Structural characterisation, EPR and magnetic properties of f‒f and f‒d lanthanide(iii) phenolic cryptates
Avecilla, Fernando; Platas-Iglesias, Carlos; Rodríguez-Cortiñas, Raquel; Guillemot, Geoffroy; Bünzli, Jean-Claude G.; Brondino, Carlos D.; Geraldes, Carlos F. G. C.; Blas, Andrés de; Rodríguez-Blas, Teresa; Journal of the Chemical Society, Dalton Transactions  (2002) 4658–; doi:10.1039/b206615g

data_7702861
_publ_section_title
;
 Structural characterisation, EPR and magnetic properties of f--f and f--d
 lanthanide(iii) phenolic cryptates
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4658
_journal_paper_doi               10.1039/b206615g
_journal_year                    2002
_chemical_formula_sum            'C45 H65 N11 O16 Tb2'
_chemical_formula_weight         1333.92
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.2130(17)
_cell_length_b                   28.2130(17)
_cell_length_c                   30.107(3)
_cell_measurement_temperature    150(2)
_cell_volume                     23964(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            78945
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  0.6991
_exptl_absorpt_correction_T_min  0.5127
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             10720
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.742
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         14729
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+160.6459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2017
_reflns_number_gt                10010
_reflns_number_total             14729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206615g.txt
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        23965(3)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7702861