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#$Date: 2016-03-22 23:02:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179046 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/08/4300878.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4300878
loop_
_publ_author_name
'Emma Gallo'
'Alessandro Caselli'
'Fabio Ragaini'
'Simone Fantauzzi'
'Norberto Masciocchi'
'Angelo Sironi'
'Sergio Cenini'
_publ_section_title
;

Structural Determination of Ruthenium-Porphyrin Complexes Relevant to

Catalytic Epoxidation of Olefins

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2039
_journal_page_last               2049
_journal_paper_doi               10.1021/ic048587w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C45 H30 N4 O2 Ru'
_chemical_formula_weight         759.80
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5580(15)
_cell_length_b                   13.5580(15)
_cell_length_c                   9.6846(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1780.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9948
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0364
_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/[σ²(Fo²)+(0.0556P)²+0.6881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                786
_reflns_number_total             842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048587wsi20041008_102918.cif
_cod_data_source_block           RuTPPCOH2O
_cod_database_code               4300878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.0000 0.0000 0.0000 0.0287(3) Uani 1 8 d S . .
N N 0.1461(2) 0.0376(2) 0.0000 0.0334(8) Uani 1 2 d S . .
C1 C 0.2248(3) -0.0265(3) 0.0000 0.0347(9) Uani 1 2 d S . .
C2 C 0.3146(3) 0.0298(3) 0.0000 0.0429(11) Uani 1 2 d S . .
H2 H 0.3783 0.0043 0.0000 0.052 Uiso 1 2 calc SR . .
C3 C 0.2902(3) 0.1256(3) 0.0000 0.0414(11) Uani 1 2 d S . .
H3 H 0.3337 0.1786 0.0000 0.050 Uiso 1 2 calc SR . .
C4 C 0.1845(3) 0.1314(3) 0.0000 0.0358(10) Uani 1 2 d S . .
C5 C 0.2185(3) -0.1293(3) 0.0000 0.0338(9) Uani 1 2 d S . .
C6 C 0.3145(3) -0.1856(3) 0.0000 0.0360(10) Uani 1 2 d S . .
C7 C 0.3587(3) -0.2112(3) -0.1209(4) 0.0550(10) Uani 1 1 d . . .
H7 H 0.3298 -0.1937 -0.2045 0.066 Uiso 1 1 calc R . .
C8 C 0.4478(3) -0.2637(3) -0.1201(4) 0.0631(11) Uani 1 1 d . . .
H8 H 0.4778 -0.2805 -0.2032 0.076 Uiso 1 1 calc R . .
C9 C 0.4901(3) -0.2901(4) 0.0000 0.0517(13) Uani 1 2 d S . .
H9 H 0.5483 -0.3263 0.0000 0.062 Uiso 1 2 calc SR . .
O1 O 0.0000 0.0000 0.3011(17) 0.054(4) Uani 0.50 4 d SP . .
C C 0.0000 0.0000 0.181(7) 0.044(12) Uani 0.50 4 d SP . .
O2 O 0.0000 0.0000 0.229(4) 0.044(12) Uani 0.50 4 d SP . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C Ru C 180.000(2) . 9 ?
C Ru N 90.0 . 11 ?
C Ru N 90.0 9 11 ?
C Ru N 90.0 . . ?
C Ru N 90.0 9 . ?
N Ru N 90.0 11 . ?
C Ru N 90.0 . 9 ?
C Ru N 90.0 9 9 ?
N Ru N 90.0 11 9 ?
N Ru N 180.0 . 9 ?
C Ru N 90.0 . 3 ?
C Ru N 90.0 9 3 ?
N Ru N 180.00(18) 11 3 ?
N Ru N 90.0 . 3 ?
N Ru N 90.0 9 3 ?
C Ru O2 0.000(2) . . ?
C Ru O2 180.0 9 . ?
N Ru O2 90.0 11 . ?
N Ru O2 90.0 . . ?
N Ru O2 90.0 9 . ?
N Ru O2 90.0 3 . ?
C Ru O2 180.000(2) . 9 ?
C Ru O2 0.000(1) 9 9 ?
N Ru O2 90.0 11 9 ?
N Ru O2 90.0 . 9 ?
N Ru O2 90.0 9 9 ?
N Ru O2 90.0 3 9 ?
O2 Ru O2 180.000(1) . 9 ?
C4 N C1 106.9(3) . . ?
C4 N Ru 126.7(3) . . ?
C1 N Ru 126.4(3) . . ?
N C1 C5 125.7(4) . . ?
N C1 C2 108.7(4) . . ?
C5 C1 C2 125.6(4) . . ?
C3 C2 C1 107.8(4) . . ?
C2 C3 C4 107.4(4) . . ?
N C4 C5 125.4(4) . 3 ?
N C4 C3 109.1(4) . . ?
C5 C4 C3 125.5(4) 3 . ?
C1 C5 C4 125.8(4) . 11 ?
C1 C5 C6 116.9(4) . . ?
C4 C5 C6 117.3(4) 11 . ?
C7 C6 C7 118.8(4) 10 . ?
C7 C6 C5 120.6(2) 10 . ?
C7 C6 C5 120.6(2) . . ?
C6 C7 C8 120.3(3) . . ?
C9 C8 C7 120.5(4) . . ?
C8 C9 C8 119.7(5) . 10 ?
O2 O1 C 0.000(7) . . ?
O1 C Ru 180.000(1) . . ?
O1 O2 Ru 180.000(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru C 1.75(7) . ?
Ru C 1.75(7) 9 ?
Ru N 2.045(3) 11 ?
Ru N 2.045(3) . ?
Ru N 2.045(3) 9 ?
Ru N 2.045(3) 3 ?
Ru O2 2.22(4) . ?
Ru O2 2.22(4) 9 ?
N C4 1.373(5) . ?
N C1 1.377(5) . ?
C1 C5 1.395(6) . ?
C1 C2 1.438(6) . ?
C2 C3 1.340(6) . ?
C3 C4 1.435(6) . ?
C4 C5 1.399(6) 3 ?
C5 C4 1.399(6) 11 ?
C5 C6 1.509(6) . ?
C6 C7 1.361(4) 10 ?
C6 C7 1.361(4) . ?
C7 C8 1.402(5) . ?
C8 C9 1.345(5) . ?
C9 C8 1.345(5) 10 ?
O1 O2 0.70(3) . ?
O1 C 1.16(8) . ?
