Chlorido(2,3,7,8,12,13,17,18-octaethylporphyrinato)iron(III): a new triclinic polymorph of Fe(OEP)Cl
Kohnhorst, Saifon A.; Haller, Kenneth J.; Acta Crystallographica Section C 70 (2014) 368–374; doi:10.1107/S2053229614005002

data_2019442
_publ_section_title
;
 Chlorido(2,3,7,8,12,13,17,18-octaethylporphyrinato)iron(III): a new
 triclinic polymorph of Fe(OEP)Cl
;
_journal_coeditor_code           SF3221
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              368
_journal_page_last               374
_journal_paper_doi               10.1107/S2053229614005002
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Fe (C36 H44 N4) Cl]'
_chemical_formula_moiety         'C36 H44 Cl Fe N4'
_chemical_formula_sum            'C36 H44 Cl Fe N4'
_chemical_formula_weight         624.05
_chemical_name_common            iron(III)chlorooctaethylporphyrin
_chemical_name_systematic
;
Chlorido(2,3,7,8,12,13,17,18-octaethylporphyrinato)iron(III)
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           'SHELXL-97 plus hand edits'
_cell_angle_alpha                71.9490(10)
_cell_angle_beta                 73.0340(10)
_cell_angle_gamma                82.4400(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4495(3)
_cell_length_b                   10.7805(4)
_cell_length_c                   15.7360(5)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.75
_cell_volume                     1610.42(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34934
_diffrn_reflns_theta_full        30.63
_diffrn_reflns_theta_max         30.63
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         9534
_refine_ls_number_restraints     1185
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.072
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.9291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                7545
_reflns_number_total             9534
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            sf3221sup1.cf
_cod_data_source_block           I
_cod_database_code               2019442
_cod_database_fobs_code          2019442