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_7029098
_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         1733.49
_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             2013-02-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.458(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   41.2572(13)
_cell_length_b                   12.8318(4)
_cell_length_c                   45.5789(17)
_cell_measurement_reflns_used    5277
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.4084
_cell_measurement_theta_min      2.5519
_cell_volume                     22457.1(14)
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_details
;
  1 omega    2.00   34.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065   38.0000  -30.0000 43

  2 omega  -33.00   47.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065   38.0000  120.0000 107

  3 omega  -67.00   29.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065   95.0000   -3.0000 128

  4 omega   60.00  113.25   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7190  179.0000 -150.0000 71

  5 omega -100.00    5.75   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065  -57.0000    0.0000 141

  6 omega -115.00  -34.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065 -179.0000  120.0000 108

  7 omega -100.00    5.75   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.4065  -57.0000 -180.0000 141

  8 omega   -7.00   86.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7190   57.0000  -30.0000 124

  9 omega  -23.00   28.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7190   95.0000  176.0000 68
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0165522000
_diffrn_orient_matrix_UB_12      -0.0224892000
_diffrn_orient_matrix_UB_13      0.0082463000
_diffrn_orient_matrix_UB_21      0.0048257000
_diffrn_orient_matrix_UB_22      0.0088358000
_diffrn_orient_matrix_UB_23      -0.0132251000
_diffrn_orient_matrix_UB_31      0.0066268000
_diffrn_orient_matrix_UB_32      0.0496900000
_diffrn_orient_matrix_UB_33      0.0060746000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.2077
_diffrn_reflns_av_unetI/netI     0.1902
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            118863
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.63
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.853
_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)
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    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10704
_exptl_crystal_size_max          0.6726
_exptl_crystal_size_mid          0.1765
_exptl_crystal_size_min          0.0362
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1387
_refine_ls_number_reflns         25414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.2262
_refine_ls_R_factor_gt           0.0973
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2819
_reflns_number_gt                10209
_reflns_number_total             25414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           bishep_kpf6_meoh
_cod_original_cell_volume        22457.2(13)
_cod_database_code               7029098
_chemical_oxdiff_formula         'C12 H20 N2 O3 K P F6'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H6A,H6B} of C6, {H8A,H8B} of C8, {H21A,H21B} of C21, {H5A,H5B} of C5, {H2C,
  H2D} of C2, {H50A,H50B} of C50, {H56A,H56B} of C56, {H66A,H66B} of C66, {H64A,
  H64B} of C64, {H52A,H52B} of C52, {H16A,H16B} of C16, {H26A,H26B} of C26,
  {H38A,H38B} of C38, {H20,H2B} of C20, {H34A,H34B} of C34, {H29A,H29B} of C29,
  {H47A,H47B} of C47, {H57A,H57B} of C57, {H65A,H65B} of C65, {H6,H68} of C68,
  {H31A,H31B} of C31, {H53A,H53B} of C53, {H9A,H9B} of C9, {H51A,H51B} of C51,
  {H40A,H40B} of C40, {H45A,H45B} of C45, {H54A,H54B} of C54, {H55A,H55B} of
  C55, {H27A,H27B} of C27, {H23A,H23B} of C23, {H4,H41} of C41, {H22A,H22B} of
  C22, {H43A,H43B} of C43, {H15A,H15B} of C15, {H4A,H4B} of C4, {H18A,H18B} of
  C18, {H14A,H14B} of C14, {H19A,H19B} of C19, {H62A,H62B} of C62, {H7A,H7B} of
  C7, {H32A,H32B} of C32, {H33A,H33B} of C33, {H44A,H44B} of C44, {H42A,H42B}
  of C42, {H35A,H35B} of C35, {H11A,H11B} of C11, {H2A,H17} of C17, {H63A,H63B}
  of C63, {H46A,H46B} of C46, {H59A,H59B} of C59, {H10A,H10B} of C10, {H30A,
  H30B} of C30, {H67A,H67B} of C67, {H3A,H3B} of C3, {H71A,H71B} of C71, {H28A,
  H28B} of C28, {H39A,H39B} of C39, {H70A,H70B} of C70, {H69A,H69B} of C69,
  {H58A,H58B} of C58
2. Others
 Fixed Sof: O3S(0.5) O4S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C21(H21A,H21B), C5(H5A,H5B), C2(H2C,H2D), C23(H23A,
 H23B), C41(H4,H41), C22(H22A,H22B), C43(H43A,H43B), C15(H15A,H15B), C4(H4A,
 H4B), C18(H18A,H18B), C14(H14A,H14B), C19(H19A,H19B), C62(H62A,H62B), C7(H7A,
 H7B), C32(H32A,H32B), C33(H33A,H33B), C44(H44A,H44B), C42(H42A,H42B), C35(H35A,
 H35B), C11(H11A,H11B), C17(H2A,H17), C63(H63A,H63B), C46(H46A,H46B), C59(H59A,
 H59B), C10(H10A,H10B), C30(H30A,H30B), C67(H67A,H67B), C3(H3A,H3B), C50(H50A,
 H50B), C56(H56A,H56B), C66(H66A,H66B), C64(H64A,H64B), C52(H52A,H52B),
 C16(H16A,H16B), C26(H26A,H26B), C38(H38A,H38B), C20(H20,H2B), C34(H34A,H34B),
 C29(H29A,H29B), C47(H47A,H47B), C57(H57A,H57B), C65(H65A,H65B), C68(H6,H68),
 C31(H31A,H31B), C53(H53A,H53B), C9(H9A,H9B), C51(H51A,H51B), C40(H40A,H40B),
 C45(H45A,H45B), C54(H54A,H54B), C55(H55A,H55B), C27(H27A,H27B), C58(H58A,H58B),
  C69(H69A,H69B), C70(H70A,H70B), C39(H39A,H39B), C28(H28A,H28B), C71(H71A,H71B)
;