#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:01:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179227 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/47/4314761.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_4314761
loop_
_publ_author_name
'Nicole L. Fry'
'Michael J. Rose'
'David L. Rogow'
'Crystal Nyitray'
'Manpreet Kaur'
'Pradip K. Mascharak'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
University of California, Santa Cruz,
1156 High Street,
Santa Cruz, CA 95064
USA
;
_publ_contact_author_email       pradip@chemsitry.ucsc.edu
_publ_contact_author_fax         '+1 831 459 2935'
_publ_contact_author_name        'Pradip Mascharak'
_publ_contact_author_phone       '+1 831 459 4251'
_publ_section_title
;
 Ruthenium Nitrosyls Derived from Tetradentate Ligands Containing
 Carboxamido-N and Phenolato-O Donors: Syntheses, Structures,
 Photolability, and Time Dependent Density Functional Theory Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1487
_journal_page_last               1495
_journal_paper_doi               10.1021/ic9017129
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C20 H17 N5 O4 Ru'
_chemical_formula_weight         492.46
_chemical_name_common            '[(bpb)Ru(NO)(OEt)]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   15.6611(17)
_cell_length_b                   13.0504(15)
_cell_length_c                   9.1589(10)
_cell_measurement_reflns_used    9413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0.7459
_cell_measurement_theta_min      0.6881
_cell_volume                     1871.9(4)
_computing_cell_refinement       'Bruker SAINT v7.34'
_computing_data_collection       'Bruker APEX-II v2.1-4'
_computing_data_reduction        'Bruker SAINT v7.34'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ω/2θ-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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20882
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0213
_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)+(0.0236P)²+1.2942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                2359
_reflns_number_total             2669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9017129_si_002_1.cif
_cod_data_source_block           xsc09018
_cod_database_code               4314761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-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
Ru1 Ru 0.483372(10) 0.2500 0.679805(17) 0.01552(6) Uani 1 2 d S . .
O2 O 0.37542(8) -0.02393(9) 0.56557(14) 0.0330(3) Uani 1 1 d . . .
N3 N 0.55961(11) 0.2500 0.54125(19) 0.0182(3) Uani 1 2 d S . .
N2 N 0.40970(8) 0.14830(10) 0.57899(13) 0.0183(2) Uani 1 1 d . . .
O3 O 0.60631(12) 0.2500 0.44389(19) 0.0317(4) Uani 1 2 d S . .
C4 C 0.23868(10) 0.19673(14) 0.30190(18) 0.0256(3) Uani 1 1 d . . .
H4A H 0.2007 0.1606 0.2395 0.038 Uiso 1 1 calc R . .
N4 N 0.53165(8) 0.11245(10) 0.77388(14) 0.0199(3) Uani 1 1 d . . .
C14 C 0.48743(10) 0.03037(12) 0.72468(17) 0.0203(3) Uani 1 1 d . . .
C17 C 0.61436(12) 0.00142(15) 0.9241(2) 0.0337(4) Uani 1 1 d . . .
H17A H 0.6593 -0.0068 0.9928 0.040 Uiso 1 1 calc R . .
C15 C 0.50440(11) -0.06765(13) 0.77443(19) 0.0261(3) Uani 1 1 d . . .
H15A H 0.4723 -0.1243 0.7393 0.031 Uiso 1 1 calc R . .
C13 C 0.41733(10) 0.04854(12) 0.61292(16) 0.0211(3) Uani 1 1 d . . .
C18 C 0.59407(11) 0.09742(14) 0.87140(18) 0.0270(3) Uani 1 1 d . . .
H18A H 0.6255 0.1549 0.9055 0.032 Uiso 1 1 calc R . .
C16 C 0.56891(12) -0.08214(14) 0.87627(19) 0.0315(4) Uani 1 1 d . . .
H16A H 0.5814 -0.1487 0.9123 0.038 Uiso 1 1 calc R . .
O4 O 0.40408(10) 0.2500 0.84632(16) 0.0218(3) Uani 1 2 d S . .
C2 C 0.35033(9) 0.19555(12) 0.48388(15) 0.0185(3) Uani 1 1 d . . .
C3 C 0.29395(10) 0.14265(13) 0.39268(17) 0.0222(3) Uani 1 1 d . . .
H3A H 0.2933 0.0699 0.3926 0.027 Uiso 1 1 calc R . .
