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_4313830
_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         '[Yb{(SiMe2NPh)3-tacn}].C6H5Me'
_chemical_formula_sum            'C37 H53 N6 Si3 Yb'
_chemical_formula_weight         839.16
_chemical_name_systematic
;
 ?
;
_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                 91.150(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9131(10)
_cell_length_b                   16.355(2)
_cell_length_c                   22.560(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      7.5
_cell_volume                     4025.8(8)
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.1711
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7212
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.445
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular-needle
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00039(9)
_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   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7025
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.2117
_refine_ls_R_factor_gt           0.0897
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+31.0128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1925
_reflns_number_gt                3246
_reflns_number_total             7025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034090vrom20030128_020813_4.cif
_cod_data_source_block           ybtacn
_cod_original_cell_volume        4025.9(9)
_cod_database_code               4313830