Tetra- and Octapyrroles Synthesized from Confusion and Fusion Approaches.
Kong, Jiahui; Zhang, Qiong; Savage, Mathew; Li, Minzhi; Li, Xin; Yang, Sihai; Liang, Xu; Zhu, Weihua; Ågren, Hans; Xie, Yongshu; Organic letters 18 (2016) 5046–5049; doi:10.1021/acs.orglett.6b02495

data_1555789
_publ_section_title
;
 Tetra- and Octapyrroles Synthesized from Confusion and Fusion Approaches.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5046
_journal_page_last               5049
_journal_paper_doi               10.1021/acs.orglett.6b02495
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C74 H18 F30 N8'
_chemical_formula_weight         1588.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.537(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.864(3)
_cell_length_b                   23.111(4)
_cell_length_c                   18.348(3)
_cell_measurement_reflns_used    6806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.16
_cell_volume                     7094(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45494
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.369
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       strip
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_platon_squeeze_details          ' '
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         13909
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1361P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7473
_reflns_number_total             13909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02495_si_002.cif
_cod_data_source_block           mo_50612b
_cod_original_cell_volume        7093(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1555789
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2013-2
_shelx_res_checksum              99584
_shelx_hkl_checksum              4467