Template Synthesis of Decaphyrin without Meso-Bridges: Cyclo[10]pyrrole.
Okujima, Tetsuo; Ando, Chie; Agrawal, Saurabh; Matsumoto, Hiroki; Mori, Shigeki; Ohara, Keishi; Hisaki, Ichiro; Nakae, Takahiro; Takase, Masayoshi; Uno, Hidemitsu; Kobayashi, Nagao; Journal of the American Chemical Society 138 (2016) 7540–7543; doi:10.1021/jacs.6b04941

data_4130588
_publ_section_title
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 Template Synthesis of Decaphyrin without Meso-Bridges: Cyclo[10]pyrrole.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7540
_journal_page_last               7543
_journal_paper_doi               10.1021/jacs.6b04941
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C220 H230 N10'
_chemical_formula_sum            'C220 H230 N10'
_chemical_formula_weight         3014.30
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                114.8358(7)
_cell_angle_beta                 97.8836(7)
_cell_angle_gamma                103.4842(5)
_cell_formula_units_Z            1
_cell_length_a                   13.8029(2)
_cell_length_b                   24.1019(4)
_cell_length_c                   24.1387(3)
_cell_measurement_reflns_used    21294
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.855
_cell_measurement_theta_min      2.260
_cell_volume                     6830.69(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type  PIRATUS
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.853
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21312
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         28.855
_diffrn_reflns_theta_min         2.260
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1620.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         21292
_refine_ls_number_restraints     2318
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.1130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0790P)^2^+4.8900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2844
_refine_ls_wR_factor_ref         0.2909
_reflns_number_gt                14806
_reflns_number_total             21312
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja6b04941_si_002.cif
_cod_data_source_block           Cyclo10pyrrole
_cod_original_cell_volume        6830.69(19)
_cod_database_code               4130588
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2013-2
_shelx_res_checksum              72864
_shelx_hkl_checksum              33014