Isomorphous free-base, Ni(ii)- and Cu(ii)-5,10,15,20-tetra(4-hydroxyphenyl)porphyrin nitrobenzene hexasolvates with tetragonal 3D hydrogen-bonded network structures
Seidel, Rüdiger W.; Goddard, Richard; Oppel, Iris M.; CrystEngComm 16 (2014) 10505–; doi:10.1039/C4CE01881H

data_7218344
_publ_section_title
;
 Isomorphous free-base, Ni(ii)- and
 Cu(ii)-5,10,15,20-tetra(4-hydroxyphenyl)porphyrin nitrobenzene
 hexasolvates with tetragonal 3D hydrogen-bonded network structures
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              10505
_journal_paper_doi               10.1039/C4CE01881H
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C44 H30 N4 O4, 6(C6 H5 N O2)'
_chemical_formula_sum            'C80 H60 N10 O16'
_chemical_formula_weight         1417.38
_chemical_name_systematic
'5,10,15,20-tetra(4-hydroxyphenyl)-21,23H-porphyrin nitrobenzene hexasolvate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           103
_space_group_name_Hall           'P 4 -2c'
_space_group_name_H-M_alt        'P 4 c c'
_symmetry_space_group_name_Hall  'P 4 -2c'
_symmetry_space_group_name_H-M   'P 4 c c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.4518(11)
_cell_length_b                   27.4518(11)
_cell_length_c                   18.2099(8)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.4449
_cell_measurement_theta_min      3.2197
_cell_volume                     13723.0(10)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'PROTEUM2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'Diamond 3.2i (Crystal Impact GbR, 2012)'
_computing_publication_material  'enCIFer (Allen et al., 2002)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.52
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  'focusing multilayer X-ray optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            180455
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        55.262
_diffrn_reflns_theta_max         55.262
_diffrn_reflns_theta_min         1.609
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.96259
_exptl_absorpt_correction_T_min  0.79218
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             5904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/nitrobenzene'
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 3483 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.29(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         8581
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^+37.4986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                7944
_reflns_number_total             8581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01881h2.cif
_cod_data_source_block           6883sadabsP4cc
_cod_depositor_comments
'Adding full bibliography for 7218344--7218346.cif.'
_cod_original_cell_volume        13723.0(13)
_cod_database_code               7218344
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2014/6
_shelx_res_checksum              66137