Synthesis and reactivity of α-cationic phosphines: the effect of imidazolinium and amidinium substituents.
Haldón, Estela; Kozma, Ágnes; Tinnermann, Hendrik; Gu, Lianghu; Goddard, Richard; Alcarazo, Manuel; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1872–1876; doi:10.1039/c5dt02341f

data_7035815
_publ_section_title
;
 Synthesis and reactivity of \a-cationic phosphines: the effect of
 imidazolinium and amidinium substituents.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1872
_journal_page_last               1876
_journal_paper_doi               10.1039/c5dt02341f
_journal_volume                  45
_journal_year                    2016
_chemical_compound_source        dichloromethane
_chemical_formula_moiety         'C17 H32 N2 P, F6 Sb'
_chemical_formula_sum            'C17 H32 F6 N2 P Sb'
_chemical_formula_weight         531.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                HAI-HA-114-01
_audit_creation_date             2014-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                75.926(3)
_cell_angle_beta                 82.983(3)
_cell_angle_gamma                74.157(3)
_cell_formula_units_Z            6
_cell_length_a                   15.028(3)
_cell_length_b                   15.072(3)
_cell_length_c                   15.430(3)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.4371
_cell_measurement_theta_min      2.5136
_cell_volume                     3255.4(11)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (G. M. Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            79160
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.512
_diffrn_reflns_theta_min         1.363
_diffrn_source                   1\mS
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.400
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         16429
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+3.9758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11965
_reflns_number_total             16429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02341f2.cif
_cod_data_source_block           8725sadabs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035812--7035820.cif.
;
_cod_original_cell_volume        3255.4(10)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7035815
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F15C-F17C \\sim F15C-F16C \\sim F15C-F14C \\sim F16A-F15A \\sim F16A-F14A
\\sim F16A-F18A \\sim F13B-
 F15B \\sim F13B-F16B \\sim F13B-F14B \\sim F15B-F16B \\sim F15B-F14B \\sim
F17C-F16C \\sim F17C-F14C ~
 F15A-F14A \\sim F14A-F18A
 with sigma of 0.02
 Sb3-F15C \\sim Sb3-F16A \\sim Sb3-F13B \\sim Sb3-F15B \\sim Sb3-F17C \\sim
Sb3-F16C \\sim Sb3-F16B ~
 Sb3-F15A \\sim Sb3-F14A \\sim Sb3-F18A \\sim Sb3-F14C \\sim Sb3-F14B
 with sigma of 0.01
3. Others
 Fixed Sof: F13C(0.25) F14C(0.25) F15C(0.25) F16C(0.25) F17C(0.25) F18C(0.25)
 F16A(0.5) F15A(0.5) F14B(0.25) F17A(0.5) F15B(0.25) F18A(0.5) F16B(0.25)
 F13A(0.5) F17B(0.25) F13B(0.25) F14A(0.5) F18B(0.25)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C26(H26), C32(H32), C46(H46), C52(H52)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C42(H42A,H42B), C43(H43A,H43B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
  C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              96040