Cyclometalation and coupling of a rigid 4,5-bis(imino)acridanide pincer ligand on yttrium.
Wong, Edwin W. Y.; Emslie, David J. H.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11601–11612; doi:10.1039/c5dt01636c

data_7035319
_publ_section_title
;
 Cyclometalation and coupling of a rigid 4,5-bis(imino)acridanide pincer
 ligand on yttrium.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11601
_journal_page_last               11612
_journal_paper_doi               10.1039/c5dt01636c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C86 H71 N6 Y1, 3.348(C6 H6)'
_chemical_formula_sum            'C106.09 H91.09 N6 Y'
_chemical_formula_weight         1538.91
_chemical_properties_physical    Air-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_update_record
;
2015-04-30 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                106.793(3)
_cell_angle_beta                 94.276(3)
_cell_angle_gamma                98.405(3)
_cell_formula_units_Z            2
_cell_length_a                   13.055(3)
_cell_length_b                   14.122(3)
_cell_length_c                   24.089(5)
_cell_measurement_reflns_used    9329
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.50
_cell_volume                     4174.0(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            100346
_diffrn_reflns_theta_full        28.734
_diffrn_reflns_theta_max         28.734
_diffrn_reflns_theta_min         1.518
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2001)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1617.236
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane/benzene'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         21480
_refine_ls_number_restraints     164
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.0018540
_refine_ls_shift/su_mean         0.0000714
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 4.89P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1209
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1208
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                16009
_reflns_number_total             21554
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.85
_oxford_diffrn_Wilson_scale      108.99
_oxford_refine_ls_r_factor_ref   0.0660
_oxford_refine_ls_scale          0.106536(19)
_oxford_reflns_number_all        21483
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c5dt01636c2.cif
_cod_data_source_block           cpd2
_cod_depositor_comments
'Adding full bibliography for 7035317--7035320.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C106.09 H91.09 N6 Y1'
_cod_database_code               7035319