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_7035318
_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         'C95.50 H85 N6 Y1'
_chemical_formula_sum            'C95.5 H85 N6 Y'
_chemical_formula_weight         1405.67
_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                82.938(4)
_cell_angle_beta                 71.274(4)
_cell_angle_gamma                74.886(4)
_cell_formula_units_Z            2
_cell_length_a                   13.744(2)
_cell_length_b                   14.389(2)
_cell_length_c                   20.904(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.90
_cell_measurement_theta_min      2.20
_cell_volume                     3776.3(9)
_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      100
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.082
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60126
_diffrn_reflns_theta_full        25.267
_diffrn_reflns_theta_max         25.267
_diffrn_reflns_theta_min         1.467
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker AXS Inc., 2001) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1478
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane/toluene'
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.072
_refine_diff_density_max         1.82
_refine_diff_density_min         -2.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         11930
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.0008454
_refine_ls_shift/su_mean         0.0000275
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +11.19P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1867
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1865
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7264
_reflns_number_total             11994
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      85.86
_oxford_refine_ls_r_factor_ref   0.1271
_oxford_refine_ls_scale          0.12211(6)
_oxford_reflns_number_all        11932
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c5dt01636c2.cif
_cod_data_source_block           cpd1
_cod_depositor_comments
'Adding full bibliography for 7035317--7035320.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C95.50 H85 N6 Y1'
_cod_database_code               7035318