Synthesis of Selected Cationic Pnictanes [LnPnX3-n](n+) (L = Imidazolium-2-yl; Pn = P, As; n = 1-3) and Replacement Reactions with Pseudohalogens.
Henne, F. D.; Dickschat, A. T.; Hennersdorf, F.; Feldmann, K.-O.; Weigand, J. J.; Inorganic chemistry 54 (2015) 6849–6861; doi:10.1021/acs.inorgchem.5b00765

data_4343579
_publ_section_title
;
 Synthesis of Selected Cationic Pnictanes [LnPnX3-n](n+) (L =
 Imidazolium-2-yl; Pn = P, As; n = 1-3) and Replacement Reactions with
 Pseudohalogens.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6849
_journal_page_last               6861
_journal_paper_doi               10.1021/acs.inorgchem.5b00765
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C28 H34 Cl2 F3 N8 O3 P S'
_chemical_formula_sum            'C28 H34 Cl2 F3 N8 O3 P S'
_chemical_formula_weight         721.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-02
_audit_creation_method
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Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
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_cell_angle_alpha                90
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_cell_length_b                   18.0557(8)
_cell_length_c                   16.0631(7)
_cell_measurement_reflns_used    12211
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.2710
_cell_measurement_theta_min      2.5900
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:01:44)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
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  1 omega  -95.55    9.15   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6903  -73.7594  145.7463 349

  2 omega  -49.07   19.93   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6903   88.7887  -92.1850 230

  3 omega  -95.55    9.45   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6903  -73.7594   25.7463 350

  4 phi     -9.83  349.87   0.3000   19.9990
omega____ theta____ kappa____ phi______ frames
  63.2669  -16.6903   30.1700     -     1199

  5 phi     27.14  141.74   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
  11.8813  -16.6903  -77.1462     -     382
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_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      0.0268673000
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_diffrn_orient_matrix_UB_13      -0.0227052000
_diffrn_orient_matrix_UB_21      -0.0308054000
_diffrn_orient_matrix_UB_22      0.0146991000
_diffrn_orient_matrix_UB_23      -0.0388715000
_diffrn_orient_matrix_UB_31      0.0460744000
_diffrn_orient_matrix_UB_32      0.0252368000
_diffrn_orient_matrix_UB_33      -0.0009722000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66447
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.395
_diffrn_reflns_theta_max         25.395
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33t (release 27-03-2014 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.527
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         15649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.1178
_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^)+(0.1427P)^2^+28.9438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2994
_refine_ls_wR_factor_ref         0.3122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14094
_reflns_number_total             15649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00765_si_013.cif
_cod_data_source_block
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_cod_depositor_comments
'Adding full bibliography for 4343576--4343580.cif.'
_cod_database_code               4343579
_chemical_oxdiff_formula         C28H34Cl2F3N8O3PS
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.640(3) 0.360(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C10(H10), C25(H25), C13(H13), C22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C6(H6), C20(H20), C19(H19), C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C14(H14A,H14B,
 H14C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              88492
_shelx_hkl_checksum              21098
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'