#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:53:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179904 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/00/7020012.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_7020012
loop_
_publ_author_name
'Oresmaa, Larisa'
'Tarvainen, Heli'
'Machal, Kalle'
'Haukka, Matti'
_publ_section_title
;
 Ruthenium imidazole oxime carbonyls and their activities as CO-releasing
 molecules.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11170
_journal_page_last               11175
_journal_paper_doi               10.1039/c2dt31002c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C9 H10 Cl N3 O5 Ru'
_chemical_formula_sum            'C9 H10 Cl N3 O5 Ru'
_chemical_formula_weight         376.72
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.761(5)
_cell_angle_beta                 89.253(5)
_cell_angle_gamma                63.954(4)
_cell_formula_units_Z            2
_cell_length_a                   6.8943(3)
_cell_length_b                   7.7902(4)
_cell_length_c                   13.9622(9)
_cell_measurement_reflns_used    10438
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     645.49(7)
_computing_cell_refinement       'EvalCCD (Duisenberg, 1998-2003)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998-2003)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12272
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0236
_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)+(0.0129P)²+0.2721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                2488
_reflns_number_total             2954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31002c.txt
_cod_data_source_block           3
_cod_original_cell_volume        645.49(6)
_cod_database_code               7020012
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
Ru1 Ru 0.67731(3) 0.28350(3) 0.256513(13) 0.01326(6) Uani 1 1 d .
Cl2 Cl 0.82498(8) 0.27317(7) 0.41610(4) 0.01737(11) Uani 1 1 d .
O1 O 1.1299(3) 0.0665(2) 0.20484(12) 0.0270(4) Uani 1 1 d .
O3 O 0.5089(3) 0.2883(2) 0.05892(12) 0.0291(4) Uani 1 1 d .
O4 O 0.2448(2) 0.6263(2) 0.28743(12) 0.0233(3) Uani 1 1 d .
H4O H 0.3111 0.6770 0.2521 0.035 Uiso 1 1 d R
O5 O 0.5202(2) 0.7103(2) 0.19174(11) 0.0223(3) Uani 1 1 d .
O6 O 0.8478(2) 0.5529(2) 0.14842(11) 0.0184(3) Uani 1 1 d .
N1 N 0.3643(3) 0.4260(3) 0.30248(13) 0.0176(4) Uani 1 1 d .
N2 N 0.6111(3) 0.0403(3) 0.33777(13) 0.0166(4) Uani 1 1 d .
N3 N 0.3779(3) -0.0463(3) 0.41742(13) 0.0204(4) Uani 1 1 d .
H3N H 0.2586 -0.0329 0.4429 0.031 Uiso 1 1 d R
C1 C 0.9602(4) 0.1470(3) 0.22472(16) 0.0169(5) Uani 1 1 d .
C3 C 0.5682(3) 0.2896(3) 0.13382(17) 0.0191(5) Uani 1 1 d .
C4 C 0.6744(3) 0.5510(3) 0.19231(15) 0.0169(4) Uani 1 1 d .
C5 C 0.8345(4) 0.7484(3) 0.10023(17) 0.0212(5) Uani 1 1 d .
H5A H 0.8299 0.8184 0.1507 0.025 Uiso 1 1 calc R
H5B H 0.7017 0.8306 0.0518 0.025 Uiso 1 1 calc R
C6 C 1.0332(4) 0.7143(3) 0.04760(17) 0.0270(5) Uani 1 1 d .
H6A H 1.1630 0.6394 0.0968 0.040 Uiso 1 1 calc R
H6B H 1.0264 0.8431 0.0109 0.040 Uiso 1 1 calc R
H6C H 1.0400 0.6383 0.0007 0.040 Uiso 1 1 calc R
C7 C 0.2818(3) 0.3164(3) 0.35110(16) 0.0195(5) Uani 1 1 d .
H7 H 0.1428 0.3693 0.3738 0.023 Uiso 1 1 calc R
C8 C 0.4159(3) 0.1074(3) 0.36854(15) 0.0176(5) Uani 1 1 d .
C9 C 0.5555(4) -0.2171(3) 0.41701(16) 0.0214(5) Uani 1 1 d .
