Diverse Reactivity of the cyclo-Diphosphinophosphonium Cation [(PtBu)3Me](+): Parallels with Epoxides and New catena-Phosphorus Frameworks.
Robertson, Alasdair P. M.; Dyker, C. Adam; Gray, Paul A.; Patrick, Brian O.; Decken, Andreas; Burford, Neil; Journal of the American Chemical Society 136 (2014) 14941–14950; doi:10.1021/ja507741s

data_4122801
_publ_section_title
;
 Diverse Reactivity of the cyclo-Diphosphinophosphonium Cation
 [(PtBu)3Me](+): Parallels with Epoxides and New catena-Phosphorus
 Frameworks.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14941
_journal_page_last               14950
_journal_paper_doi               10.1021/ja507741s
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C20 H40 N2 P3, C F3 O3 S'
_chemical_formula_sum            'C21 H40 F3 N2 O3 P3 S'
_chemical_formula_weight         550.52
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-16
_audit_creation_method
; 
Olex2 1.2 
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90.185(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.884(12)
_cell_length_b                   10.814(7)
_cell_length_c                   27.811(18)
_cell_measurement_reflns_used    9139
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.62
_cell_volume                     5679(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.001
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            35443
_diffrn_reflns_point_group_measured_fraction_full 1.001
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0527 before and 0.0391 after correction. 
The Ratio of minimum to maximum transmission is 0.9051. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       blade
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         13898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+2.7283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12855
_reflns_number_total             13898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja507741s_si_002.cif
_cod_data_source_block           nb001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4122801--4122802.cif.
;
_cod_original_cell_volume        5680(6)
_cod_database_code               4122801
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.848
_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.a Me refined with riding coordinates: 
 C6(H6A,H6B,H6C) 
2.b Aromatic/amide H refined with riding coordinates: 
 C1(H1), C2(H2), C4(H4), C5(H5), C22(H22), C23(H23), C25(H25), C26(H26) 
2.c Idealised Me refined as rotating group: 
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), 
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B, 
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A, 
 H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), 
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B, 
 H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A, 
 H41B,H41C) 
;
_shelx_res_checksum              45486
_shelx_hkl_checksum              57172
_olex2_submission_special_instructions 'No special instructions were received'