; Mitzel, Norbert W.; Willner, Helge; Zeng, Xiaoqing; Physical chemistry chemical physics : PCCP 18 (2016) 26245–26253; doi:10.1039/c6cp05377g

data_7226478
_publ_section_title
;
 Dichlorophosphanyl isocyanate - spectroscopy, conformation and molecular
 structure in the gas phase and the solid state.
;
_journal_issue                   37
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              26245
_journal_page_last               26253
_journal_paper_doi               10.1039/c6cp05377g
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C Cl2 N O P'
_chemical_formula_sum            'C Cl2 N O P'
_chemical_formula_weight         143.89
_chemical_melting_point          187
_chemical_name_common            'Dichlorophosphanyl Isocyanate'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-01-16
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-07-05 deposited with the CCDC.
2016-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.196(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8078(6)
_cell_length_b                   6.1587(3)
_cell_length_c                   7.7148(4)
_cell_measurement_reflns_used    13749
_cell_measurement_temperature    95.0(8)
_cell_measurement_theta_max      31.8730
_cell_measurement_theta_min      1.9360
_cell_volume                     497.83(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      95.0(8)
_diffrn_detector_area_resol_mean 8.0951
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9678
_diffrn_measurement_details
;
  1 omega  -46.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295    0.0000  150.0000 141

  2 omega  -30.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -38.0000  -60.0000 76

  3 omega    3.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -99.0000  150.0000 63

  4 omega   -3.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   77.0000  150.0000 96

  5 omega   -2.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   77.0000  -30.0000 96

  6 omega   28.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295 -125.0000  -52.0000 49

  7 omega    7.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   57.0000  -90.0000 45

  8 omega    8.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   57.0000   90.0000 47

  9 omega   26.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -99.0000   30.0000 38

 10 omega  -40.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295    0.0000    0.0000 112

 11 omega  -92.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000 -120.0000 87

 12 omega  -92.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000  -57.0000  -30.0000 87

 13 omega    7.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   57.0000   90.0000 86

 14 omega  -20.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -99.0000   30.0000 86

 15 omega   34.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295 -178.0000  -30.0000 66

 16 omega    7.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   57.0000 -180.0000 86

 17 omega   35.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  178.0000 -120.0000 64

 18 omega  -46.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -38.0000   60.0000 93

 19 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -180.0000 143

 20 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -150.0000 143

 21 omega  -95.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000 -120.0000 143

 22 omega    3.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   38.0000    0.0000 93

 23 omega  -46.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -38.0000  -30.0000 93

 24 omega  -20.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295  -99.0000 -180.0000 86

 25 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295   77.0000 -150.0000 98

 26 omega   34.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0295 -178.0000    0.0000 66

 27 omega  -95.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000    0.0000  -90.0000 110
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0656692000
_diffrn_orient_matrix_UB_12      0.0270018000
_diffrn_orient_matrix_UB_13      -0.0286532000
_diffrn_orient_matrix_UB_21      0.0155715000
_diffrn_orient_matrix_UB_22      0.1118191000
_diffrn_orient_matrix_UB_23      0.0112467000
_diffrn_orient_matrix_UB_31      0.0053773000
_diffrn_orient_matrix_UB_32      0.0054721000
_diffrn_orient_matrix_UB_33      -0.0896955000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27194
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       needle
_exptl_crystal_F_000             280
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0279P)^2^+0.6353P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1347
_reflns_number_total             1457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cp05377g2.cif
_cod_data_source_block           jasc01_1_95_00
_cod_depositor_comments          'Adding full bibliography for 7226478.cif.'
_cod_database_code               7226478
_chemical_oxdiff_formula         'C Cl2 N O P'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_res_checksum              33527
_shelxl_version_number           2013-2