#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:30:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179114 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307626.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_4307626
loop_
_publ_author_name
'Michael J. Rose'
'Apurba K. Patra'
'Eric A. Alcid'
'Marylin M. Olmstead'
'Pradip K. Mascharak'
_publ_section_title
;
Ruthenium Nitrosyls Derived from Polypyridine Ligands with Carboxamide or
Imine Nitrogen Donor(s): Isoelectronic Complexes with Different NO
Photolability
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2328
_journal_page_last               2338
_journal_paper_doi               10.1021/ic0620945
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C21 H19 Cl N5 O2 Ru, C2 H3 N'
_chemical_formula_sum            'C23 H22 Cl N6 O2 Ru'
_chemical_formula_weight         550.99
_chemical_name_common            (Py3P)Ru(Cl).CH3CN
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.899(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1334(12)
_cell_length_b                   12.7761(15)
_cell_length_c                   17.245(2)
_cell_measurement_reflns_used    981
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.2
_cell_volume                     2224.5(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 5.1, 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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29566
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.7250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.641
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0381P)²+1.4314P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                5743
_reflns_number_total             6734
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic0620945si20061102_062827_5.cif
_cod_data_source_block           mn1611
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.199685(13) 0.207984(10) 0.914620(7) 0.01297(5) Uani 1 1 d . . .
Cl1 Cl 0.22825(4) 0.05696(3) 0.84025(3) 0.01917(9) Uani 1 1 d . . .
O1 O 0.24279(14) 0.03817(11) 1.11825(8) 0.0225(3) Uani 1 1 d . . .
O2 O 0.53255(14) 0.32367(12) 0.82715(9) 0.0259(3) Uani 1 1 d . . .
N1 N 0.16472(15) 0.33699(12) 0.98824(9) 0.0161(3) Uani 1 1 d . . .
N2 N 0.14789(15) 0.12850(12) 1.01046(9) 0.0166(3) Uani 1 1 d . . .
N3 N 0.37474(15) 0.18153(12) 0.96896(9) 0.0150(3) Uani 1 1 d . . .
N4 N 0.31194(15) 0.29329(11) 0.84784(9) 0.0164(3) Uani 1 1 d . . .
N5 N 0.02606(15) 0.23295(12) 0.84087(9) 0.0157(3) Uani 1 1 d . . .
C1 C 0.25218(19) 0.41653(14) 0.99631(11) 0.0200(3) Uani 1 1 d . . .
H1A H 0.3209 0.4195 0.9622 0.024 Uiso 1 1 calc R . .
C2 C 0.2466(2) 0.49420(16) 1.05209(13) 0.0262(4) Uani 1 1 d . . .
H2A H 0.3086 0.5502 1.0552 0.031 Uiso 1 1 calc R . .
C3 C 0.1484(2) 0.48819(18) 1.10326(13) 0.0311(5) Uani 1 1 d . . .
H3A H 0.1439 0.5386 1.1435 0.037 Uiso 1 1 calc R . .
C4 C 0.0571(2) 0.40751(17) 1.09473(12) 0.0269(4) Uani 1 1 d . . .
H4A H -0.0115 0.4030 1.1289 0.032 Uiso 1 1 calc R . .
C5 C 0.06506(18) 0.33311(15) 1.03653(11) 0.0189(3) Uani 1 1 d . . .
C6 C -0.03628(18) 0.24703(15) 1.02546(11) 0.0199(3) Uani 1 1 d . . .
H6A H -0.0751 0.2478 0.9708 0.024 Uiso 1 1 calc R . .
H6B H -0.1085 0.2610 1.0593 0.024 Uiso 1 1 calc R . .
C7 C 0.02151(18) 0.13760(15) 1.04447(11) 0.0210(4) Uani 1 1 d . . .
H7A H 0.0347 0.1279 1.1016 0.025 Uiso 1 1 calc R . .
H7B H -0.0404 0.0830 1.0228 0.025 Uiso 1 1 calc R . .
C8 C 0.25120(18) 0.08972(14) 1.05808(10) 0.0168(3) Uani 1 1 d . . .
C9 C 0.38353(17) 0.12008(13) 1.03213(10) 0.0159(3) Uani 1 1 d . . .
C10 C 0.50793(19) 0.09481(14) 1.06760(11) 0.0201(3) Uani 1 1 d . . .
