#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:38:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179149 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/10/4311044.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_4311044
loop_
_publ_author_name
'Sylvie Ferlay'
'Helmut W. Schmalle'
'Giancarlo Francese'
'Helen Stoeckli-Evans'
'Mirco Imlau'
'Dominik Schaniel'
'Theo Woike'
_publ_section_title
;
 Light-Induced Metastable States in Oxalatenitrosylruthenium(II) and
 Terpyridinenitrosylruthenium(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3500
_journal_page_last               3506
_journal_paper_doi               10.1021/ic0350178
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C15 H12 Cl F6 N4 O2 P Ru'
_chemical_formula_weight         561.78
_chemical_name_systematic
; 
 Chlorohydroxy-terpy-ruthenium-nitrosyl hexafluorophosphate
;
_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                 105.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.688(2)
_cell_length_b                   13.936(3)
_cell_length_c                   14.544(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      10.4
_cell_measurement_theta_min      7.5
_cell_volume                     1888.9(7)
_computing_cell_refinement       'Enraf Nonius CAD-4 software'
_computing_data_collection       'Enraf Nonius CAD-4 software'
_computing_data_reduction        'MolEN (Fair, 1991)'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Enraf Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'ω-2θ scan'
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5789
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.8392
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Coppens et al. 1965'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0526P)²+3.3277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                4401
_reflns_number_total             5498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0350178si20040323_112720_3.cif
_cod_data_source_block           gianc8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+3.3277P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+3.3277P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4311044
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.01116(3) 0.209022(18) 0.887412(18) 0.02959(7) Uani 1 d . . .
N1 N 0.0693(3) 0.2101(2) 1.0135(2) 0.0384(6) Uani 1 d . . .
O1 O 0.0927(4) 0.2065(3) 1.0943(2) 0.0725(11) Uani 1 d . . .
O2 O 0.9420(3) 0.20455(19) 0.74697(18) 0.0416(6) Uani 1 d . . .
Cl1 Cl -0.18518(11) 0.10871(7) 0.89458(8) 0.0492(2) Uani 1 d . . .
N11 N 0.1605(3) 0.2918(2) 0.85794(19) 0.0329(6) Uani 1 d . . .
C21 C 0.2729(4) 0.2484(3) 0.8396(2) 0.0362(7) Uani 1 d . . .
C31 C 0.3658(4) 0.3032(3) 0.8036(3) 0.0464(9) Uani 1 d . . .
C41 C 0.3378(5) 0.3988(3) 0.7865(3) 0.0529(10) Uani 1 d . . .
C51 C 0.2167(4) 0.4411(3) 0.8036(3) 0.0466(9) Uani 1 d . . .
C61 C 0.1276(4) 0.3849(3) 0.8400(2) 0.0361(7) Uani 1 d . . .
C12 C 0.2792(4) 0.1439(3) 0.8576(2) 0.0378(7) Uani 1 d . . .
N22 N 0.1602(3) 0.1051(2) 0.8760(2) 0.0364(6) Uani 1 d . . .
C32 C 0.1549(5) 0.0113(3) 0.8911(3) 0.0509(10) Uani 1 d . . .
C42 C 0.2669(6) -0.0482(3) 0.8891(4) 0.0662(13) Uani 1 d . . .
C52 C 0.3881(6) -0.0104(4) 0.8733(3) 0.0683(14) Uani 1 d . . .
C62 C 0.3952(4) 0.0878(3) 0.8562(3) 0.0504(10) Uani 1 d . . .
C13 C -0.0069(4) 0.4152(2) 0.8612(2) 0.0357(7) Uani 1 d . . .
N23 N -0.0872(3) 0.3428(2) 0.8832(2) 0.0348(6) Uani 1 d . . .
C33 C -0.2091(4) 0.3636(3) 0.9063(3) 0.0441(8) Uani 1 d . . .
C43 C -0.2567(5) 0.4566(3) 0.9066(3) 0.0527(10) Uani 1 d . . .
C53 C -0.1783(5) 0.5295(3) 0.8822(3) 0.0516(10) Uani 1 d . . .
C63 C -0.0521(5) 0.5098(3) 0.8591(3) 0.0458(9) Uani 1 d . . .
P1 P -0.47407(11) 0.19057(7) 0.59333(7) 0.0405(2) Uani 1 d . . .
F1 F -0.3955(3) 0.2623(2) 0.6759(2) 0.0653(7) Uani 1 d . . .
F2 F -0.4416(3) 0.2581(2) 0.5140(2) 0.0689(8) Uani 1 d . . .
