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_7029097
_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         'C48 H84 F24 K4 N8 O14 P4'
_chemical_formula_sum            'C48 H84 F24 K4 N8 O14 P4'
_chemical_formula_weight         1733.51
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 120.757(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.4413(11)
_cell_length_b                   12.8337(3)
_cell_length_c                   23.8944(8)
_cell_measurement_reflns_used    14684
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.2487
_cell_measurement_theta_min      2.6810
_cell_volume                     7494.9(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_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  -52.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604   57.0000  120.0000 90

  2 omega -100.00   -3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000  -30.0000 97

  3 omega -114.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  179.0000 -180.0000 79

  4 omega  -35.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292  -57.0000 -180.0000 80

  5 omega   68.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292  179.0000  -90.0000 25

  6 omega   47.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292 -127.0000  147.0000 49

  7 omega  -18.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292    0.0000  -30.0000 89

  8 omega -105.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000   60.0000 103

  9 omega -105.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000 -150.0000 103

 10 omega -119.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  179.0000  -90.0000 87

 11 omega -107.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -77.0000  150.0000 112
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0128049000
_diffrn_orient_matrix_UB_12      -0.0044629000
_diffrn_orient_matrix_UB_13      0.0187484000
_diffrn_orient_matrix_UB_21      0.0256829000
_diffrn_orient_matrix_UB_22      0.0071095000
_diffrn_orient_matrix_UB_23      0.0289124000
_diffrn_orient_matrix_UB_31      -0.0043836000
_diffrn_orient_matrix_UB_32      0.0546146000
_diffrn_orient_matrix_UB_33      -0.0022143000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57703
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72909
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.941
_exptl_crystal_size_mid          0.6432
_exptl_crystal_size_min          0.3017
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+32.6055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                7330
_reflns_number_total             8606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           ap61_1
_cod_original_cell_volume        7494.9(4)
_cod_database_code               7029097
_chemical_oxdiff_formula         'C12 H20 N2 O3 K P F6'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H19A,H19B} of C19, {H20A,H20B} of C20, {H24A,H24B} of C24, {H22A,H22B} of
  C22, {H23A,H23B} of C23, {H2AA,H2AB} of C2A, {H3AA,H3AB} of C3A, {H4AA,H4AB}
  of C4A, {H10C,H10D} of C10A, {H11C,H11D} of C11A, {H12C,H12D} of C12A, {H14A,
  H14B} of C14, {H7A,H7B} of C7, {H1,H5} of C5, {H17A,H17B} of C17, {H15A,H15B}
  of C15, {H18A,H18B} of C18, {H10A,H10B} of C10B, {H16A,H16B} of C16, {H4BA,
  H4BB} of C4B, {H2BA,H2BB} of C2B, {H3BA,H3BB} of C3B, {H11A,H11B} of C11B,
  {H8A,H8B} of C8, {H12A,H12B} of C12B, {H6A,H6B} of C6
2. Others
 1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=
 1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=Sof(O1A)=Sof(C1A)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)
 1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-
 Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=Sof(O3A)=Sof(C9A)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=
 Sof(H12C)=Sof(H12D)
 Fixed Sof: O1S(0.5) O2S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C15(H15A,H15B), C17(H17A,H17B), C5(H1,H5), C7(H7A,H7B),
 C14(H14A,H14B), C10B(H10A,H10B), C16(H16A,H16B), C4B(H4BA,H4BB), C2B(H2BA,
 H2BB), C3B(H3BA,H3BB), C11B(H11A,H11B), C8(H8A,H8B), C12B(H12A,H12B), C6(H6A,
 H6B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,H24B), C22(H22A,H22B), C23(H23A,
 H23B), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C10A(H10C,H10D),
 C11A(H11C,H11D), C12A(H12C,H12D)
;