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_7105828
_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         'C30 H39 N3 '
_chemical_formula_sum            'C30 H39 N3'
_chemical_formula_weight         441.66
_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                 105.3790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5650(3)
_cell_length_b                   6.28328(13)
_cell_length_c                   28.6812(6)
_cell_measurement_reflns_used    14653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.1
_cell_volume                     2530.80(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_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 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'VariMax 2.4 kW Ultra fine focus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27028
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.00073(19)
_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   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                3297
_reflns_number_total             4635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC04286B.TXT
_cod_data_source_block           '_20100528_2'
_cod_original_cell_volume        2530.81(9)
_cod_original_formula_sum        'C30 H39 N3 '
_cod_database_code               7105828