Crystal structure of bis(tetraphenylphosphonium) bis(cyanido-κC)(29H,31H-tetrabenzo[b,g,l,q]porphinato-κ4N29,N30,N31,N32)ferrate(II) acetone disolvate
Nishi, Miki; Matsuda, Masaki; Hoshino, Norihisa; Akutagawa, Tomoyuki; Acta Crystallographica Section E Crystallographic Communications 71 (2015) m48–; doi:10.1107/S2056989015001735

data_2019831
_publ_section_title
;
 Crystal structure of bis(tetraphenylphosphonium)
 bis(cyanido-\kC)(29H,31H-tetrabenzo[b,g,l,q]porphinato-\k4N29,N30,N31,N32)ferrate(II)
 acetone disolvate
;
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              m48
_journal_paper_doi               10.1107/S2056989015001735
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'(C24 H20 P)2 [Fe (C36 H20 N4) (C N)2], 2C3 H6 O'
_chemical_formula_moiety
'2(C24 H20 P +), C38 H20 Fe N6 2-, 2(C3 H6 O)'
_chemical_formula_sum            'C92 H72 Fe N6 O2 P2'
_chemical_formula_weight         1411.35
_chemical_name_systematic
;Bis(tetraphenylphosphonium)
bis(cyanido-\k<i>C</i>)(29<i>H</i>,31<i>H</i>-tetrabenzo[<i>b</i>,<i>g</i>,<i>l</i>,<i>q</i>]porphinato-\k^4^<i>N</i>^29^,<i>N</i>^30^,<i>N</i>^31^,<i>N</i>^32^)ferrate(II) acetone disolvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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                67.2170(10)
_cell_angle_beta                 66.9150(10)
_cell_angle_gamma                85.5100(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8412(3)
_cell_length_b                   12.7764(3)
_cell_length_c                   13.8298(3)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    120
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      3.77
_cell_volume                     1767.88(7)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 1999)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 1999)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 1999)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
Yadokari-XG (Wakita, 2001) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20279
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 2001)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.362
_refine_ls_extinction_coef       0.0038(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0991P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                3518
_reflns_number_total             6348
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5120sup1.cf
_cod_data_source_block           I
_cod_database_code               2019831
_cod_database_fobs_code          2019831