Synthesis of lithium corrole and its use as a reagent for the preparation of cyclopentadienyl zirconium and titanium corrole complexes
John Arnold; Heather Buckley; Penelope J. Brothers; Daniel Gryko; Chem.Commun. 48 (2012) 10766–; doi:10.1039/c2cc35984g

data_7108513
_publ_section_title
;
 Synthesis of lithium corrole and its use as a reagent for the preparation
 of cyclopentadienyl zirconium and titanium corrole complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              10766
_journal_paper_doi               10.1039/c2cc35984g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C54 H52 N4 O Ti'
_chemical_formula_weight         820.90
_chemical_name_common            HB028b
_chemical_name_systematic
;
?
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                96.477(4)
_cell_angle_beta                 93.780(4)
_cell_angle_gamma                104.095(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8502(10)
_cell_length_b                   14.0504(13)
_cell_length_c                   14.6264(13)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.33
_cell_measurement_theta_min      4.64
_cell_volume                     2138.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34085
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.13
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.7921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.9522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                7230
_reflns_number_total             7564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35984g.txt
_cod_data_source_block           shelxl_hb028b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108513