Cyanide-Promoted Demetalation of TrpyNiNCO: A Route to Sensitive Metallotripyrrins of CoII, FeII, and MnII
Martin Bröring; Serguei Prikhodovski; Carsten D. Brandt; Esther Cónsul Tejero; Silke Köhler; Clemens Pietzonka; Inorganic Chemistry 46 (2007) 917–925; doi:10.1021/ic062009t

data_4307509
_publ_section_title
;
Cyanide-Promoted Demetalation of TrpyNiNCO: A Route to Sensitive
Metallotripyrrins of CoII, FeII, and MnII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              917
_journal_page_last               925
_journal_paper_doi               10.1021/ic062009t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C27 H34 Co N4 O'
_chemical_formula_weight         489.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0670(6)
_cell_length_b                   10.6803(6)
_cell_length_c                   20.8687(12)
_cell_measurement_reflns_used    6034
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.464
_cell_measurement_theta_min      2.205
_cell_volume                     2447.5(2)
_computing_cell_refinement       'SAINT-NT V6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V6.0'
_computing_molecular_graphics    'Mercury 1.3'
_computing_publication_material  'WinGx-Version 1.70.00'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
_diffrn_measurement_method       '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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23749
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0581P)^2^+1.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                3951
_reflns_number_total             4473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062009tsi20061019_115859_2.cif
_cod_data_source_block           sp8ec
_cod_database_code               4307509