F3 F -0.5502(4) 0.1178(2) 0.5129(2) 0.0880(11) Uani 1 d . . .
F4 F -0.5001(4) 0.1200(3) 0.6721(2) 0.0903(11) Uani 1 d . . .
F5 F -0.3238(4) 0.1396(3) 0.6029(2) 0.0893(11) Uani 1 d . . .
F6 F -0.6199(4) 0.2408(4) 0.5834(3) 0.1139(15) Uani 1 d . . .
H2 H 0.8569 0.2041 0.7273 0.071(17) Uiso 1 d . . .
H31 H 0.4541 0.2795 0.7975 0.051(13) Uiso 1 d . . .
H41 H 0.3942 0.4413 0.7565 0.086(18) Uiso 1 d . . .
H51 H 0.2054 0.4970 0.7894 0.10(2) Uiso 1 d . . .
H32 H 0.0807 -0.010(4) 0.9034 0.062(15) Uiso 1 d . . .
H42 H 0.2522 -0.108(4) 0.9090 0.057(13) Uiso 1 d . . .
H52 H 0.4610 -0.052(4) 0.8718 0.073(16) Uiso 1 d . . .
H62 H 0.4786 0.1176 0.8438 0.042(11) Uiso 1 d . . .
H33 H -0.255(6) 0.3009 0.9134 0.071(16) Uiso 1 d . . .
H43 H -0.349(5) 0.4668 0.9074 0.072(16) Uiso 1 d . . .
H53 H -0.206(5) 0.5830 0.8844 0.052(13) Uiso 1 d . . .
H63 H 0.008(5) 0.5557 0.8350 0.058(13) Uiso 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'
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ru1 O2 178.17(12) . 1_455 yes
N1 Ru1 N11 100.08(13) . . yes
O2 Ru1 N11 81.71(11) 1_455 . yes
N1 Ru1 N22 93.27(13) . . yes
O2 Ru1 N22 86.68(11) 1_455 . yes
N11 Ru1 N22 79.93(12) . . yes
N1 Ru1 N23 92.08(13) . . yes
O2 Ru1 N23 88.56(11) 1_455 . yes
N11 Ru1 N23 80.14(11) . . yes
N22 Ru1 N23 159.97(12) . . yes
N1 Ru1 Cl1 89.50(11) . . yes
O2 Ru1 Cl1 88.71(9) 1_455 . yes
N11 Ru1 Cl1 170.42(8) . . yes
N22 Ru1 Cl1 100.03(9) . . yes
N23 Ru1 Cl1 99.30(8) . . yes
O1 N1 Ru1 172.6(3) . . yes
Ru1 O2 H2 113.5(2) 1_655 . yes
C21 N11 C61 124.2(3) . . yes
C21 N11 Ru1 117.6(2) . . yes
C61 N11 Ru1 117.0(2) . . yes
N11 C21 C31 118.4(4) . . yes
N11 C21 C12 114.0(3) . . yes
C31 C21 C12 127.5(3) . . yes
C41 C31 C21 119.1(4) . . yes
C41 C31 H31 117.6(4) . . yes
C21 C31 H31 122.8(4) . . yes
C31 C41 C51 120.9(4) . . yes
C31 C41 H41 124.0(4) . . yes
C51 C41 H41 114.9(4) . . yes
C61 C51 C41 118.4(4) . . yes
C61 C51 H51 126.4(5) . . yes
C41 C51 H51 115.2(4) . . yes
N11 C61 C51 119.0(3) . . yes
N11 C61 C13 114.2(3) . . yes
C51 C61 C13 126.8(3) . . yes
N22 C12 C62 121.0(4) . . yes
N22 C12 C21 115.4(3) . . yes
C62 C12 C21 123.6(4) . . yes
C32 N22 C12 119.7(3) . . yes
C32 N22 Ru1 127.7(3) . . yes
C12 N22 Ru1 112.4(2) . . yes
N22 C32 C42 121.6(4) . . yes
N22 C32 H32 117(3) . . yes
C42 C32 H32 121(3) . . yes
C52 C42 C32 119.5(4) . . yes
C52 C42 H42 128.9(9) . . yes
C32 C42 H42 110.7(11) . . yes
C42 C52 C62 119.8(4) . . yes
C42 C52 H52 117(3) . . yes
C62 C52 H52 123(3) . . yes
C12 C62 C52 118.4(4) . . yes
