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_7108512
_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            'C49 H42 N4 O Zr'
_chemical_formula_weight         794.09
_chemical_name_common            HB026
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2272(9)
_cell_length_b                   19.8419(10)
_cell_length_c                   20.2471(9)
_cell_measurement_temperature    100(2)
_cell_volume                     7724.4(6)
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            127751
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.18
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.9342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0333P)^2^+9.2735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                5315
_reflns_number_total             7116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35984g.txt
_cod_data_source_block           shelxl_hb026
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7108512