H9 H 0.5752 -0.3494 0.4457 0.026 Uiso 1 1 calc R
C10 C 0.6994(4) -0.1623(3) 0.36774(16) 0.0206(5) Uani 1 1 d .
H10 H 0.8392 -0.2509 0.3561 0.025 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'
Cl Cl 0.1484 0.1585 '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_publ_flag
C3 Ru1 C1 88.88(9) ?
C3 Ru1 C4 89.69(8) ?
C1 Ru1 C4 91.16(8) yes
C3 Ru1 N1 94.13(8) ?
C1 Ru1 N1 176.21(8) ?
C4 Ru1 N1 91.17(8) ?
C3 Ru1 N2 92.95(8) ?
C1 Ru1 N2 102.08(7) ?
C4 Ru1 N2 166.53(7) ?
N1 Ru1 N2 75.48(7) yes
C3 Ru1 Cl2 179.18(7) yes
C1 Ru1 Cl2 90.30(6) ?
C4 Ru1 Cl2 90.30(6) ?
N1 Ru1 Cl2 86.69(5) ?
N2 Ru1 Cl2 87.25(5) ?
N1 O4 H4O 105.4 ?
C4 O6 C5 116.38(16) ?
C7 N1 O4 116.19(17) ?
C7 N1 Ru1 118.07(14) ?
O4 N1 Ru1 125.71(12) ?
C8 N2 C10 106.67(17) ?
C8 N2 Ru1 111.34(14) ?
C10 N2 Ru1 141.97(15) ?
C8 N3 C9 107.58(18) ?
C8 N3 H3N 124.0 ?
C9 N3 H3N 128.4 ?
O1 C1 Ru1 179.3(2) ?
O3 C3 Ru1 177.57(19) ?
O5 C4 O6 118.90(19) ?
O5 C4 Ru1 122.65(15) ?
O6 C4 Ru1 118.46(15) ?
O6 C5 C6 106.90(17) ?
O6 C5 H5A 110.3 ?
C6 C5 H5A 110.3 ?
O6 C5 H5B 110.3 ?
C6 C5 H5B 110.3 ?
H5A C5 H5B 108.6 ?
C5 C6 H6A 109.5 ?
C5 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
C5 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
N1 C7 C8 114.36(19) ?
N1 C7 H7 122.8 ?
C8 C7 H7 122.8 ?
N2 C8 N3 110.10(19) ?
N2 C8 C7 120.70(19) ?
N3 C8 C7 129.2(2) ?
C10 C9 N3 106.72(19) ?
C10 C9 H9 126.6 ?
N3 C9 H9 126.6 ?
C9 C10 N2 108.9(2) ?
C9 C10 H10 125.5 ?
N2 C10 H10 125.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 C3 1.861(2) yes
Ru1 C1 1.881(2) yes
Ru1 C4 2.032(2) yes
Ru1 N1 2.1298(17) yes
Ru1 N2 2.1683(17) yes
Ru1 Cl2 2.4291(5) yes
O1 C1 1.130(3) ?
O3 C3 1.132(2) ?
O4 N1 1.364(2) yes
O4 H4O 0.8116 ?
O5 C4 1.227(2) ?
O6 C4 1.340(2) ?
O6 C5 1.456(2) ?
N1 C7 1.275(3) yes
N2 C8 1.325(3) ?
N2 C10 1.360(3) ?
N3 C8 1.345(3) ?
N3 C9 1.358(3) ?
N3 H3N 0.8664 ?
C5 C6 1.498(3) ?
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 H6A 0.9800 ?
C6 H6B 0.9800 ?
C6 H6C 0.9800 ?
C7 C8 1.429(3) ?
C7 H7 0.9500 ?
C9 C10 1.356(3) ?
C9 H9 0.9500 ?
C10 H10 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4O O5 0.81 1.74 2.526(2) 161.8 . yes
O4 H4O O1 0.81 2.62 3.046(2) 114.7 1_465 yes
N3 H3N Cl2 0.87 2.59 3.2263(18) 131.4 2_656 yes
N3 H3N Cl2 0.87 2.84 3.5172(19) 136.3 1_455 yes
