Synthesis and structures of complexes with axially chiral isoquinolinyl-naphtholate ligands
Howard, Ruth H.; Alonso-Moreno, Carlos; Broomfield, Lewis M.; Hughes, David L.; Wright, Joseph A.; Bochmann, Manfred; Dalton Transactions  (2009) 8667–8682; doi:10.1039/b907982c

data_7002458
_publ_section_title
;
 Synthesis and structures of complexes with axially chiral
 isoquinolinyl-naphtholate ligands
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8667
_journal_page_last               8682
_journal_paper_doi               10.1039/b907982c
_journal_year                    2009
_chemical_formula_moiety         'C62 H72 Li2 N2 O4, C4 H8 O'
_chemical_formula_structural     '[Li2{L(H)}2(THF)2].THF'
_chemical_formula_sum            'C66 H80 Li2 N2 O5'
_chemical_formula_weight         995.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.995(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.524(6)
_cell_length_b                   10.431(4)
_cell_length_c                   37.439(13)
_cell_measurement_reflns_used    897
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      4.60
_cell_volume                     6429(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2smx'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7977
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            31733
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         4.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0073(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         11065
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                5747
_reflns_number_total             11065
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907982c.txt
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7002458