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_7029089
_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         'F6 P, C12 H21 N2 O3'
_chemical_formula_sum            'C12 H21 F6 N2 O3 P'
_chemical_formula_weight         386.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-31
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.6287(6)
_cell_length_b                   13.8824(7)
_cell_length_c                   20.0682(10)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.5485
_cell_measurement_theta_min      2.6757
_cell_volume                     3239.7(3)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -86.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429 -179.0000   90.0000 52

  2 omega  -50.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429   38.0000   30.0000 92

  3 omega  -92.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429    0.0000 -180.0000 123

  4 omega   60.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000 -150.0000 26

  5 omega   67.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000 -180.0000 29

  6 omega   42.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -127.0000 -142.0000 44

  7 omega  -30.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -57.0000 -120.0000 75

  8 omega   46.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -127.0000   37.0000 40

  9 omega  -96.00  -47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -77.0000   30.0000 49
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0117337000
_diffrn_orient_matrix_UB_12      0.0483570000
_diffrn_orient_matrix_UB_13      0.0091664000
_diffrn_orient_matrix_UB_21      0.0009073000
_diffrn_orient_matrix_UB_22      -0.0136827000
_diffrn_orient_matrix_UB_23      0.0340827000
_diffrn_orient_matrix_UB_31      0.0597972000
_diffrn_orient_matrix_UB_32      -0.0092404000
_diffrn_orient_matrix_UB_33      -0.0023404000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30797
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.68
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65202
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.6976
_exptl_crystal_size_mid          0.1279
_exptl_crystal_size_min          0.1267
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0618
_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          0.1604
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                2595
_reflns_number_total             3708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           ap60_17
_cod_database_code               7029089
_chemical_oxdiff_formula         'C12 H20 N2 O3 Li P F6'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H3A,H3B} of C3, {H4A,H4B} of C4, {H10A,H10B} of C10, {H11A,H11B} of C11,
  {H2A,H2B} of C2, {H5A,H5B} of C5, {H12A,H12B} of C12, {H8A,H8B} of C8, {H6A,
  H6B} of C6, {H7A,H7B} of C7
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B), C12(H12A,H12B), C5(H5A,H5B), C2(H2A,
 H2B), C11(H11A,H11B), C10(H10A,H10B), C4(H4A,H4B), C3(H3A,H3B)
;