Novel yttrium and zirconium catalysts featuring reduced Ar-BIANH2 ligands for olefin hydroamination (Ar-BIANH2 = bis-arylaminoacenaphthylene)
Cimino, Alessandro; Moscatelli, Filippo; Ferretti, Francesco; Ragaini, Fabio; Germain, Stéphane; Hannedouche, Jérôme; Schulz, Emmanuelle; Luconi, Lapo; Rossin, Andrea; Giambastiani, Giuliano; New J. Chem. 40 (2016) 10285–; doi:10.1039/C6NJ02199A

data_7055832
_publ_section_title
;
 Novel yttrium and zirconium catalysts featuring reduced Ar-BIANH2 ligands
 for olefin hydroamination (Ar-BIANH2 = bis-arylaminoacenaphthylene)
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10285
_journal_paper_doi               10.1039/C6NJ02199A
_journal_volume                  40
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H59 N5 Zr1'
_chemical_formula_sum            'C42 H59 N5 Zr'
_chemical_formula_weight         725.16
_chemical_name_systematic        Zr(L)(NMe2)2(NHMe2)
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Hygroscopic'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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_date             2014-04-08T10:37:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-10-14 deposited with the CCDC.
2016-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.478(2)
_cell_length_b                   14.351(2)
_cell_length_c                   21.722(3)
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.154
_cell_measurement_theta_min      4.682
_cell_measurement_wavelength     1.5418
_cell_volume                     3889.8(10)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0564158
_diffrn_orient_matrix_UB_12      -0.0864589
_diffrn_orient_matrix_UB_13      0.0267445
_diffrn_orient_matrix_UB_21      -0.1097352
_diffrn_orient_matrix_UB_22      -0.0439016
_diffrn_orient_matrix_UB_23      0.014469
_diffrn_orient_matrix_UB_31      -0.0011038
_diffrn_orient_matrix_UB_32      -0.0461646
_diffrn_orient_matrix_UB_33      -0.0640801
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14133
_diffrn_reflns_theta_full        72.39
_diffrn_reflns_theta_max         72.39
_diffrn_reflns_theta_min         4.07
_exptl_absorpt_coefficient_mu    2.569
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.51433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.053(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.1827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.09
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                5600
_reflns_number_total             6478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02199a2.cif
_cod_data_source_block           gg206
_cod_depositor_comments          'Adding full bibliography for 7055832.cif.'
_cod_original_cell_volume        3890(10)
_cod_database_code               7055832