1H NMR in Solution and Solid State Structural Study of Lanthanide(III) Cryptates
C. Platas; F. Avecilla; A. de Blas; C. F. G. C. Geraldes; T. Rodríguez-Blas; H. Adams; J. Mahía; Inorganic Chemistry 38 (1999) 3190–3199; doi:10.1021/ic981314e

data_4322101
_publ_section_title
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 1H NMR in Solution and Solid State Structural Study of Lanthanide(III)
 Cryptates
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3190
_journal_page_last               3199
_journal_paper_doi               10.1021/ic981314e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C40 H54 Ce N11 O14'
_chemical_formula_weight         1053.06
_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                98.09(2)
_cell_angle_beta                 89.99(2)
_cell_angle_gamma                96.34(2)
_cell_formula_units_Z            2
_cell_length_a                   10.853(3)
_cell_length_b                   12.746(3)
_cell_length_c                   17.907(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2437.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7574
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.8089
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.477
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+5.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                5406
_reflns_number_total             6362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic981314e_1.cif
_cod_data_source_block           compound3
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+5.2250P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+5.2250P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322101