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_4343577
_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         'C27 H34 Cl4 N2 P, C F3 O3 S'
_chemical_formula_sum            'C28 H34 Cl4 F3 N2 O3 P S'
_chemical_formula_weight         708.40
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.840(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1467(4)
_cell_length_b                   19.2370(5)
_cell_length_c                   14.2131(4)
_cell_measurement_reflns_used    5729
_cell_measurement_temperature    153
_cell_measurement_theta_max      68.299
_cell_measurement_theta_min      3.890
_cell_volume                     3290.08(17)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18850
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.389
_diffrn_reflns_theta_min         3.890
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.754
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0750 after correction.
The Ratio of minimum to maximum transmission is 0.5726.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1230P)^2^+2.1679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4851
_reflns_number_total             5921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00765_si_002.cif
_cod_data_source_block           jjw0290
_cod_depositor_comments
'Adding full bibliography for 4343576--4343580.cif.'
_cod_database_code               4343577
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.200
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B)
Uanis(S1A) = Uanis(S1B)
3. Others
 Sof(S1B)=Sof(O3B)=Sof(O2B)=1-FVAR(1)
 Sof(O2A)=Sof(O3A)=Sof(S1A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              41411
_shelx_hkl_checksum              12958
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 20.07.2011
_olex2_date_sample_submission    20.07.2011
_olex2_submission_original_sample_id jjw0290
_olex2_submission_special_instructions 'No special instructions were received'