Probing the Structure, Conformation, and Stereochemical Exchange in a Family of Lanthanide Complexes Derived from Tetrapyridyl-Appended Cyclen
Louise S. Natrajan; Ntai M. Khoabane; Benjamin L. Dadds; Christopher A. Muryn; Robin G. Pritchard; Sarah L. Heath; Alan M. Kenwright; Ilya Kuprov; Stephen Faulkner; Inorganic Chemistry 49 (2010) 7700–7709; doi:10.1021/ic100447m

data_4316341
_publ_section_title
;
 Probing the Structure, Conformation, and Stereochemical Exchange in a
 Family of Lanthanide Complexes Derived from Tetrapyridyl-Appended Cyclen
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7700
_journal_page_last               7709
_journal_paper_doi               10.1021/ic100447m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C38 H44.5 F9 N9.5 O9 S3 Tb'
_chemical_formula_weight         1204.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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            8
_cell_length_a                   10.6712(8)
_cell_length_b                   40.118(3)
_cell_length_c                   21.2798(18)
_cell_measurement_reflns_used    9393
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9912
_cell_measurement_theta_min      2.6164
_cell_volume                     9110.0(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET)
(compiled May 11 2006,17:41:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET)
(compiled May 11 2006,17:41:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET)
(compiled May 11 2006,17:41:17)
;
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.1164
_diffrn_reflns_av_sigmaI/netI    0.1648
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38911
_diffrn_reflns_theta_full        20.84
_diffrn_reflns_theta_max         20.84
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  1.19661
_exptl_absorpt_correction_T_min  0.80171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET)
(compiled May 11 2006,17:41:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.828
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         9548
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                5587
_reflns_number_total             9548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100447m_si_009.cif
_cod_data_source_block           osf19
_cod_original_cell_volume        9110.1(12)
_cod_original_formula_sum        'C38 H44.50 F9 N9.50 O9 S3 Tb'
_cod_database_code               4316341