Synthesis, structure, and reactivity of tris(amidate) mono(amido) and tetrakis(amidate) complexes of group 4 transition metals.
Payne, Philippa R.; Thomson, Robert K.; Medeiros, Diane M.; Wan, Geoff; Schafer, Laurel L.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15670–15677; doi:10.1039/c3dt51868j

data_7023738
_publ_section_title
;
 Synthesis, structure, and reactivity of tris(amidate) mono(amido) and
 tetrakis(amidate) complexes of group 4 transition metals.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15670
_journal_page_last               15677
_journal_paper_doi               10.1039/c3dt51868j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C71 H78 N4 O3 Zr'
_chemical_formula_sum            'C71 H78 N4 O3 Zr'
_chemical_formula_weight         1126.59
_chemical_name_common
'tris(N-(2,6-dimethylphenyl)naphthylamidate) mono(dimethylamido) zirconium, 4'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.864(2)
_cell_angle_beta                 84.741(2)
_cell_angle_gamma                67.350(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9659(8)
_cell_length_b                   12.5520(8)
_cell_length_c                   23.178(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.590
_cell_measurement_theta_min      2.448
_cell_volume                     3199.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       area-detector
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20144
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.9783
_exptl_absorpt_correction_T_min  0.9019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1192
_exptl_crystal_recrystallization_method 'Hot hexanes'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         8118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                5228
_reflns_number_total             8118
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt51868j.txt
_cod_data_source_block           ls087-sr
_cod_database_code               7023738