Synthesis of Group 4 Metal Complexes Stabilized by an Amine-Bridged Bis(phenolato) Ligand and Their Catalytic Behavior in Intermolecular Hydroamination Reactions
Sun, Qiu; Wang, Yaorong; Yuan, Dan; Yao, Yingming; Shen, Qi; Organometallics 33 (2014) 994–; doi:10.1021/om401158a

data_4082378
_publ_section_title
;
 Synthesis of Group 4 Metal Complexes Stabilized by an Amine-Bridged
 Bis(phenolato) Ligand and Their Catalytic Behavior in Intermolecular
 Hydroamination Reactions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              994
_journal_paper_doi               10.1021/om401158a
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C38 H64.50 N4 O2 Zr'
_chemical_formula_sum            'C38 H64.5 N4 O2 Zr'
_chemical_formula_weight         700.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.867(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.446(3)
_cell_length_b                   19.325(4)
_cell_length_c                   17.213(4)
_cell_measurement_temperature    223(2)
_cell_volume                     4101.1(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19265
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  0.8639
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7569
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0861
_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^)+(0.0922P)^2^+6.4416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                5913
_reflns_number_total             7569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401158a_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4101.2(16)
_cod_original_formula_sum        'C38 H64.50 N4 O2 Zr'
_cod_database_code               4082378