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_7029095
_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 H80 N8 Na2 O12, 2(C24 H20 B)'
_chemical_formula_sum            'C96 H120 B2 N8 Na2 O12'
_chemical_formula_weight         1645.60
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-08
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                71.514(5)
_cell_angle_beta                 79.756(4)
_cell_angle_gamma                66.772(5)
_cell_formula_units_Z            1
_cell_length_a                   11.5127(6)
_cell_length_b                   13.7549(9)
_cell_length_c                   15.9209(7)
_cell_measurement_reflns_used    6602
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6616
_cell_measurement_theta_min      2.6974
_cell_volume                     2193.2(2)
_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
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_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  -92.00  -17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000   90.0000 75

  2 omega  -95.00  -64.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000   60.0000 31

  3 omega  -48.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429   57.0000 -150.0000 90

  4 omega  -78.00  -32.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  179.0000 -180.0000 46

  5 omega   30.00   63.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000   30.0000 33

  6 omega   43.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000   60.0000 26

  7 omega    6.00   32.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000   60.0000 26

  8 omega   33.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000  -90.0000 36

  9 omega   42.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000 -150.0000 27

 10 omega  -36.00   48.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -38.0000  -60.0000 84

 11 omega  -95.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000  -30.0000 90

 12 omega  -95.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000  150.0000 90

 13 omega -103.00  -78.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429 -179.0000    0.0000 25

 14 omega  -95.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000 -120.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0652741000
_diffrn_orient_matrix_UB_12      0.0257549000
_diffrn_orient_matrix_UB_13      0.0109331000
_diffrn_orient_matrix_UB_21      0.0134038000
_diffrn_orient_matrix_UB_22      0.0404582000
_diffrn_orient_matrix_UB_23      0.0109818000
_diffrn_orient_matrix_UB_31      -0.0084384000
_diffrn_orient_matrix_UB_32      0.0332046000
_diffrn_orient_matrix_UB_33      -0.0444374000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31465
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.70
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_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 1.171.36.20 (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_primary    colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.4125
_exptl_crystal_size_mid          0.2418
_exptl_crystal_size_min          0.1581
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0444P)^2^+0.4208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                6919
_reflns_number_total             9579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           ap74_16a
_cod_database_code               7029095
_chemical_oxdiff_formula         NaBC48H60N4O6
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C4(H4A,H4B), C5(H5A,H5B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B),
 C24(H24A,H24B), C3(H3A,H3B), C12(H12A,H12B), C11(H11A,H11B), C20(H20A,H20B),
 C10(H10A,H10B), C17(H17A,H17B), C16(H16A,H16B), C18(H18A,H18B), C14(H14A,H14B),
  C19(H19A,H19B), C23(H23A,H23B), C15(H15A,H15B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C44(H44), C30(H30), C48(H48), C32(H32), C34(H34), C45(H45),
 C35(H35), C42(H42), C38(H38), C33(H33), C46(H46), C29(H29), C26(H26), C47(H47),
  C28(H28), C39(H39), C41(H41), C40(H40), C27(H27)
;