H10A H 0.5166 0.0533 1.1134 0.024 Uiso 1 1 calc R . .
C11 C 0.61968(19) 0.13188(15) 1.03433(12) 0.0220(4) Uani 1 1 d . . .
H11A H 0.7055 0.1147 1.0574 0.026 Uiso 1 1 calc R . .
C12 C 0.60666(18) 0.19395(15) 0.96752(12) 0.0209(4) Uani 1 1 d . . .
H12A H 0.6826 0.2188 0.9445 0.025 Uiso 1 1 calc R . .
C13 C 0.48020(17) 0.21851(13) 0.93566(10) 0.0162(3) Uani 1 1 d . . .
C14 C 0.44530(19) 0.28431(14) 0.86392(11) 0.0184(3) Uani 1 1 d . . .
C15 C 0.26167(19) 0.35432(15) 0.78044(11) 0.0204(4) Uani 1 1 d . . .
H15A H 0.2584 0.3100 0.7332 0.025 Uiso 1 1 calc R . .
H15B H 0.3220 0.4138 0.7731 0.025 Uiso 1 1 calc R . .
C16 C 0.12294(18) 0.39574(14) 0.79164(11) 0.0198(3) Uani 1 1 d . . .
H16A H 0.1262 0.4328 0.8422 0.024 Uiso 1 1 calc R . .
H16B H 0.0988 0.4478 0.7503 0.024 Uiso 1 1 calc R . .
C17 C 0.01448(18) 0.31410(14) 0.79002(10) 0.0168(3) Uani 1 1 d . . .
C18 C -0.09840(19) 0.32445(15) 0.73830(11) 0.0203(3) Uani 1 1 d . . .
H18A H -0.1056 0.3820 0.7033 0.024 Uiso 1 1 calc R . .
C19 C -0.19965(19) 0.25209(16) 0.73743(11) 0.0225(4) Uani 1 1 d . . .
H19A H -0.2776 0.2604 0.7033 0.027 Uiso 1 1 calc R . .
C20 C -0.18512(19) 0.16678(15) 0.78758(11) 0.0209(4) Uani 1 1 d . . .
H20A H -0.2518 0.1145 0.7875 0.025 Uiso 1 1 calc R . .
C21 C -0.07144(18) 0.16001(14) 0.83745(10) 0.0174(3) Uani 1 1 d . . .
H21A H -0.0610 0.1012 0.8711 0.021 Uiso 1 1 calc R . .
N6 N 0.3954(3) 0.60112(18) 0.90460(14) 0.0478(6) Uani 1 1 d . . .
C22 C 0.4597(3) 0.59623(19) 0.85454(15) 0.0354(5) Uani 1 1 d . . .
C23 C 0.5405(3) 0.5866(3) 0.78859(16) 0.0456(7) Uani 1 1 d . . .
H23A H 0.5562 0.5124 0.7783 0.068 Uiso 1 1 calc R . .
H23B H 0.6254 0.6221 0.8008 0.068 Uiso 1 1 calc R . .
H23C H 0.4939 0.6187 0.7425 0.068 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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 N4 80.46(6) . . ?
N3 Ru1 N2 79.20(6) . . ?
N4 Ru1 N2 158.38(6) . . ?
N3 Ru1 N5 171.39(6) . . ?
N4 Ru1 N5 93.23(6) . . ?
N2 Ru1 N5 107.72(6) . . ?
N3 Ru1 N1 92.19(6) . . ?
N4 Ru1 N1 93.04(6) . . ?
N2 Ru1 N1 80.52(6) . . ?
N5 Ru1 N1 94.01(6) . . ?
N3 Ru1 Cl1 88.32(4) . . ?
N4 Ru1 Cl1 91.75(5) . . ?
N2 Ru1 Cl1 94.90(5) . . ?
N5 Ru1 Cl1 86.00(4) . . ?
N1 Ru1 Cl1 175.20(4) . . ?
C1 N1 C5 118.62(16) . . ?
C1 N1 Ru1 120.26(12) . . ?
C5 N1 Ru1 120.39(12) . . ?
C8 N2 C7 116.18(15) . . ?
C8 N2 Ru1 115.40(12) . . ?
C7 N2 Ru1 125.46(12) . . ?
C9 N3 C13 123.67(15) . . ?
