N-Alkyl pyrrolidone ether podands as versatile alkali metal ion chelants.
Perrin, Andrea; Myers, Dominic; Fucke, Katharina; Musa, Osama M.; Steed, Jonathan W.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 3153–3161; doi:10.1039/c3dt53001a

data_7029092
_publ_section_title
;
 N-Alkyl pyrrolidone ether podands as versatile alkali metal ion chelants.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3153
_journal_page_last               3161
_journal_paper_doi               10.1039/c3dt53001a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '3(F6 P), C48 H80 N8 Na3 O12, 0.28(H2O)'
_chemical_formula_sum            'C48 H80.56 F18 N8 Na3 O12.28 P3'
_chemical_formula_weight         1470.16
_chemical_name_systematic
;
 ? 
;
_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_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_creation_date             2012-12-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                85.700(2)
_cell_angle_beta                 84.890(2)
_cell_angle_gamma                88.882(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2010(4)
_cell_length_b                   13.6768(4)
_cell_length_c                   18.1009(5)
_cell_measurement_reflns_used    12895
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.2198
_cell_measurement_theta_min      2.6150
_cell_volume                     3245.65(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -79.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000  -60.0000 90

  2 omega  -88.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000   90.0000 99

  3 omega  -73.00  -46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000  -30.0000 27

  4 omega   38.00   87.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616   57.0000  120.0000 49

  5 omega   36.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -125.0000   42.0000 31

  6 omega   18.00   70.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -125.0000 -120.0000 52

  7 omega  -49.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616  -57.0000 -150.0000 88

  8 omega  -50.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616  -57.0000  -30.0000 88

  9 omega  -87.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000  120.0000 90

 10 omega  -94.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000 -180.0000 60

 11 omega  -94.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000   30.0000 60

 12 omega  -90.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -38.0000 -180.0000 98

 13 omega   -3.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000   60.0000 64

 14 omega   -7.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616   38.0000   60.0000 98

 15 omega  -39.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000  150.0000 90

 16 omega  -39.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000  -90.0000 25

 17 omega   18.00   76.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -125.0000 -137.0000 58

 18 omega   -3.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000  -30.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0199504000
_diffrn_orient_matrix_UB_12      -0.0482653000
_diffrn_orient_matrix_UB_13      0.0055205000
_diffrn_orient_matrix_UB_21      0.0114799000
_diffrn_orient_matrix_UB_22      -0.0014418000
_diffrn_orient_matrix_UB_23      -0.0389400000
_diffrn_orient_matrix_UB_31      0.0487932000
_diffrn_orient_matrix_UB_32      0.0193303000
_diffrn_orient_matrix_UB_33      0.0030718000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76405
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1525
_exptl_crystal_size_max          0.7422
_exptl_crystal_size_mid          0.4462
_exptl_crystal_size_min          0.1434
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         14788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+2.0947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                10349
_reflns_number_total             14788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           12srv067
_cod_database_code               7029092
_chemical_oxdiff_formula         'C12 H20 N2 O3 Na P F6'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H6A,H6B} of C6, {H41,H3} of C41, {H22A,H22B} of C22, {H16A,H16B} of C16,
  {H23A,H23B} of C23, {H20A,H20B} of C20, {H29A,H29B} of C29, {H30A,H30B} of
  C30, {H15A,H15B} of C15, {H18A,H18B} of C18, {H44A,H44B} of C44, {H7A,H7B} of
  C7, {H27A,H27B} of C27, {H40A,H40B} of C40, {H47A,H47B} of C47, {H14A,H14B}
  of C14, {H2A,H2B} of C2, {H48A,H48B} of C48, {H4A,H4B} of C4, {H39A,H39B} of
  C39, {H43A,H43B} of C43, {H35A,H35B} of C35, {H38A,H38B} of C38, {H42A,H42B}
  of C42, {H46A,H46B} of C46, {H8A,H8B} of C8, {H34A,H34B} of C34, {H17A,H17B}
  of C17, {H28A,H28B} of C28, {H24A,H24B} of C24, {H31A,H31B} of C31, {H19A,
  H19B} of C19, {H36A,H36B} of C36, {H32,H2} of C32, {H5A,H5B} of C5, {H26A,
  H26B} of C26, {H11A,H11B} of C11, {H3A,H3B} of C3, {H12A,H12B} of C12, {H10A,
  H10B} of C10
2. Others
 Sof(F7A)=Sof(F9A)=Sof(F8A)=Sof(F10)=Sof(F11A)=Sof(F12A)=1-Sof(F9A)=1-Sof(F9A)=
 1-Sof(F9A)=1-Sof(F9A)=1-Sof(F9A)=1-Sof(F9A)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C41(H41,H3), C22(H22A,H22B), C16(H16A,H16B), C23(H23A,H23B),
 C20(H20A,H20B), C29(H29A,H29B), C30(H30A,H30B), C15(H15A,H15B), C26(H26A,H26B),
  C5(H5A,H5B), C32(H32,H2), C36(H36A,H36B), C19(H19A,H19B), C31(H31A,H31B),
 C24(H24A,H24B), C28(H28A,H28B), C17(H17A,H17B), C34(H34A,H34B), C8(H8A,H8B),
 C46(H46A,H46B), C42(H42A,H42B), C38(H38A,H38B), C35(H35A,H35B), C18(H18A,H18B),
  C44(H44A,H44B), C7(H7A,H7B), C27(H27A,H27B), C40(H40A,H40B), C47(H47A,H47B),
 C14(H14A,H14B), C2(H2A,H2B), C48(H48A,H48B), C4(H4A,H4B), C39(H39A,H39B),
 C43(H43A,H43B), C10(H10A,H10B), C12(H12A,H12B), C3(H3A,H3B), C11(H11A,H11B)
;