Destruction of chemical warfare agent simulants by air and moisture stable metal NHC complexes.
Weetman, Catherine; Notman, Stuart; Arnold, Polly L.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2568–2574; doi:10.1039/c7dt04805j

data_7045483
_publ_section_title
;
 Destruction of chemical warfare agent simulants by air and moisture
 stable metal NHC complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2568
_journal_page_last               2574
_journal_paper_doi               10.1039/c7dt04805j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'Cl O2.5 P0.5 V0.5, Na'
_chemical_formula_sum            'Cl Na O2.5 P0.5 V0.5'
_chemical_formula_weight         139.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-10-17 deposited with the CCDC.
2018-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.318(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.3580(6)
_cell_length_b                   6.3903(6)
_cell_length_c                   15.2247(16)
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0940
_cell_measurement_theta_min      4.1390
_cell_volume                     715.85(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_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    -35.00  52.00   1.00   45.00    --  -16.31  57.00   0.00   87
  2  \w    -85.00   2.00   1.00   45.00    --  -16.31 -57.00-150.00   87
  3  \w    -25.00  24.00   1.00   45.00    --  -16.31 -99.00 120.00   49
  4  \w    -35.00  52.00   1.00   45.00    --  -16.31  57.00 120.00   87
  5  \w    -25.00  24.00   1.00   45.00    --  -16.31 -99.00-120.00   49
  6  \w    -25.00  59.00   1.00   45.00    --   18.03 -99.00  60.00   84
  7  \w    -35.00  52.00   1.00   45.00    --  -16.31  57.00-120.00   87
  8  \w    -85.00   2.00   1.00   45.00    --  -16.31 -57.00  90.00   87
  9  \w    -85.00   2.00   1.00   45.00    --  -16.31 -57.00 -30.00   87
 10  \w    -25.00  59.00   1.00   45.00    --   18.03 -99.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0877115000
_diffrn_orient_matrix_UB_12      0.0080071000
_diffrn_orient_matrix_UB_13      -0.0191828000
_diffrn_orient_matrix_UB_21      -0.0126744000
_diffrn_orient_matrix_UB_22      0.0981183000
_diffrn_orient_matrix_UB_23      0.0208833000
_diffrn_orient_matrix_UB_31      0.0378129000
_diffrn_orient_matrix_UB_32      0.0513470000
_diffrn_orient_matrix_UB_33      -0.0369601000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5177
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         3.068
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale green'
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.529
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0977
_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^)+(0.1246P)^2^+35.8176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                566
_reflns_number_total             675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04805j2.cif
_cod_data_source_block           p16148a_mono
_cod_depositor_comments          'Adding full bibliography for 7045483.cif.'
_cod_original_formula_sum        'Cl Na O2.50 P0.50 V0.50'
_cod_database_code               7045483
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C50 H50 V1 O3'
_chemical_oxdiff_usercomment     '@ 170 K Rm 564 F DMF/Et2O'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(P1)
Uanis(O3) = Uanis(O4)
;
_shelx_res_checksum              28503
_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 1.459
_oxdiff_exptl_absorpt_empirical_full_min 0.686