#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:41:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179151 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/12/4311232.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_4311232
loop_
_publ_author_name
'Apurba K. Patra'
'Michael J. Rose'
'Karen A. Murphy'
'Marilyn M. Olmstead'
'Pradip K. Mascharak'
_publ_section_title
;
 Photolabile Ruthenium Nitrosyls with Planar Dicarboxamide Tetradentate N4
 Ligands: Effects of In-Plane and Axial Ligand Strength on NO Release
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4487
_journal_page_last               4495
_journal_paper_doi               10.1021/ic040030t
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C25 H21 N6 O3 Ru, B F4'
_chemical_formula_sum            'C25 H21 B F4 N6 O3 Ru'
_chemical_formula_weight         641.36
_chemical_name_common            '[(Me2bpb)Ru(NO)(py)](BF4)'
_chemical_name_systematic
;
  ?
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.560(7)
_cell_angle_beta                 97.412(12)
_cell_angle_gamma                97.951(7)
_cell_formula_units_Z            2
_cell_length_a                   8.894(2)
_cell_length_b                   10.969(3)
_cell_length_c                   12.991(3)
_cell_measurement_reflns_used    960
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.1
_cell_volume                     1230.2(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16092
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.566
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0455
_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/[σ²(Fo²)+(0.0800P)²+0.1995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                5972
_reflns_number_total             7269
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic040030t_3.cif
_cod_data_source_block           mn1562
_cod_database_code               4311232
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ru1 Ru 0.72536(2) 0.663295(19) 0.858556(17) 0.01305(8) Uani 1 1 d . . .
O1 O 1.1387(2) 0.8916(2) 0.96085(17) 0.0221(4) Uani 1 1 d . . .
O2 O 0.3921(2) 0.6447(2) 1.04839(17) 0.0209(4) Uani 1 1 d . . .
O3 O 0.8671(3) 0.4424(2) 0.87065(19) 0.0234(5) Uani 1 1 d . . .
N1 N 0.8974(3) 0.7757(2) 0.95362(19) 0.0155(4) Uani 1 1 d . . .
N2 N 0.6240(3) 0.6811(2) 0.98575(18) 0.0145(4) Uani 1 1 d . . .
N3 N 0.8813(3) 0.6997(2) 0.74924(19) 0.0162(5) Uani 1 1 d . . .
N4 N 0.4974(3) 0.5772(2) 0.79318(19) 0.0151(4) Uani 1 1 d . . .
N5 N 0.6407(3) 0.8256(2) 0.81543(19) 0.0148(4) Uani 1 1 d . . .
N6 N 0.8026(3) 0.5261(2) 0.87178(19) 0.0156(4) Uani 1 1 d . . .
C1 C 0.8718(3) 0.7943(3) 1.0600(2) 0.0165(5) Uani 1 1 d . . .
C2 C 0.7244(3) 0.7436(3) 1.0771(2) 0.0152(5) Uani 1 1 d . . .
C3 C 0.6869(3) 0.7575(3) 1.1789(2) 0.0155(5) Uani 1 1 d . . .
H3 H 0.5878 0.7226 1.1905 0.019 Uiso 1 1 calc R . .
C4 C 0.7940(3) 0.8223(3) 1.2638(2) 0.0159(5) Uani 1 1 d . . .
C5 C 0.9411(3) 0.8738(3) 1.2460(2) 0.0181(5) Uani 1 1 d . . .
C6 C 0.9783(3) 0.8588(3) 1.1449(2) 0.0186(5) Uani 1 1 d . . .
H6 H 1.0778 0.8930 1.1333 0.022 Uiso 1 1 calc R . .
C7 C 1.0233(3) 0.8235(3) 0.9143(2) 0.0168(5) Uani 1 1 d . . .
C8 C 1.0092(3) 0.7785(3) 0.7975(2) 0.0168(5) Uani 1 1 d . . .
C9 C 1.1285(3) 0.8157(3) 0.7438(2) 0.0187(5) Uani 1 1 d . . .
H9 H 1.2163 0.8724 0.7787 0.022 Uiso 1 1 calc R . .
C10 C 1.1173(3) 0.7686(3) 0.6381(2) 0.0197(6) Uani 1 1 d . . .
H10 H 1.1975 0.7928 0.5997 0.024 Uiso 1 1 calc R . .
C11 C 0.9878(3) 0.6858(3) 0.5891(2) 0.0194(6) Uani 1 1 d . . .