C12 C62 H62 119.1(4) . . yes
C52 C62 H62 122.5(4) . . yes
N23 C13 C63 120.8(3) . . yes
N23 C13 C61 115.4(3) . . yes
C63 C13 C61 123.8(3) . . yes
C33 N23 C13 119.6(3) . . yes
C33 N23 Ru1 127.6(2) . . yes
C13 N23 Ru1 112.5(2) . . yes
N23 C33 C43 121.5(4) . . yes
N23 C33 H33 107(3) . . yes
C43 C33 H33 132(3) . . yes
C53 C43 C33 119.1(4) . . yes
C53 C43 H43 120.2(7) . . yes
C33 C43 H43 118.8(7) . . yes
C43 C53 C63 120.4(4) . . yes
C43 C53 H53 118(3) . . yes
C63 C53 H53 122(3) . . yes
C53 C63 C13 118.6(4) . . yes
C53 C63 H63 126.9(18) . . yes
C13 C63 H63 114.3(17) . . yes
F6 P1 F3 89.5(2) . . yes
F6 P1 F4 91.5(2) . . yes
F3 P1 F4 90.17(17) . . yes
F6 P1 F2 91.2(2) . . yes
F3 P1 F2 89.26(16) . . yes
F4 P1 F2 177.2(2) . . yes
F6 P1 F1 91.3(2) . . yes
F3 P1 F1 178.85(18) . . yes
F4 P1 F1 88.99(16) . . yes
F2 P1 F1 91.55(16) . . yes
F6 P1 F5 179.5(2) . . yes
F3 P1 F5 90.5(2) . . yes
F4 P1 F5 89.0(2) . . yes
F2 P1 F5 88.24(19) . . yes
F1 P1 F5 88.68(19) . . yes
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 N1 1.766(3) . yes
Ru1 O2 1.969(3) 1_455 yes
Ru1 N11 1.986(3) . yes
Ru1 N22 2.084(3) . yes
Ru1 N23 2.086(3) . yes
Ru1 Cl1 2.3857(10) . yes
N1 O1 1.135(4) . yes
O2 Ru1 1.969(3) 1_655 yes
O2 H2 0.796(3) . yes
N11 C21 1.334(4) . yes
N11 C61 1.344(4) . yes
C21 C31 1.387(5) . yes
C21 C12 1.478(5) . yes
C31 C41 1.369(6) . yes
C31 H31 0.943(4) . yes
C41 C51 1.394(6) . yes
C41 H41 0.985(4) . yes
C51 C61 1.375(5) . yes
C51 H51 0.805(4) . yes
C61 C13 1.480(5) . yes
C12 N22 1.365(5) . yes
C12 C62 1.373(5) . yes
N22 C32 1.329(5) . yes
C32 C42 1.373(6) . yes
C32 H32 0.839(19) . yes
C42 C52 1.363(8) . yes
C42 H42 0.90(5) . yes
C52 C62 1.395(7) . yes
C52 H52 0.92(3) . yes
C62 H62 0.968(4) . yes
C13 N23 1.364(4) . yes
C13 C63 1.386(5) . yes
N23 C33 1.345(5) . yes
C33 C43 1.375(5) . yes
C33 H33 1.00(3) . yes
C43 C53 1.373(6) . yes
C43 H43 0.91(5) . yes
C53 C63 1.381(6) . yes
C53 H53 0.796(15) . yes
C63 H63 0.99(3) . yes
P1 F6 1.548(4) . yes
P1 F3 1.572(3) . yes
P1 F4 1.581(3) . yes
P1 F2 1.585(3) . yes
P1 F1 1.588(3) . yes
P1 F5 1.592(3) . yes
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
O2 Ru1 N1 O1 -23(6) 1_455 . . . yes
N11 Ru1 N1 O1 168(3) . . . . yes
N22 Ru1 N1 O1 -112(3) . . . . yes
N23 Ru1 N1 O1 87(3) . . . . yes
Cl1 Ru1 N1 O1 -12(3) . . . . yes
N1 Ru1 N11 C21 95.6(3) . . . . yes
O2 Ru1 N11 C21 -84.1(2) 1_455 . . . yes
N22 Ru1 N11 C21 4.0(2) . . . . yes
N23 Ru1 N11 C21 -174.1(3) . . . . yes
Cl1 Ru1 N11 C21 -86.6(6) . . . . yes
N1 Ru1 N11 C61 -96.9(3) . . . . yes
