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_7029088
_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_absolute_configuration unk
_chemical_formula_sum            'C36 H60 F12 N6 Na2 O6 P2'
_chemical_formula_weight         1008.82
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   23.9245(6)
_cell_length_b                   23.9245(6)
_cell_length_c                   13.3123(4)
_cell_measurement_reflns_used    4546
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.1580
_cell_measurement_theta_min      2.4862
_cell_volume                     6598.9(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -84.00    8.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -19.0000 -120.0000 92

  2 omega   14.00   57.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616  -92.0000  -48.0000 43

  3 omega  -89.00    5.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -48.0000  167.0000 94

  4 omega  -91.00   26.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -19.0000    0.0000 117

  5 omega  -39.00   51.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000    0.0000 90

  6 omega  -39.00   51.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000 -150.0000 90

  7 omega  -20.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616   92.0000 -116.0000 53

  8 omega   26.00   84.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000  176.0000 58

  9 omega  -94.00  -34.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000  -60.0000 60

 10 omega   26.00   51.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000   -3.0000 25

 11 omega   -3.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616   57.0000  150.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0244423000
_diffrn_orient_matrix_UB_12      0.0312347000
_diffrn_orient_matrix_UB_13      -0.0149925000
_diffrn_orient_matrix_UB_21      -0.0231437000
_diffrn_orient_matrix_UB_22      0.0040850000
_diffrn_orient_matrix_UB_23      -0.0273755000
_diffrn_orient_matrix_UB_31      -0.0061797000
_diffrn_orient_matrix_UB_32      0.0134315000
_diffrn_orient_matrix_UB_33      0.0431790000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.2215
_diffrn_reflns_av_unetI/netI     0.1204
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            104425
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.978
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.2116
_exptl_crystal_size_mid          0.1894
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         10093
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1770
_refine_ls_R_factor_gt           0.1126
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+26.0447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2853
_refine_ls_wR_factor_ref         0.3214
_reflns_number_gt                5779
_reflns_number_total             10093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           vpd_napf6
_cod_depositor_comments
;

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C18 H30 F6 N3 Na O3 P'
_cod_original_formula_weight         504.41
_cod_original_formula_moiety         '0.25(C72 H120 N12 Na4 O12), F6 P'
_cod_original_formula_units_Z            12
_cod_database_code               7029088
_chemical_oxdiff_formula         'C12 H20 N2 O2 Na P F6'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H23A,H23B} of C23, {H26A,H26B} of C26, {H35A,H35B} of C35, {H24A,H24B} of
  C24, {H19A,H19B} of C19, {H15A,H15B} of C15, {H20A,H20B} of C20, {H22A,H22B}
  of C22, {H14A,H14B} of C14, H17 of C17, {H16A,H16B} of C16, {H11A,H11B} of
  C11, {H2A,H2B} of C2, {H10A,H10B} of C10, {H8A,H8B} of C8, {H7A,H7B} of C7,
  {H3A,H3B} of C3, {H12A,H12B} of C12, {H4A,H4B} of C4, H5 of C5, {H28A,H28B}
  of C28, {H36A,H36B} of C36, {H31A,H31B} of C31, {H27A,H27B} of C27, {H32A,
  H32B} of C32, {H34A,H34B} of C34, H29 of C29
 At 1.5 times of:
  {H18A,H18B,H18C} of C18, {H6A,H6B,H6C} of C6, {H30A,H30B,H30C} of C30
2. Uiso/Uaniso restraints and constraints
Uanis(C1) ~ Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C21) = Uanis(O4)
3.a Ternary CH refined with riding coordinates:
 C29(H29), C5(H5), C17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C26(H26A,H26B), C34(H34A,H34B), C32(H32A,H32B), C27(H27A,
 H27B), C31(H31A,H31B), C36(H36A,H36B), C28(H28A,H28B), C4(H4A,H4B), C12(H12A,
 H12B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C2(H2A,H2B),
 C11(H11A,H11B), C16(H16A,H16B), C14(H14A,H14B), C22(H22A,H22B), C20(H20A,H20B),
  C15(H15A,H15B), C19(H19A,H19B), C24(H24A,H24B), C23(H23A,H23B)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C6(H6A,H6B,H6C), C18(H18A,H18B,H18C)
;