Yttrium and Erbium Halide Complexes with [{Ti(η5-C5Me5)(μ-NH)}3(μ3-N)] as a Neutral Tridentate Ligand
Jorge Caballo; María García-Castro; Avelino Martín; Miguel Mena; Adrián Pérez-Redondo; Carlos Yélamos; Inorganic Chemistry 47 (2008) 7077–7079; doi:10.1021/ic8010426

data_4306121
_publ_section_title
;
Yttrium and Erbium Halide Complexes with [{Ti(\h5-C5Me5)(\m-NH)}3(\m3-N)]
as a Neutral Tridentate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7077
_journal_page_last               7079
_journal_paper_doi               10.1021/ic8010426
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H48 Cl3 Er1 N4 Ti3'
_chemical_formula_sum            'C30 H48 Cl3 Er N4 Ti3'
_chemical_formula_weight         882.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2008-02-28T18:02:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.177(4)
_cell_length_b                   17.907(2)
_cell_length_c                   37.753(6)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     7534(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1764
_diffrn_reflns_av_unetI/netI     0.2386
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            97638
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.00105(11)
_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   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         13606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.2115
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1132P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2525
_reflns_number_gt                5909
_reflns_number_total             13606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8010426-file001_1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C30 H48 Cl3 Er1 N4 Ti3'
_cod_database_code               4306121