O2 Ru1 N11 C61 83.4(3) 1_455 . . . yes
N22 Ru1 N11 C61 171.5(3) . . . . yes
N23 Ru1 N11 C61 -6.5(2) . . . . yes
Cl1 Ru1 N11 C61 80.9(6) . . . . yes
C61 N11 C21 C31 3.0(5) . . . . yes
Ru1 N11 C21 C31 169.5(3) . . . . yes
C61 N11 C21 C12 -174.8(3) . . . . yes
Ru1 N11 C21 C12 -8.3(4) . . . . yes
N11 C21 C31 C41 -1.3(5) . . . . yes
C12 C21 C31 C41 176.2(4) . . . . yes
C21 C31 C41 C51 -0.8(6) . . . . yes
C31 C41 C51 C61 1.4(6) . . . . yes
C21 N11 C61 C51 -2.4(5) . . . . yes
Ru1 N11 C61 C51 -169.1(3) . . . . yes
C21 N11 C61 C13 176.6(3) . . . . yes
Ru1 N11 C61 C13 10.0(4) . . . . yes
C41 C51 C61 N11 0.2(5) . . . . yes
C41 C51 C61 C13 -178.7(4) . . . . yes
N11 C21 C12 N22 9.5(4) . . . . yes
C31 C21 C12 N22 -168.1(3) . . . . yes
N11 C21 C12 C62 -170.7(3) . . . . yes
C31 C21 C12 C62 11.7(6) . . . . yes
C62 C12 N22 C32 -1.3(5) . . . . yes
C21 C12 N22 C32 178.6(3) . . . . yes
C62 C12 N22 Ru1 174.1(3) . . . . yes
C21 C12 N22 Ru1 -6.1(4) . . . . yes
N1 Ru1 N22 C32 76.6(3) . . . . yes
O2 Ru1 N22 C32 -101.5(3) 1_455 . . . yes
N11 Ru1 N22 C32 176.3(3) . . . . yes
N23 Ru1 N22 C32 -178.1(3) . . . . yes
Cl1 Ru1 N22 C32 -13.4(3) . . . . yes
N1 Ru1 N22 C12 -98.2(2) . . . . yes
O2 Ru1 N22 C12 83.6(2) 1_455 . . . yes
N11 Ru1 N22 C12 1.4(2) . . . . yes
N23 Ru1 N22 C12 7.0(5) . . . . yes
Cl1 Ru1 N22 C12 171.7(2) . . . . yes
C12 N22 C32 C42 0.3(6) . . . . yes
Ru1 N22 C32 C42 -174.2(3) . . . . yes
N22 C32 C42 C52 1.4(7) . . . . yes
C32 C42 C52 C62 -2.1(8) . . . . yes
N22 C12 C62 C52 0.6(6) . . . . yes
C21 C12 C62 C52 -179.3(4) . . . . yes
C42 C52 C62 C12 1.1(7) . . . . yes
N11 C61 C13 N23 -8.4(4) . . . . yes
C51 C61 C13 N23 170.5(3) . . . . yes
N11 C61 C13 C63 171.9(3) . . . . yes
C51 C61 C13 C63 -9.2(6) . . . . yes
C63 C13 N23 C33 -2.2(5) . . . . yes
C61 C13 N23 C33 178.0(3) . . . . yes
C63 C13 N23 Ru1 -177.2(3) . . . . yes
C61 C13 N23 Ru1 3.0(4) . . . . yes
N1 Ru1 N23 C33 -73.0(3) . . . . yes
O2 Ru1 N23 C33 105.2(3) 1_455 . . . yes
N11 Ru1 N23 C33 -172.9(3) . . . . yes
N22 Ru1 N23 C33 -178.5(3) . . . . yes
Cl1 Ru1 N23 C33 16.8(3) . . . . yes
N1 Ru1 N23 C13 101.5(2) . . . . yes
O2 Ru1 N23 C13 -80.3(2) 1_455 . . . yes
N11 Ru1 N23 C13 1.6(2) . . . . yes
N22 Ru1 N23 C13 -4.0(5) . . . . yes
Cl1 Ru1 N23 C13 -168.7(2) . . . . yes
C13 N23 C33 C43 1.2(6) . . . . yes
Ru1 N23 C33 C43 175.4(3) . . . . yes
N23 C33 C43 C53 0.4(7) . . . . yes
C33 C43 C53 C63 -1.0(7) . . . . yes
C43 C53 C63 C13 0.0(6) . . . . yes
N23 C13 C63 C53 1.6(6) . . . . yes
C61 C13 C63 C53 -178.7(3) . . . . yes