C19 C 0.3155(2) 0.2267(2) 0.8440(4) 0.0274(10) Uani 0.50 1 d P A -1
H19A H 0.3008 0.1856 0.9313 0.033 Uiso 0.50 1 calc PR A -1
H19B H 0.3026 0.1849 0.7565 0.033 Uiso 0.50 1 calc PR A -1
C20 C 0.2606(2) 0.3246(4) 0.8415(5) 0.0436(10) Uani 0.50 1 d P A -1
H20A H 0.2001 0.3058 0.8397 0.065 Uiso 0.50 1 calc PR A -1
H20B H 0.2744 0.3648 0.7542 0.065 Uiso 0.50 1 calc PR A -1
H20C H 0.2726 0.3654 0.9289 0.065 Uiso 0.50 1 calc PR A -1
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
N3 Ru1 O4 175.90(7) . . ?
N3 Ru1 N2 93.41(6) . . ?
O4 Ru1 N2 89.64(5) . . ?
N3 Ru1 N2 93.41(6) . 7_565 ?
O4 Ru1 N2 89.64(5) . 7_565 ?
N2 Ru1 N2 83.86(7) . 7_565 ?
N3 Ru1 N4 92.94(5) . 7_565 ?
O4 Ru1 N4 84.86(4) . 7_565 ?
N2 Ru1 N4 163.22(5) . 7_565 ?
N2 Ru1 N4 80.28(5) 7_565 7_565 ?
N3 Ru1 N4 92.94(5) . . ?
O4 Ru1 N4 84.86(4) . . ?
N2 Ru1 N4 80.28(5) . . ?
N2 Ru1 N4 163.22(5) 7_565 . ?
N4 Ru1 N4 114.88(7) 7_565 . ?
O3 N3 Ru1 176.10(17) . . ?
C13 N2 C2 128.52(13) . . ?
C13 N2 Ru1 119.22(10) . . ?
C2 N2 Ru1 112.12(10) . . ?
C4 C4 C3 120.46(10) 7_565 . ?
C18 N4 C14 118.70(14) . . ?
C18 N4 Ru1 130.74(12) . . ?
C14 N4 Ru1 110.54(10) . . ?
N4 C14 C15 121.60(14) . . ?
N4 C14 C13 118.08(14) . . ?
C15 C14 C13 120.32(15) . . ?
C16 C17 C18 119.32(16) . . ?
C14 C15 C16 119.15(16) . . ?
O2 C13 N2 128.01(15) . . ?
O2 C13 C14 120.20(14) . . ?
N2 C13 C14 111.79(13) . . ?
N4 C18 C17 122.32(16) . . ?
C17 C16 C15 118.91(16) . . ?
C19 O4 C19 24.8(3) 7_565 . ?
C19 O4 Ru1 127.21(16) 7_565 . ?
C19 O4 Ru1 127.21(16) . . ?
C3 C2 N2 124.57(14) . . ?
C3 C2 C2 119.60(9) . 7_565 ?
N2 C2 C2 115.83(8) . 7_565 ?
C4 C3 C2 119.94(15) . . ?
O4 C19 C20 111.5(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 N3 1.7424(18) . ?
Ru1 O4 1.9667(15) . ?
Ru1 N2 1.9863(12) . ?
Ru1 N2 1.9863(12) 7_565 ?
Ru1 N4 2.1299(13) 7_565 ?
Ru1 N4 2.1299(13) . ?
O2 C13 1.2303(19) . ?
N3 O3 1.153(2) . ?
N2 C13 1.344(2) . ?
N2 C2 1.4155(18) . ?
C4 C4 1.390(4) 7_565 ?
C4 C3 1.392(2) . ?
N4 C18 1.339(2) . ?
N4 C14 1.353(2) . ?
C14 C15 1.384(2) . ?
C14 C13 1.520(2) . ?
C17 C16 1.374(3) . ?
C17 C18 1.380(2) . ?
C15 C16 1.388(2) . ?
O4 C19 1.420(3) 7_565 ?
O4 C19 1.420(3) . ?
C2 C3 1.398(2) . ?
C2 C2 1.421(3) 7_565 ?
C19 C20 1.540(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Ru1 N3 O3 180.000(3) . . . . ?
N2 Ru1 N3 O3 42.02(4) . . . . ?
