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_7105830
_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 N3 O3 Re '
_chemical_formula_sum            'C33 H38 N3 O3 Re'
_chemical_formula_weight         710.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                87.855(4)
_cell_angle_beta                 87.178(5)
_cell_angle_gamma                84.036(6)
_cell_formula_units_Z            2
_cell_length_a                   10.1361(17)
_cell_length_b                   10.5681(18)
_cell_length_c                   13.789(2)
_cell_measurement_reflns_used    5583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      1.5
_cell_volume                     1466.5(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24082
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    4.181
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6703
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.9677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0389
_reflns_number_gt                6578
_reflns_number_total             6703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04286B.TXT
_cod_data_source_block           '__kuzuhara_1'
_cod_original_formula_sum        'C33 H38 N3 O3 Re '
_cod_database_code               7105830