Supramolecular frameworks based on 5,10,15,20-tetra(4-carboxyphenyl)porphyrins.
Morshedi, Mahbod; Ward, Jas S.; Kruger, Paul E.; White, Nicholas G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 783–790; doi:10.1039/c7dt04162d

data_7045051
_publ_section_title
;
 Supramolecular frameworks based on
 5,10,15,20-tetra(4-carboxyphenyl)porphyrins.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              783
_journal_page_last               790
_journal_paper_doi               10.1039/c7dt04162d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H24 N4 Ni O8, C29 H32 N8'
_chemical_formula_sum            'C77 H56 N12 Ni O8'
_chemical_formula_weight         1336.04
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.556(3)
_cell_length_b                   17.556(3)
_cell_length_c                   56.930(11)
_cell_measurement_reflns_used    939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.2
_cell_measurement_theta_min      3.0
_cell_volume                     17547(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.740
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.740
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            42023
_diffrn_reflns_point_group_measured_fraction_full 0.740
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.746
_diffrn_reflns_theta_min         0.715
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.506
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.014
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.470(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         11743
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.739
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                7204
_reflns_number_total             11743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04162d2.cif
_cod_data_source_block           1_4
_cod_depositor_comments
'Adding full bibliography for 7045051--7045058.cif.'
_cod_original_cell_volume        17547(6)
_cod_database_code               7045051
_exptl_absorpt_special_details   'XDS (Kabsch, 1993)'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.530(18)
 0.470(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3. Restrained distances
 C53-C53_$1
 1.42 with sigma of 0.01
 C73_$1-C73
 1.42 with sigma of 0.01
 C72-C73
 1.42 with sigma of 0.01
 O89-C87 = O88-C87
 1.3 with sigma of 0.02
 N71-C72
 1.42 with sigma of 0.01
 C66-C65
 1.3 with sigma of 0.01
 C53-C52
 1.42 with sigma of 0.01
 N51-C52
 1.42 with sigma of 0.01
 C84-C87
 1.45 with sigma of 0.02
 C81-C56
 1.4 with sigma of 0.01
 C56-C52
 1.5 with sigma of 0.01
 C97-C94
 1.5 with sigma of 0.02
 O99-C97 = O98-C97
 1.3 with sigma of 0.02
 N12-C14
 2.3 with sigma of 0.01
 N11-N12
 2.05 with sigma of 0.02
 H11A-H12A
 2.1 with sigma of 0.01
 C72_$1-C72
 2.3 with sigma of 0.02
 C52_$1-C52
 2.3 with sigma of 0.02
 O88-C84
 2.4 with sigma of 0.02
 O89-C84
 2.4 with sigma of 0.02
4. Restrained planarity
 O88_$2, O89_$2, N11_$1, H11A_$1, H11B_$1, N12_$1, H12A_$1, H12B_$1, C87_$2,
 C13_$1
 with sigma of 0.1
 N71, C73, C73_$1, C72
 with sigma of 0.1
 N61_$1, C62_$1, C64_$1, C63_$1, C65_$1
 with sigma of 0.1
 N71, N61, C62, C64, C73, C73_$1, C63, C65, C66, C72, C72_$1
 with sigma of 0.1
 N51, C52_$1, C52, C53, C53_$1
 with sigma of 0.1
 O88, O89, C83, C87, C85, C81, C84, C82, C86
 with sigma of 0.1
 O98, O99, C93, C95, C97, C96, C92, C94, C91
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(N11) = Uanis(N12)
6. Rigid body (RIGU) restrains
 N1, H1A, H1B, N2, H2A, H2B, N11, H11A, H11B, N12, H12A, H12B, C5, H5, C4, C17,
  C16, H16, C9, H9, C3, C8, H8, C7, C6, H6, C10, C13, C15, H15, C14, C19, H19,
 C18, H18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ni51, O88, O98, O99, O89, N71, N51, N61, C83, C93, C87, C85, C81, C95, C84,
 C97, C82, C86, C62, C96, C92, C94, C64, C73, C52, C63, C53, C65, C91, C66, C72,
  C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Others
 Fixed Uiso: H63(0.2) H64(0.2) H85(0.2) H83(0.2) H82(0.2) H86(0.2) H96(0.2)
 H92(0.2) H93(0.2) H95(0.2) H73(0.2) H53(0.2)
 Fixed Z: Ni51(0.570889)
8.a Aromatic/amide H refined with riding coordinates:
 C63(H63), C64(H64), C5(H5), C9(H9), C8(H8), C6(H6), C85(H85), C83(H83),
 C82(H82), C86(H86), C96(H96), C92(H92), C93(H93), C95(H95), C15(H15), C19(H19),
  C18(H18), C16(H16), C73(H73), C53(H53)
8.b Fitted pentagon refined as free rotating group:
 N61(C62,C63,C64,C65)
8.c Fitted hexagon refined as free rotating group:
 C5(C4,C9,C8,C7,C6), C85(C84,C83,C82,C81,C86), C96(C91,C92,C93,C94,C95),
 C15(C14,C19,C18,C17,C16)
8.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N11(H11A,H11B), N12(H12A,H12B)
;
_shelx_res_checksum              86324
_shelx_fab_checksum              49571
_olex2_submission_special_instructions 'No special instructions were received'