Supramolecular Crystal Chemistry with Porphyrin Tinkertoys. Hydrogen-Bonding and Coordination Networks with the “Chair” and “Table” Conformers of Tetra(3-carboxyphenyl)porphyrin
Lipstman, Sophia; Goldberg, Israel; Crystal Growth & Design 13 (2013) 942–; doi:10.1021/cg301728r

data_4507404
_publ_section_title
;
 Supramolecular Crystal Chemistry with Porphyrin Tinkertoys.
 Hydrogen-Bonding and Coordination Networks with the &#x201C;Chair&#x201D;
 and &#x201C;Table&#x201D; Conformers of Tetra(3-carboxyphenyl)porphyrin
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              942
_journal_paper_doi               10.1021/cg301728r
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C48 H28 N4 O8, 2(C9 H17 N2)'
_chemical_formula_sum            'C66 H62 N8 O8'
_chemical_formula_weight         1095.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.769(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1066(7)
_cell_length_b                   13.1551(12)
_cell_length_c                   29.311(3)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      1.70
_cell_volume                     2738.9(5)
_computing_cell_refinement       'Saint, Bruker-Axs'
_computing_data_collection       'ApexII, Bruker-Axs'
_computing_data_reduction        'Sain, Bruker-Axs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Apex-Duo, Bruker-Axs'
_diffrn_measurement_method       '0.5  \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16865
_diffrn_reflns_theta_full        26.19
_diffrn_reflns_theta_max         26.19
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.9729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+3.3162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                4134
_reflns_number_total             5459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301728r_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        2738.9(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4507404