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_7218345
_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 H28 N4 Ni O4, 6(C6 H5 N O2)'
_chemical_formula_sum            'C80 H58 N10 Ni O16'
_chemical_formula_weight         1474.07
_chemical_name_systematic
'5,10,15,20-tetra(4-hydroxyphenyl)porphyrinatonickel(II) 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                   27.3385(7)
_cell_length_b                   27.3385(7)
_cell_length_c                   18.3255(8)
_cell_measurement_reflns_used    4795
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      30.9320
_cell_measurement_theta_min      3.5270
_cell_volume                     13696.4(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      108(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur2, Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80726
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.513
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetontrile/methanol/ethylacetate/nitrobenzene'
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.497
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         13993
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0781
_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^)+(0.0828P)^2^+19.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.2180
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7301
_reflns_number_total             13993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01881h2.cif
_cod_data_source_block           rs726
_cod_depositor_comments
'Adding full bibliography for 7218344--7218346.cif.'
_cod_original_cell_volume        13696.4(9)
_cod_database_code               7218345
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2014/6
_shelx_res_checksum              64787