Rare-Earth-Metal Complexes Supported by New Chiral Tetra-Azane Chelating Ligands: Synthesis, Characterization, and Catalytic Properties for Intramolecular Asymmetric Hydroamination
Zhang, Yanyu; Yao, Wei; Li, He; Mu, Ying; Organometallics 31 (2012) 4670–; doi:10.1021/om201286u

data_4078621
_publ_section_title
;
 Rare-Earth-Metal Complexes Supported by New Chiral Tetra-Azane Chelating
 Ligands: Synthesis, Characterization, and Catalytic Properties for
 Intramolecular Asymmetric Hydroamination
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4670
_journal_paper_doi               10.1021/om201286u
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C52 H70 Cl2 Li N4 O4 Y'
_chemical_formula_weight         981.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3497(16)
_cell_length_b                   18.816(3)
_cell_length_c                   22.036(3)
_cell_measurement_temperature    203(2)
_cell_volume                     5120.5(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1630
_diffrn_reflns_av_sigmaI/netI    0.2493
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28744
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10106
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                4770
_reflns_number_total             10106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201286u_si_001.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5120.5(12)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4078621