Simple access to ionic liquids and organic salts containing the phosphaethynolate (PCO(-)) and Zintl (Sb11(3-)) anions.
Jost, Maximilian; Finger, Lars H.; Sundermeyer, Jörg; von Hänisch, Carsten; Chemical communications (Cambridge, England) 52 (2016) 11646–11648; doi:10.1039/c6cc06620h

data_7125071
_publ_section_title
;
 Simple access to ionic liquids and organic salts containing the
 phosphaethynolate (PCO(-)) and Zintl (Sb11(3-)) anions.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11646
_journal_page_last               11648
_journal_paper_doi               10.1039/c6cc06620h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C2 H3 N, 2(C O P), 2(C7 H18 N3)'
_chemical_formula_sum            'C18 H39 N7 O2 P2'
_chemical_formula_weight         447.50
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.012(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8762(6)
_cell_length_b                   15.7545(8)
_cell_length_c                   13.6079(6)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.168
_cell_measurement_theta_min      2.553
_cell_volume                     2539.8(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            49655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.198
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1228 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.9421.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       needle
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0278P)^2^+0.7915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4619
_reflns_number_total             5654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06620h2.cif
_cod_data_source_block           compound5
_cod_database_code               7125071
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(N13)=Sof(N11)=Sof(N12)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(1)
 Sof(N4)=Sof(N5)=Sof(N6)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(N9)=Sof(N8)=Sof(N10)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(2)
 Sof(N1)=Sof(N3)=Sof(N2)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(H7C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(2)
3.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,
 H24B,H24C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C),
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C),
 C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              4307
_olex2_submission_special_instructions 'No special instructions were received'