H11 H 0.9793 0.6517 0.5171 0.023 Uiso 1 1 calc R . .
C12 C 0.8704(3) 0.6533(3) 0.6463(2) 0.0178(5) Uani 1 1 d . . .
H12 H 0.7812 0.5975 0.6126 0.021 Uiso 1 1 calc R . .
C13 C 0.4718(3) 0.6393(2) 0.9783(2) 0.0140(5) Uani 1 1 d . . .
C14 C 0.4021(3) 0.5823(2) 0.8670(2) 0.0145(5) Uani 1 1 d . . .
C15 C 0.2463(3) 0.5388(3) 0.8426(2) 0.0177(5) Uani 1 1 d . . .
H15 H 0.1823 0.5428 0.8957 0.021 Uiso 1 1 calc R . .
C16 C 0.1841(3) 0.4886(3) 0.7384(2) 0.0192(6) Uani 1 1 d . . .
H16 H 0.0776 0.4574 0.7195 0.023 Uiso 1 1 calc R . .
C17 C 0.2821(3) 0.4860(3) 0.6641(2) 0.0181(5) Uani 1 1 d . . .
H17 H 0.2428 0.4542 0.5926 0.022 Uiso 1 1 calc R . .
C18 C 0.4369(3) 0.5295(3) 0.6935(2) 0.0164(5) Uani 1 1 d . . .
H18 H 0.5029 0.5256 0.6416 0.020 Uiso 1 1 calc R . .
C19 C 0.7518(4) 0.8357(3) 1.3728(2) 0.0214(6) Uani 1 1 d . . .
H19A H 0.7492 0.9236 1.3976 0.032 Uiso 1 1 calc R . .
H19B H 0.8283 0.8054 1.4202 0.032 Uiso 1 1 calc R . .
H19C H 0.6505 0.7868 1.3716 0.032 Uiso 1 1 calc R . .
C20 C 1.0590(4) 0.9417(3) 1.3367(2) 0.0236(6) Uani 1 1 d . . .
H20A H 1.0999 0.8812 1.3774 0.035 Uiso 1 1 calc R . .
H20B H 1.0108 0.9986 1.3820 0.035 Uiso 1 1 calc R . .
H20C H 1.1428 0.9894 1.3097 0.035 Uiso 1 1 calc R . .
C21 C 0.6455(3) 0.9284(3) 0.8862(2) 0.0164(5) Uani 1 1 d . . .
H21 H 0.6799 0.9263 0.9582 0.020 Uiso 1 1 calc R . .
C22 C 0.6017(3) 1.0371(3) 0.8568(2) 0.0200(6) Uani 1 1 d . . .
H22 H 0.6056 1.1080 0.9082 0.024 Uiso 1 1 calc R . .
C23 C 0.5523(3) 1.0410(3) 0.7522(3) 0.0207(6) Uani 1 1 d . . .
H23 H 0.5247 1.1152 0.7303 0.025 Uiso 1 1 calc R . .
C24 C 0.5435(3) 0.9333(3) 0.6790(2) 0.0195(6) Uani 1 1 d . . .
H24 H 0.5072 0.9326 0.6068 0.023 Uiso 1 1 calc R . .
C25 C 0.5886(3) 0.8283(3) 0.7134(2) 0.0164(5) Uani 1 1 d . . .
H25 H 0.5828 0.7554 0.6637 0.020 Uiso 1 1 calc R . .
F1 F 0.6050(3) 0.3847(2) 0.52386(17) 0.0429(6) Uani 1 1 d . . .
F2 F 0.8389(3) 0.3563(2) 0.60119(19) 0.0395(6) Uani 1 1 d . . .
F3 F 0.6331(2) 0.33323(18) 0.68801(14) 0.0243(4) Uani 1 1 d . . .
F4 F 0.6481(2) 0.18955(18) 0.54733(15) 0.0265(4) Uani 1 1 d . . .
B1 B 0.6802(4) 0.3156(3) 0.5905(3) 0.0206(6) Uani 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
N6 Ru1 N2 100.56(10) . . ?
N6 Ru1 N1 95.21(11) . . ?
N2 Ru1 N1 82.28(10) . . ?
N6 Ru1 N4 97.29(10) . . ?
N2 Ru1 N4 79.93(10) . . ?
N1 Ru1 N4 159.84(10) . . ?
N6 Ru1 N5 170.08(10) . . ?
N2 Ru1 N5 89.12(9) . . ?
N1 Ru1 N5 88.19(10) . . ?
