A low-temperature polymorph of [5,10,15,20-<i>meso</i>-tetrakis(4-chlorophenyl)porphyrinato-κ^4^<i>N</i>]zinc(II) nitrobenzene clathrate
Mikki Vinodu; Israel Goldberg; Acta Crystallographica Section E 59 (2003) m565–m567; doi:10.1107/S1600536803014752

data_2202428
_publ_section_title
;A low-temperature polymorph of
 [5,10,15,20-<i>meso</i>-tetrakis(4-chlorophenyl)porphyrinato-\k^4^<i>N</i>]zinc(II)
 nitrobenzene clathrate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m565
_journal_page_last               m567
_journal_paper_doi               10.1107/S1600536803014752
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Zn (C44 H24 Cl4 N4)], C6 H5 N O2'
_chemical_formula_moiety         'C44 H24 Cl4 N4 Zn, C6 H5 N O2'
_chemical_formula_sum            'C50 H29 Cl4 N5 O2 Zn'
_chemical_formula_weight         938.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.7470(19)
_cell_angle_beta                 97.316(2)
_cell_angle_gamma                96.671(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9390(4)
_cell_length_b                   15.2220(4)
_cell_length_c                   16.8100(6)
_cell_measurement_reflns_used    8956
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.34
_cell_volume                     2005.47(13)
_computing_cell_refinement       'DENZO (Otwinowski, 1985)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        DENZO
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and
MERCURY (Cambridge Crystallographic Data Centre, 2002)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.1018
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19096
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_correction_T_min  0.7677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.648
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0546P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                5732
_reflns_number_total             8956
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6268.cif
_cod_data_source_block           I
_cod_database_code               2202428
_cod_database_fobs_code          2202428