Unusual Inner C-Alkylation of 2-N-Substituted N-Confused Porphyrin Cobalt Complexes in Toluene and p-Xylene
Yu-Cheng Wang; Jyh-Horung Chen; Shin-Shin Wang; Jo-Yu Tung; Inorganic Chemistry 52 (2013) 10711–10713; doi:10.1021/ic401507d

data_4336230
_publ_section_title
;
 Unusual Inner C-Alkylation of 2-N-Substituted N-Confused Porphyrin Cobalt
 Complexes in Toluene and p-Xylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10711
_journal_page_last               10713
_journal_paper_doi               10.1021/ic401507d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C61 H45 Cl Co N4 O2'
_chemical_formula_sum            'C61 H45 Cl Co N4 O2'
_chemical_formula_weight         960.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_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                 99.081(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0400(5)
_cell_length_b                   15.1258(10)
_cell_length_c                   18.4773(7)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1559
_cell_measurement_theta_min      2.7648
_cell_volume                     4702.7(4)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.1103
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21836
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         10757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.8082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                5764
_reflns_number_total             10757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401507d_si_001_3.cif
_cod_data_source_block           coxyl2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336230