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_4307512
_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            'C54 H68 Fe2 N8 O3'
_chemical_formula_weight         988.86
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.337(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9641(14)
_cell_length_b                   14.0552(16)
_cell_length_c                   19.4466(14)
_cell_measurement_reflns_used    7225
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.8
_cell_volume                     5160.9(8)
_computing_cell_refinement       'STOE Wincell (X-Area)'
_computing_data_collection       'STOE WinXpose (X-Area)'
_computing_data_reduction        'STOE WinIntegrate (X-Area)'
_computing_publication_material  'WinGx-Version 1.70.00'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'IPDS1 (Stoe)'
_diffrn_measurement_method       phi-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  0.1634
_diffrn_reflns_av_sigmaI/netI    0.2412
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38292
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.85613
_exptl_absorpt_correction_T_min  0.78860
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Face-indexed absorption correction'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.583
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9064
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.582
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                3442
_reflns_number_total             9418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062009tsi20061019_115859_5.cif
_cod_data_source_block           sp30eca
_cod_database_code               4307512