N4 Ru1 N5 82.16(9) . . ?
N6 Ru1 N3 87.53(10) . . ?
N2 Ru1 N3 160.85(10) . . ?
N1 Ru1 N3 79.70(10) . . ?
N4 Ru1 N3 116.52(10) . . ?
N5 Ru1 N3 83.90(9) . . ?
C7 N1 C1 127.1(2) . . ?
C7 N1 Ru1 119.80(19) . . ?
C1 N1 Ru1 113.05(18) . . ?
C13 N2 C2 126.9(2) . . ?
C13 N2 Ru1 119.71(19) . . ?
C2 N2 Ru1 113.38(18) . . ?
C12 N3 C8 119.3(2) . . ?
C12 N3 Ru1 129.9(2) . . ?
C8 N3 Ru1 110.74(19) . . ?
C18 N4 C14 118.5(2) . . ?
C18 N4 Ru1 130.29(19) . . ?
C14 N4 Ru1 111.02(19) . . ?
C21 N5 C25 118.7(2) . . ?
C21 N5 Ru1 121.9(2) . . ?
C25 N5 Ru1 119.23(18) . . ?
O3 N6 Ru1 170.0(2) . . ?
C6 C1 C2 119.5(3) . . ?
C6 C1 N1 125.4(3) . . ?
C2 C1 N1 115.1(3) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 N2 125.1(3) . . ?
C1 C2 N2 115.3(2) . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 119.4(3) . . ?
C3 C4 C19 119.9(3) . . ?
C5 C4 C19 120.7(3) . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 C20 120.1(3) . . ?
C4 C5 C20 120.2(3) . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O1 C7 N1 128.4(3) . . ?
O1 C7 C8 120.3(3) . . ?
N1 C7 C8 111.2(2) . . ?
N3 C8 C9 121.9(3) . . ?
N3 C8 C7 118.5(2) . . ?
C9 C8 C7 119.5(3) . . ?
C10 C9 C8 118.8(3) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
N3 C12 C11 121.1(3) . . ?
N3 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
O2 C13 N2 127.8(3) . . ?
O2 C13 C14 120.6(3) . . ?
N2 C13 C14 111.6(2) . . ?
N4 C14 C15 122.0(3) . . ?
N4 C14 C13 117.7(2) . . ?
C15 C14 C13 120.3(2) . . ?
C14 C15 C16 119.1(3) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 C15 118.1(3) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
N4 C18 C17 122.1(3) . . ?
N4 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C4 C19 H19A 109.5 . . ?
C4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C20 H20A 109.5 . . ?
C5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 C22 121.9(3) . . ?
N5 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 118.7(3) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 119.0(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
N5 C25 C24 122.2(3) . . ?
N5 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
F3 B1 F1 109.8(3) . . ?
F3 B1 F4 110.3(3) . . ?
F1 B1 F4 109.6(3) . . ?
F3 B1 F2 109.3(3) . . ?
F1 B1 F2 108.7(3) . . ?
F4 B1 F2 109.2(3) . . ?
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
Ru1 N6 1.758(2) . ?
Ru1 N2 1.983(2) . ?
Ru1 N1 1.994(2) . ?
Ru1 N4 2.130(3) . ?
Ru1 N5 2.139(2) . ?
Ru1 N3 2.146(2) . ?
O1 C7 1.219(4) . ?
O2 C13 1.224(3) . ?
O3 N6 1.147(3) . ?
N1 C7 1.358(4) . ?
N1 C1 1.422(4) . ?
N2 C13 1.354(4) . ?
N2 C2 1.421(4) . ?
N3 C12 1.353(4) . ?
N3 C8 1.355(4) . ?
N4 C18 1.343(4) . ?
N4 C14 1.360(4) . ?
N5 C21 1.350(3) . ?
N5 C25 1.353(4) . ?
C1 C6 1.399(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.402(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(4) . ?
C4 C19 1.505(4) . ?
C5 C6 1.390(4) . ?
C5 C20 1.509(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.516(4) . ?
C8 C9 1.388(4) . ?
C9 C10 1.387(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.514(4) . ?
C14 C15 1.383(4) . ?
C15 C16 1.402(4) . ?
C15 H15 0.9500 . ?
C17 C18 1.380(4) . ?
C17 C16 1.382(4) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.389(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.402(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.379(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
F1 B1 1.391(4) . ?
F2 B1 1.403(4) . ?
F3 B1 1.383(4) . ?
F4 B1 1.398(4) . ?
