#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/14/7031473.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_7031473
loop_
_publ_author_name
'Akl, Joëlle'
'Sasaki, Isabelle'
'Lacroix, Pascal G.'
'Malfant, Isabelle'
'Mallet-Ladeira, Sonia'
'Vicendo, Patricia'
'Farfán, Norberto'
'Santillan, Rosa'
_publ_section_title
;
 Comparative photo-release of nitric oxide from isomers of substituted
 terpyridinenitrosylruthenium(ii) complexes: experimental and
 computational investigations.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12721
_journal_page_last               12733
_journal_paper_doi               10.1039/c4dt00974f
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H19 Cl2 N4 O Ru, F6 P, C H4 O'
_chemical_formula_sum            'C29 H23 Cl2 F6 N4 O2 P Ru'
_chemical_formula_weight         776.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.680(2)
_cell_angle_beta                 70.488(2)
_cell_angle_gamma                67.090(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3340(5)
_cell_length_b                   13.0961(6)
_cell_length_c                   13.2279(6)
_cell_measurement_reflns_used    3902
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.18
_cell_measurement_theta_min      2.41
_cell_measurement_wavelength     0.71073
_cell_volume                     1525.02(13)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16406
_diffrn_reflns_theta_full        23.85
_diffrn_reflns_theta_max         23.85
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.9430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         4680
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0990P)²+5.0071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.178
_reflns_number_gt                3609
_reflns_number_total             4680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00974f3.cif
_cod_data_source_block           Trans(Cl,Cl)[RU(FT)Cl2(NO)](PF6)
_cod_depositor_comments
'Adding full bibliography for 7031472--7031473.cif.'
_cod_original_cell_volume        1525.02(12)
_cod_original_formula_sum        '     C29 H23 Cl2 F6 N4 O2 P Ru '
_cod_database_code               7031473
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 0.63121(6) 0.65709(4) 0.68799(4) 0.0329(2) Uani 1 1 d . . .
Cl1 Cl 0.39069(18) 0.65205(15) 0.75553(14) 0.0430(5) Uani 1 1 d . . .
Cl2 Cl 0.87925(19) 0.63715(15) 0.63116(15) 0.0472(5) Uani 1 1 d . . .
P1 P 0.3850(4) 0.9060(3) 0.3292(3) 0.0937(10) Uani 1 1 d . . .
N3 N 0.6872(6) 0.4996(4) 0.7744(4) 0.0329(13) Uani 1 1 d . . .
C6 C 0.6908(7) 0.4841(5) 0.8794(5) 0.0328(15) Uani 1 1 d . . .
C5 C 0.6586(7) 0.5897(6) 0.9143(5) 0.0345(16) Uani 1 1 d . . .
N4 N 0.6616(6) 0.5634(4) 0.5754(4) 0.0335(13) Uani 1 1 d . . .
C29 C 0.7792(7) 0.1667(6) 0.9627(6) 0.0400(18) Uani 1 1 d . . .
F2 F 0.4681(7) 0.7861(4) 0.2921(5) 0.0855(17) Uani 1 1 d . . .
C24 C 0.8683(8) -0.1600(6) 1.1605(7) 0.054(2) Uani 1 1 d . . .
N2 N 0.6238(6) 0.6839(5) 0.8375(5) 0.0373(14) Uani 1 1 d . . .
C2 C 0.5884(8) 0.7952(6) 0.9639(6) 0.0448(18) Uani 1 1 d . . .
H2 H 0.5645 0.8675 0.9797 0.054 Uiso 1 1 calc R . .
C10 C 0.7120(7) 0.4130(5) 0.7276(5) 0.0320(15) Uani 1 1 d . . .
C9 C 0.7432(7) 0.3051(5) 0.7878(6) 0.0366(16) Uani 1 1 d . . .
H9 H 0.7611 0.2439 0.7551 0.044 Uiso 1 1 calc R . .
C14 C 0.6659(8) 0.5332(7) 0.4048(6) 0.050(2) Uani 1 1 d . . .
H14 H 0.6505 0.5631 0.3334 0.06 Uiso 1 1 calc R . .
C11 C 0.7028(7) 0.4494(5) 0.6128(5) 0.0345(16) Uani 1 1 d . . .
C8 C 0.7490(7) 0.2836(6) 0.8974(6) 0.0364(17) Uani 1 1 d . . .
C4 C 0.6585(8) 0.5949(7) 1.0161(6) 0.0432(18) Uani 1 1 d . . .
H4 H 0.6839 0.5276 1.0685 0.052 Uiso 1 1 calc R . .
