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_7029091
_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 H44 F12 N4 Na3 O8 P2, F6 P'
_chemical_formula_sum            'C24 H44 F18 N4 Na3 O8 P3'
_chemical_formula_weight         1020.52
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-26
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.686(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.848(2)
_cell_length_b                   17.969(3)
_cell_length_c                   16.913(3)
_cell_measurement_reflns_used    2314
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.2233
_cell_measurement_theta_min      2.5229
_cell_volume                     4009.6(12)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details
;
  1 omega   -1.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000  150.0000 49

  2 omega  -90.00  -44.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000 -180.0000 46

  3 omega  -30.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   57.0000  120.0000 73

  4 omega  -32.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   38.0000  -90.0000 73

  5 omega  -94.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366 -179.0000 -120.0000 60

  6 omega  -88.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000    0.0000 100

  7 omega  -87.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000 -150.0000 90

  8 omega  -87.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -57.0000  120.0000 90

  9 omega   -3.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000 -120.0000 64

 10 omega   -3.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000   30.0000 64

 11 omega   -3.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -100.0000   90.0000 25

 12 omega   -3.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616   57.0000  120.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0394306000
_diffrn_orient_matrix_UB_12      0.0191295000
_diffrn_orient_matrix_UB_13      -0.0302432000
_diffrn_orient_matrix_UB_21      -0.0365456000
_diffrn_orient_matrix_UB_22      -0.0214588000
_diffrn_orient_matrix_UB_23      0.0113862000
_diffrn_orient_matrix_UB_31      -0.0017399000
_diffrn_orient_matrix_UB_32      0.0270113000
_diffrn_orient_matrix_UB_33      0.0299401000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1991
_diffrn_reflns_av_unetI/netI     0.1674
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32122
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.945
_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            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.2738
_exptl_crystal_size_mid          0.1334
_exptl_crystal_size_min          0.0759
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.3039
_refine_ls_R_factor_gt           0.1745
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4286
_refine_ls_wR_factor_ref         0.4949
_reflns_number_gt                2014
_reflns_number_total             5004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           bishep_dm001_01
_cod_depositor_comments
;

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         510.26
_cod_original_formula_moiety         'C12 H22 F9 N2 Na1.5 O4 P1.5'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        4009.8(11)
_cod_original_formula_sum        'C12 H22 F9 N2 Na1.50 O4 P1.50'
_cod_database_code               7029091
_chemical_oxdiff_formula         'C12 H22 N2 O4 Na1.5 P1.5 F9.5'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32