A [2]rotaxane-based (1)H NMR spectroscopic probe for the simultaneous identification of physiologically important metal ions in solution.
Chen, Nai-Chia; Huang, Po-Yi; Lai, Chien-Chen; Liu, Yi-Hung; Wang, Yu; Peng, Shie-Ming; Chiu, Sheng-Hsien; Chemical communications (Cambridge, England)  (2007) 4122–4124; doi:10.1039/b706461f

data_7102181
_publ_section_title
;
 A [2]rotaxane-based (1)H NMR spectroscopic probe for the simultaneous
 identification of physiologically important metal ions in solution.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4122
_journal_page_last               4124
_journal_paper_doi               10.1039/b706461f
_journal_year                    2007
_chemical_formula_sum            'C74.5 H78 F18 N3 Na O7 P5'
_chemical_formula_weight         1647.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.374(1)
_cell_angle_beta                 82.008(1)
_cell_angle_gamma                77.480(1)
_cell_formula_units_Z            2
_cell_length_a                   10.2597(2)
_cell_length_b                   14.8941(2)
_cell_length_c                   26.3207(4)
_cell_measurement_reflns_used    76358
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.
_cell_measurement_theta_min      1
_cell_volume                     3885.98(11)
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_collection       'COLLECT (Nonius BV)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24690
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0094(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.751
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         13666
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.912
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.1196
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+3.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3203
_refine_ls_wR_factor_ref         0.3381
_reflns_number_gt                9212
_reflns_number_total             13666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b706461f.txt
_cod_data_source_block           ic12642
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C74.50 H78 F18 N3 Na O7 P5'
_cod_database_code               7102181