C9 N3 Ru1 118.93(12) . . ?
C13 N3 Ru1 117.09(12) . . ?
C14 N4 C15 118.79(15) . . ?
C14 N4 Ru1 116.02(12) . . ?
C15 N4 Ru1 124.90(12) . . ?
C21 N5 C17 118.34(15) . . ?
C21 N5 Ru1 119.37(12) . . ?
C17 N5 Ru1 121.87(12) . . ?
N1 C1 C2 123.09(18) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C1 C2 C3 118.39(19) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C4 C3 C2 118.88(19) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C4 C5 120.40(19) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
N1 C5 C4 120.54(18) . . ?
N1 C5 C6 118.80(16) . . ?
C4 C5 C6 120.66(17) . . ?
C5 C6 C7 113.16(15) . . ?
C5 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
N2 C7 C6 108.53(15) . . ?
N2 C7 H7A 110.0 . . ?
C6 C7 H7A 110.0 . . ?
N2 C7 H7B 110.0 . . ?
C6 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O1 C8 N2 126.32(17) . . ?
O1 C8 C9 120.98(16) . . ?
N2 C8 C9 112.65(15) . . ?
N3 C9 C10 119.24(17) . . ?
N3 C9 C8 113.26(15) . . ?
C10 C9 C8 127.45(16) . . ?
C9 C10 C11 118.50(17) . . ?
C9 C10 H10A 120.8 . . ?
C11 C10 H10A 120.8 . . ?
C10 C11 C12 120.63(17) . . ?
C10 C11 H11A 119.7 . . ?
C12 C11 H11A 119.7 . . ?
C13 C12 C11 118.34(18) . . ?
C13 C12 H12A 120.8 . . ?
C11 C12 H12A 120.8 . . ?
N3 C13 C12 119.59(17) . . ?
N3 C13 C14 114.00(15) . . ?
C12 C13 C14 126.41(17) . . ?
O2 C14 N4 126.99(17) . . ?
O2 C14 C13 121.16(17) . . ?
N4 C14 C13 111.85(15) . . ?
N4 C15 C16 110.32(15) . . ?
N4 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N4 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 115.66(15) . . ?
C17 C16 H16A 108.4 . . ?
C15 C16 H16A 108.4 . . ?
C17 C16 H16B 108.4 . . ?
C15 C16 H16B 108.4 . . ?
H16A C16 H16B 107.4 . . ?
N5 C17 C18 120.44(17) . . ?
N5 C17 C16 119.48(16) . . ?
C18 C17 C16 120.05(16) . . ?
C19 C18 C17 120.76(17) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C20 118.61(17) . . ?
C18 C19 H19A 120.7 . . ?
C20 C19 H19A 120.7 . . ?
C21 C20 C19 118.35(18) . . ?
C21 C20 H20A 120.8 . . ?
C19 C20 H20A 120.8 . . ?
N5 C21 C20 123.39(17) . . ?
N5 C21 H21A 118.3 . . ?
C20 C21 H21A 118.3 . . ?
N6 C22 C23 178.0(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
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 1.9634(15) . ?
Ru1 N4 2.0079(15) . ?
Ru1 N2 2.0461(15) . ?
Ru1 N5 2.1054(15) . ?
Ru1 N1 2.1285(15) . ?
Ru1 Cl1 2.3484(5) . ?
O1 C8 1.238(2) . ?
O2 C14 1.238(2) . ?
N1 C1 1.348(2) . ?
N1 C5 1.364(2) . ?
N2 C8 1.367(2) . ?
N2 C7 1.458(2) . ?
N3 C9 1.340(2) . ?
N3 C13 1.342(2) . ?
N4 C14 1.361(2) . ?
N4 C15 1.455(2) . ?
N5 C21 1.356(2) . ?
N5 C17 1.356(2) . ?
C1 C2 1.386(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.388(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.385(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.506(3) . ?
C6 C7 1.540(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.500(3) . ?
C9 C10 1.391(2) . ?
C10 C11 1.395(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.396(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.386(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.513(3) . ?
C15 C16 1.530(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.514(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.395(3) . ?
C18 C19 1.380(3) . ?
C18 H18A 0.9500 . ?
C19 C20 1.391(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.380(2) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
N6 C22 1.127(3) . ?
C22 C23 1.462(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
