New synthesis of meso-free-[14]triphyrin(2.1.1) by McMurry coupling and its derivatization to Mn(I) and Re(I) complexes
Daiki Kuzuhara; Hiroko Yamada; ZhaoLi Xue; Tetsuo Okujima; Shigeki Mori; Zhen Shen; Hidemitsu Uno; Chem.Commun. 47 (2011) 722–; doi:10.1039/c0cc04286b

data_7105829
_publ_section_title
;
 New synthesis of meso-free-[14]triphyrin(2.1.1) by McMurry coupling and
 its derivatization to Mn(I) and Re(I) complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              722
_journal_paper_doi               10.1039/c0cc04286b
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C33 H38 Mn N3 O3 '
_chemical_formula_sum            'C33 H38 Mn N3 O3'
_chemical_formula_weight         579.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.781(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.844(2)
_cell_length_b                   15.867(3)
_cell_length_c                   17.615(4)
_cell_measurement_reflns_used    8824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.3
_cell_volume                     2986.8(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'VariMax 50 kV 24 mA Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48856
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6835
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+2.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                6371
_reflns_number_total             6835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04286B.TXT
_cod_data_source_block           '__kuzuhara'
_cod_original_cell_volume        2986.8(11)
_cod_original_formula_sum        'C33 H38 Mn N3 O3 '
_cod_database_code               7105829