N2 Ru1 N3 O3 -42.02(4) 7_565 . . . ?
N4 Ru1 N3 O3 -122.44(4) 7_565 . . . ?
N4 Ru1 N3 O3 122.44(4) . . . . ?
N3 Ru1 N2 C13 95.17(12) . . . . ?
O4 Ru1 N2 C13 -82.09(12) . . . . ?
N2 Ru1 N2 C13 -171.77(9) 7_565 . . . ?
N4 Ru1 N2 C13 -152.76(16) 7_565 . . . ?
N4 Ru1 N2 C13 2.76(12) . . . . ?
N3 Ru1 N2 C2 -88.74(10) . . . . ?
O4 Ru1 N2 C2 94.01(10) . . . . ?
N2 Ru1 N2 C2 4.33(12) 7_565 . . . ?
N4 Ru1 N2 C2 23.3(2) 7_565 . . . ?
N4 Ru1 N2 C2 178.86(10) . . . . ?
N3 Ru1 N4 C18 86.36(15) . . . . ?
O4 Ru1 N4 C18 -90.16(15) . . . . ?
N2 Ru1 N4 C18 179.32(15) . . . . ?
N2 Ru1 N4 C18 -161.50(17) 7_565 . . . ?
N4 Ru1 N4 C18 -8.26(18) 7_565 . . . ?
N3 Ru1 N4 C14 -95.53(11) . . . . ?
O4 Ru1 N4 C14 87.94(11) . . . . ?
N2 Ru1 N4 C14 -2.58(10) . . . . ?
N2 Ru1 N4 C14 16.6(2) 7_565 . . . ?
N4 Ru1 N4 C14 169.85(7) 7_565 . . . ?
C18 N4 C14 C15 1.0(2) . . . . ?
Ru1 N4 C14 C15 -177.34(13) . . . . ?
C18 N4 C14 C13 -179.42(14) . . . . ?
Ru1 N4 C14 C13 2.21(16) . . . . ?
N4 C14 C15 C16 -0.6(2) . . . . ?
C13 C14 C15 C16 179.85(15) . . . . ?
C2 N2 C13 O2 2.0(3) . . . . ?
Ru1 N2 C13 O2 177.33(14) . . . . ?
C2 N2 C13 C14 -177.67(13) . . . . ?
Ru1 N2 C13 C14 -2.29(17) . . . . ?
N4 C14 C13 O2 -179.81(15) . . . . ?
C15 C14 C13 O2 -0.3(2) . . . . ?
N4 C14 C13 N2 -0.2(2) . . . . ?
C15 C14 C13 N2 179.40(15) . . . . ?
C14 N4 C18 C17 -0.5(3) . . . . ?
Ru1 N4 C18 C17 177.47(13) . . . . ?
C16 C17 C18 N4 -0.4(3) . . . . ?
C18 C17 C16 C15 0.8(3) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
N3 Ru1 O4 C19 164.38(16) . . . 7_565 ?
N2 Ru1 O4 C19 -57.55(17) . . . 7_565 ?
N2 Ru1 O4 C19 26.31(17) 7_565 . . 7_565 ?
N4 Ru1 O4 C19 106.57(17) 7_565 . . 7_565 ?
N4 Ru1 O4 C19 -137.82(17) . . . 7_565 ?
N3 Ru1 O4 C19 -164.38(16) . . . . ?
N2 Ru1 O4 C19 -26.31(17) . . . . ?
N2 Ru1 O4 C19 57.55(17) 7_565 . . . ?
N4 Ru1 O4 C19 137.82(17) 7_565 . . . ?
N4 Ru1 O4 C19 -106.57(17) . . . . ?
C13 N2 C2 C3 -8.2(2) . . . . ?
Ru1 N2 C2 C3 176.12(12) . . . . ?
C13 N2 C2 C2 172.07(12) . . . 7_565 ?
Ru1 N2 C2 C2 -3.58(10) . . . 7_565 ?
C4 C4 C3 C2 -0.44(18) 7_565 . . . ?
N2 C2 C3 C4 -179.26(14) . . . . ?
C2 C2 C3 C4 0.43(18) 7_565 . . . ?
C19 O4 C19 C20 0.4(3) 7_565 . . . ?
Ru1 O4 C19 C20 -99.2(3) . . . . ?
