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_7125073
_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         '3(C13 H30 P), Sb11'
_chemical_formula_sum            'C39 H90 P3 Sb11'
_chemical_formula_weight         1991.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-18 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.210(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.443(2)
_cell_length_b                   11.2133(7)
_cell_length_c                   21.6617(11)
_cell_measurement_reflns_used    8794
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      1.49
_cell_volume                     6390.0(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       rotational
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1463
_diffrn_reflns_av_unetI/netI     0.1957
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29052
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.827
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    4.667
_exptl_absorpt_correction_T_max  0.8823
_exptl_absorpt_correction_T_min  0.5248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.13(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.719
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         12094
_refine_ls_number_restraints     386
_refine_ls_restrained_S_all      0.713
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.800
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                5394
_reflns_number_total             12094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06620h2.cif
_cod_data_source_block           mj47
_cod_original_cell_volume        6390.1(7)
_cod_database_code               7125073
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.504
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C13
 1.55 with sigma of 0.02
 C4-C5
 1.55 with sigma of 0.02
 C4-C5A
 1.55 with sigma of 0.02
 C8-C9
 1.55 with sigma of 0.02
 C8-C9A
 1.55 with sigma of 0.02
 C19-C20
 1.55 with sigma of 0.02
 C21-C22
 1.55 with sigma of 0.02
 C20-C21
 1.55 with sigma of 0.02
 C38-C39
 1.55 with sigma of 0.02
 C7-C9A
 2.6 with sigma of 0.04
3. Rigid bond restraints
 P1, C1, C2, C3, C4, C5, C5A, C6, C7, C8, C9, C9A, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P2, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P3, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C5A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 P1, C1, C2, C3, C4, C5, C5A, C6, C7, C8, C9, C9A, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P3, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C6, C7, C8, C9} sigma for 1-2: 0.02, 1-3: 0.04
as
{C10, C11, C12, C13}
{C15, C16, C17, C18} sigma for 1-2: 0.02, 1-3: 0.04
as
{C19, C20, C21, C22}
7. Others
 Fixed Sof: H4AA(0.7) H4AB(0.7) H4BC(0.3) H4BD(0.3) C5(0.7) H5A(0.7) H5B(0.7)
 H5C(0.7) C5A(0.3) H5AA(0.3) H5AB(0.3) H5AC(0.3) H8AA(0.7) H8AB(0.7) H8BC(0.3)
 H8BD(0.3) C9(0.7) H9A(0.7) H9B(0.7) H9C(0.7) C9A(0.3) H9AA(0.3) H9AB(0.3)
 H9AC(0.3)
8.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4AA,H4AB), C4(H4BC,H4BD), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8AA,H8AB), C8(H8BC,H8BD), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,
 H12B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
8.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C9(H9A,H9B,H9C),
 C9A(H9AA,H9AB,H9AC), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,
 H31B,H31C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              55114
_olex2_submission_special_instructions 'No special instructions were received'