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_7002461
_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         '2(C60 H70 N2 O4 Ti), 3(C4 H10 O)'
_chemical_formula_structural     '[Ti{OPr(i)}2{L(H)}2]'
_chemical_formula_sum            'C132 H170 N4 O11 Ti2'
_chemical_formula_weight         2084.52
_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
_cell_angle_alpha                96.2270(10)
_cell_angle_beta                 91.6590(10)
_cell_angle_gamma                107.0150(10)
_cell_formula_units_Z            3
_cell_length_a                   13.7337(4)
_cell_length_b                   16.2802(5)
_cell_length_c                   42.8540(14)
_cell_measurement_reflns_used    36779
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     9089.6(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1083
_diffrn_reflns_av_sigmaI/netI    0.1288
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            146935
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             3366
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2135
_refine_ls_number_reflns         40617
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0941
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+15.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.2021
_reflns_number_gt                23409
_reflns_number_total             40617
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907982c.txt
_cod_data_source_block           12
_cod_database_code               7002461