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_4316338
_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_moiety         'C8 H40 N8'
_chemical_formula_sum            'C32 H40 N8'
_chemical_formula_weight         536.72
_chemical_name_common
;
 1,4,7,10-(2-pyridylmethyl)-1,4,7,10-tetra aza cyclodecane
;
_chemical_name_systematic
;
 1,4,7,10-(2-pyridylmethyl)-1,4,7,10-tetra aza cyclodecane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.802(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.7979(12)
_cell_length_b                   6.5984(5)
_cell_length_c                   15.9867(12)
_cell_measurement_reflns_used    3620
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7836
_cell_measurement_theta_min      2.5776
_cell_volume                     1439.0(2)
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10545
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.18422
_exptl_absorpt_correction_T_min  0.84748
_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    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombahedral
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0049(13)
_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   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                1790
_reflns_number_total             2929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100447m_si_006.cif
_cod_data_source_block           sf1
_cod_original_cell_volume        1438.99(19)
_cod_database_code               4316338