Synthesis and structure of the first non ?ate? heteroleptic lanthanoid complexes bearing monoanionic 2-amidopyridine ligands
Cole, Marcus L.; Junk, Peter C.; New Journal of Chemistry 27 (2003) 1032–; doi:10.1039/b304197b

data_7050616
_publ_section_title
;
 Synthesis and structure of the first non ?ate? heteroleptic lanthanoid
 complexes bearing monoanionic 2-amidopyridine ligands
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1032
_journal_paper_doi               10.1039/b304197b
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C29 H45 N2 Si Tb'
_chemical_formula_weight         608.68
_chemical_name_common            '[TbCp*2(AMPTMS)]'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   17.207(2)
_cell_length_b                   17.207(2)
_cell_length_c                   50.082(10)
_cell_measurement_temperature    123(2)
_cell_volume                     12842(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi 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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            20174
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_T_max  0.6307
_exptl_absorpt_correction_T_min  0.4300
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.416
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0298P)^2^+4.6584P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                5933
_reflns_number_total             7058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304197b.txt
_cod_data_source_block           compound3
_cod_original_cell_volume        12841(4)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7050616