Triamidotriazacyclononane Complexes of Group 3 Metals. Synthesis and Crystal Structures
Bernardo Monteiro; Dmitrii Roitershtein; Humberto Ferreira; José R. Ascenso; Ana M. Martins; Ângela Domingos; Noémia Marques; Inorganic Chemistry 42 (2003) 4223–4231; doi:10.1021/ic034090v

data_4313828
_publ_section_title
;
 Triamidotriazacyclononane Complexes of Group 3 Metals. Synthesis and
 Crystal Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4223
_journal_page_last               4231
_journal_paper_doi               10.1021/ic034090v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[La{(SiMe2NPh)3-tacn}(THF)]'
_chemical_formula_sum            'C34 H53 La N6 O Si3'
_chemical_formula_weight         785.00
_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                 105.082(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.752(2)
_cell_length_b                   18.536(2)
_cell_length_c                   18.301(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      7.6
_cell_volume                     3849.3(9)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    'ORTEP-3 (Farrugia,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscans
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9655
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9441
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.784
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+5.2008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                6195
_reflns_number_total             9221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034090vrom20030128_020813_2.cif
_cod_data_source_block           latacn
_cod_original_cell_volume        3849.5(9)
_cod_database_code               4313828