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_7029093
_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         'C26 H48 F12 N4 Na2 O8 P2'
_chemical_formula_sum            'C26 H48 F12 N4 Na2 O8 P2'
_chemical_formula_weight         880.60
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.547(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1886(5)
_cell_length_b                   13.3508(5)
_cell_length_c                   13.6275(6)
_cell_measurement_reflns_used    2442
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.9219
_cell_measurement_theta_min      2.5306
_cell_volume                     1893.37(15)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -84.00  -11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000  -60.0000 73

  2 omega  -46.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000 -150.0000 42

  3 omega  -81.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000 -180.0000 67

  4 omega   11.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000 -180.0000 47

  5 omega  -87.00  -50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000   30.0000 37

  6 omega  -39.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000  -30.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0531317000
_diffrn_orient_matrix_UB_12      0.0052672000
_diffrn_orient_matrix_UB_13      0.0161661000
_diffrn_orient_matrix_UB_21      -0.0424719000
_diffrn_orient_matrix_UB_22      -0.0119804000
_diffrn_orient_matrix_UB_23      -0.0518120000
_diffrn_orient_matrix_UB_31      0.0044562000
_diffrn_orient_matrix_UB_32      -0.0514760000
_diffrn_orient_matrix_UB_33      0.0136913000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13061
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.987
_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    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2888
_exptl_crystal_size_mid          0.1892
_exptl_crystal_size_min          0.0992
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0441P)^2^+2.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                2880
_reflns_number_total             4262
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           bishep_napf6_dmp
_cod_original_cell_volume        1893.37(14)
_cod_database_code               7029093
_chemical_oxdiff_formula         'C12 H20 N2 O3 Na 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:
  {H3A,H3B} of C3, {H5A,H5B} of C5, {H6A,H6B} of C6, {H4A,H4B} of C4, {H7A,
  H7B} of C7, {H8A,H8B} of C8, {H11A,H11B} of C11, {H10A,H10B} of C10, {H12A,
  H12B} of C12, {H2A,H2B} of C2
 At 1.5 times of:
  H4 of O4, {H13A,H13B,H13C} of C13
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 C13-H4
 1.896724 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B), C3(H3A,H3B), C2(H2A,H2B),
 C8(H8A,H8B), C11(H11A,H11B), C10(H10A,H10B), C12(H12A,H12B)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;