Monomeric Chiral and Achiral Basket-Handle Porphyrins: Synthesis, Structural Features, and Arrested Tautomerism.
Gehrold, Andreas C.; Bruhn, Torsten; Schneider, Heidi; Radius, Udo; Bringmann, Gerhard; The Journal of organic chemistry 80 (2015) 12359–12378; doi:10.1021/acs.joc.5b02259

data_4031739
_publ_section_title
;
 Monomeric Chiral and Achiral Basket-Handle Porphyrins: Synthesis,
 Structural Features, and Arrested Tautomerism.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12359
_journal_page_last               12378
_journal_paper_doi               10.1021/acs.joc.5b02259
_journal_volume                  80
_journal_year                    2015
_chemical_formula_sum            'C50 H46 Cl In N4 O2'
_chemical_formula_weight         885.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 120.622(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9867(11)
_cell_length_b                   14.2038(7)
_cell_length_c                   15.3868(8)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.125
_cell_measurement_theta_min      2.153
_cell_volume                     4135.1(4)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_radiation_monochromator  helios
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25636
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.143
_diffrn_reflns_theta_min         1.793
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6560
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_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.17
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_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+4.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0631
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_reflns_number_gt                3798
_reflns_number_total             4112
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           In-10d
_cod_depositor_comments
'Adding full bibliography for 4031738--4031739.cif.'
_cod_database_code               4031739
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