Chlorido(12,17-diethoxycarbonyl-11,18-dimethyl-2:3,6:7-dibutanocorrphycenato-κ^4^<i>N</i>)iron(III)
Ohgo, Yoshiki; Yokoyama, Yuki; Neya, Saburo; Nakamura, Mikio; Acta Crystallographica Section E 67 (2011) m1903–m1904; doi:10.1107/S1600536811051130

data_2232642
_publ_section_title
;
 Chlorido(12,17-diethoxycarbonyl-11,18-dimethyl-2:3,6:7-dibutanocorrphycenato-\k^4^<i>N</i>)iron(III)
;
_journal_coeditor_code           DS2159
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1903
_journal_page_last               m1904
_journal_paper_doi               10.1107/S1600536811051130
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Fe (C36 H36 N4 O4) Cl]'
_chemical_formula_moiety         'C36 H36 Cl Fe N4 O4'
_chemical_formula_sum            'C36 H36 Cl Fe N4 O4'
_chemical_formula_weight         679.99
_chemical_name_common            Corrphycene
_chemical_name_systematic
;
Chlorido(12,17-diethoxycarbonyl-11,18-dimethyl-2:3,6:7-dibutanocorrphycenato-
\k^4^<i>N</i>)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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.156(3)
_cell_angle_beta                 65.645(3)
_cell_angle_gamma                71.291(3)
_cell_formula_units_Z            4
_cell_length_a                   14.455(2)
_cell_length_b                   15.876(2)
_cell_length_c                   16.013(2)
_cell_measurement_reflns_used    30087
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     3156.3(7)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'CrystalClear (Rigaku, 2002)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'SV (Nemoto & Ohashi, 1993) and <i>ORTEP</i> (Johnson, 1965)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \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  0.1019
_diffrn_reflns_av_sigmaI/netI    0.1368
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30087
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi <i>et al.</i>, 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       needle
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.973
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         14011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1573P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.3046
_reflns_number_gt                5731
_reflns_number_total             14011
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ds2159.cif
_cod_data_source_block           I
_cod_database_code               2232642
_cod_database_fobs_code          2232642