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_7029094
_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         'C24 H48 N4 Na2 O10, 2(C24 H20 B)'
_chemical_formula_sum            'C72 H88 B2 N4 Na2 O10'
_chemical_formula_weight         1237.06
_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             2013-05-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                67.444(4)
_cell_angle_beta                 75.171(4)
_cell_angle_gamma                78.989(3)
_cell_formula_units_Z            1
_cell_length_a                   11.9380(5)
_cell_length_b                   12.1701(5)
_cell_length_c                   13.1018(7)
_cell_measurement_reflns_used    5119
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.5554
_cell_measurement_theta_min      2.6670
_cell_volume                     1690.15(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    '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  -30.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867   38.0000  120.0000 73

  2 omega  -91.00   35.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867    0.0000   90.0000 126

  3 omega   61.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000  -60.0000 31

  4 omega   60.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000   90.0000 43

  5 omega   42.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -109.0000  -83.0000 32

  6 omega   60.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000 -120.0000 43

  7 omega   10.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   38.0000  -60.0000 89

  8 omega   12.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -109.0000   96.0000 62

  9 omega  -95.00   -5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000  -60.0000 90

 10 omega -102.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867 -179.0000  150.0000 68

 11 omega  -96.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -77.0000  150.0000 100

 12 omega -102.00  -77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867 -179.0000   60.0000 25

 13 omega  -95.00   -5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000   30.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0011168000
_diffrn_orient_matrix_UB_12      -0.0147097000
_diffrn_orient_matrix_UB_13      -0.0476809000
_diffrn_orient_matrix_UB_21      0.0044776000
_diffrn_orient_matrix_UB_22      -0.0616968000
_diffrn_orient_matrix_UB_23      0.0334936000
_diffrn_orient_matrix_UB_31      -0.0616246000
_diffrn_orient_matrix_UB_32      0.0018659000
_diffrn_orient_matrix_UB_33      0.0136643000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28252
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.67
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.985
_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    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.5581
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.1241
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0398P)^2^+0.2426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                5539
_reflns_number_total             7743
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           ap76_3b
_cod_original_cell_volume        1690.16(13)
_cod_database_code               7029094
_chemical_oxdiff_formula         C36H40N2O3BNa
_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:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5C,H5D), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C4(H4C,H4D), C2(H2A,H2B),
 C3(H3A,H3B), C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C14(H14), C26(H26), C16(H16), C36(H36), C17(H17), C15(H15),
 C27(H27), C24(H24), C32(H32), C20(H20), C33(H33), C28(H28), C30(H30), C35(H35),
  C34(H34), C21(H21), C23(H23), C29(H29), C22(H22)
;