C7 C 0.7225(7) 0.3758(6) 0.9412(6) 0.0368(16) Uani 1 1 d . . .
H7 H 0.7262 0.3645 1.0147 0.044 Uiso 1 1 calc R . .
C1 C 0.5908(8) 0.7858(6) 0.8630(6) 0.0419(17) Uani 1 1 d . . .
H1 H 0.5688 0.8523 0.8092 0.05 Uiso 1 1 calc R . .
C15 C 0.6434(8) 0.6053(6) 0.4734(6) 0.0417(17) Uani 1 1 d . . .
H15 H 0.6148 0.6847 0.4475 0.05 Uiso 1 1 calc R . .
C12 C 0.7280(8) 0.3764(6) 0.5483(6) 0.0442(18) Uani 1 1 d . . .
H12 H 0.7573 0.2973 0.5756 0.053 Uiso 1 1 calc R . .
C13 C 0.7108(8) 0.4179(7) 0.4431(6) 0.0490(19) Uani 1 1 d . . .
H13 H 0.7297 0.3674 0.3972 0.059 Uiso 1 1 calc R . .
C3 C 0.6206(8) 0.6999(7) 1.0419(6) 0.049(2) Uani 1 1 d . . .
H3 H 0.617 0.7054 1.1129 0.059 Uiso 1 1 calc R . .
C19 C 0.8736(10) -0.1365(8) 1.2584(8) 0.067(2) Uani 1 1 d . . .
C21 C 0.9307(10) -0.3317(8) 1.3363(10) 0.077(3) Uani 1 1 d . . .
H21 H 0.9513 -0.3915 1.3964 0.093 Uiso 1 1 calc R . .
C23 C 0.8941(8) -0.2698(7) 1.1540(8) 0.063(2) Uani 1 1 d . . .
H23 H 0.888 -0.2854 1.0904 0.076 Uiso 1 1 calc R . .
C22 C 0.9292(9) -0.3581(8) 1.2409(9) 0.069(3) Uani 1 1 d . . .
H22 H 0.9517 -0.4343 1.2359 0.082 Uiso 1 1 calc R . .
C20 C 0.9029(10) -0.2204(8) 1.3463(8) 0.075(3) Uani 1 1 d . . .
H20 H 0.9045 -0.2045 1.4113 0.09 Uiso 1 1 calc R . .
F4 F 0.3019(8) 1.0267(5) 0.3639(7) 0.119(2) Uani 1 1 d . . .
F5 F 0.2277(6) 0.8985(5) 0.3392(6) 0.0935(19) Uani 1 1 d . . .
F1 F 0.3671(7) 0.8416(6) 0.4566(5) 0.106(2) Uani 1 1 d . . .
F6 F 0.5371(7) 0.9120(6) 0.3249(5) 0.105(2) Uani 1 1 d . . .
F3 F 0.4166(13) 0.9601(7) 0.2005(6) 0.164(4) Uani 1 1 d . . .
N1 N 0.5795(7) 0.7952(5) 0.6117(5) 0.0453(15) Uani 1 1 d . . .
O1 O 0.5458(8) 0.8837(5) 0.5622(5) 0.078(2) Uani 1 1 d . . .
C16 C 0.7907(8) 0.1443(6) 1.0716(6) 0.052(2) Uani 1 1 d . . .
H16 H 0.7793 0.2042 1.1036 0.062 Uiso 1 1 calc R . .
C26 C 0.8221(10) -0.0338(7) 0.9829(8) 0.062(2) Uani 1 1 d . . .
H26 H 0.8334 -0.0948 0.9524 0.075 Uiso 1 1 calc R . .
C17 C 0.8183(9) 0.0361(7) 1.1304(6) 0.053(2) Uani 1 1 d . . .
C27 C 0.7937(9) 0.0802(6) 0.9204(7) 0.055(2) Uani 1 1 d . . .
H27 H 0.785 0.0944 0.8479 0.066 Uiso 1 1 calc R . .
C25 C 0.8319(8) -0.0502(7) 1.0843(7) 0.047(2) Uani 1 1 d . . .
C18 C 0.8425(12) -0.0070(8) 1.2430(8) 0.076(3) Uani 1 1 d . . .
H18A H 0.7553 0.0265 1.2982 0.092 Uiso 1 1 calc R . .
H18B H 0.9262 0.0089 1.2477 0.092 Uiso 1 1 calc R . .
