Chemically Induced Breathing of Flexible Porphyrinic Covalent Cages.
Schoepff, Laetitia; Kocher, Lucas; Durot, Stéphanie; Heitz, Valérie; The Journal of organic chemistry 82 (2017) 5845–5851; doi:10.1021/acs.joc.7b00698

data_4032549
_publ_section_title
;
 Chemically Induced Breathing of Flexible Porphyrinic Covalent Cages.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5845
_journal_page_last               5851
_journal_paper_doi               10.1021/acs.joc.7b00698
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C142 H132 N34 O12 Zn2, 2(C3 H6 O)'
_chemical_formula_sum            'C148 H144 N34 O14 Zn2'
_chemical_formula_weight         2753.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3227(7)
_cell_length_b                   31.9115(12)
_cell_length_c                   32.7689(13)
_cell_measurement_reflns_used    9274
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.16
_cell_measurement_theta_min      2.70
_cell_volume                     22297.2(14)
_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'
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_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            123507
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.848
_diffrn_reflns_theta_min         2.697
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.820
_exptl_crystal_description       block
_exptl_crystal_F_000             5768
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.300
_platon_squeeze_details
;
 The residual electron density was assigned to ten molecules of the
 dimethylformamide solvent [3153/8 = 394 e per asymmetric unit; ten 
 molecules of C3H7NO would give 400e]. 
;
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         19490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1070P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13979
_reflns_number_total             19490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00698_si_001.cif
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_cod_database_code               4032549
_shelx_estimated_absorpt_t_min   0.738
_shelx_estimated_absorpt_t_max   0.829
_shelxl_version_number           2013-4
_shelx_res_checksum              42443
_shelx_hkl_checksum              11800