O2 O 0.999(2) 0.207(2) 0.266(2) 0.121(6) Uani 0.511(12) 1 d PDU A 1
H2A H 0.9698 0.1892 0.2235 0.182 Uiso 0.511(12) 1 calc PR A 1
C28 C 0.962(3) 0.154(2) 0.363(3) 0.128(8) Uani 0.511(12) 1 d PDU A 1
H28A H 0.9954 0.1752 0.4123 0.191 Uiso 0.511(12) 1 calc PR A 1
H28B H 1.0049 0.0727 0.3649 0.191 Uiso 0.511(12) 1 calc PR A 1
H28C H 0.8557 0.1744 0.3858 0.191 Uiso 0.511(12) 1 calc PR A 1
O2' O 0.990(2) 0.282(2) 0.178(2) 0.121(6) Uani 0.489(12) 1 d PDU A 2
H2' H 1.0041 0.2277 0.1503 0.182 Uiso 0.489(12) 1 calc PR A 2
C28' C 0.967(3) 0.374(3) 0.107(3) 0.123(8) Uani 0.489(12) 1 d PDU A 2
H28D H 0.8626 0.4105 0.1149 0.184 Uiso 0.489(12) 1 calc PR A 2
H28E H 1.0133 0.3566 0.0334 0.184 Uiso 0.489(12) 1 calc PR A 2
H28F H 1.0083 0.4247 0.1178 0.184 Uiso 0.489(12) 1 calc PR A 2
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 0 '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 0.006 '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
N1 Ru1 N3 179.0(2)
N1 Ru1 N4 100.8(2)
N3 Ru1 N4 78.7(2)
N1 Ru1 N2 102.9(2)
N3 Ru1 N2 77.6(2)
N4 Ru1 N2 156.4(2)
N1 Ru1 Cl2 93.9(2)
N3 Ru1 Cl2 86.93(16)
N4 Ru1 Cl2 89.69(15)
N2 Ru1 Cl2 89.27(16)
N1 Ru1 Cl1 93.4(2)
N3 Ru1 Cl1 85.73(15)
N4 Ru1 Cl1 87.88(15)
N2 Ru1 Cl1 90.15(16)
Cl2 Ru1 Cl1 172.58(6)
F6 P1 F4 91.6(4)
F6 P1 F2 88.6(4)
F4 P1 F2 178.9(4)
F6 P1 F3 86.5(5)
F4 P1 F3 93.2(5)
F2 P1 F3 85.7(5)
F6 P1 F5 177.6(4)
F4 P1 F5 87.9(4)
F2 P1 F5 91.9(3)
F3 P1 F5 95.9(4)
F6 P1 F1 90.7(4)
F4 P1 F1 91.5(4)
F2 P1 F1 89.6(4)
F3 P1 F1 174.6(6)
F5 P1 F1 87.0(4)
C10 N3 C6 122.4(5)
C10 N3 Ru1 118.5(4)
C6 N3 Ru1 119.0(4)
N3 C6 C7 119.2(6)
N3 C6 C5 113.5(5)
C7 C6 C5 127.3(6)
N2 C5 C4 122.0(7)
N2 C5 C6 114.0(6)
C4 C5 C6 123.9(6)
C15 N4 C11 119.7(6)
C15 N4 Ru1 125.9(5)
C11 N4 Ru1 114.3(4)
C27 C29 C16 118.6(7)
C27 C29 C8 120.7(7)
C16 C29 C8 120.7(7)
C23 C24 C19 119.8(8)
C23 C24 C25 133.4(9)
C19 C24 C25 106.8(7)
C5 N2 C1 118.2(6)
C5 N2 Ru1 115.8(5)
C1 N2 Ru1 126.0(5)
C1 C2 C3 119.6(7)
C1 C2 H2 120.2
C3 C2 H2 120.2
N3 C10 C9 119.1(6)
N3 C10 C11 113.1(5)
C9 C10 C11 127.8(6)
C10 C9 C8 121.1(6)
C10 C9 H9 119.4
C8 C9 H9 119.4
C13 C14 C15 118.7(7)
C13 C14 H14 120.6
C15 C14 H14 120.6
C12 C11 N4 121.3(6)
C12 C11 C10 123.4(6)
N4 C11 C10 115.2(6)
C7 C8 C9 117.2(6)
C7 C8 C29 122.1(6)
C9 C8 C29 120.6(7)
C5 C4 C3 119.1(7)
C5 C4 H4 120.5
C3 C4 H4 120.5
C6 C7 C8 120.9(6)
C6 C7 H7 119.5
C8 C7 H7 119.5
N2 C1 C2 121.9(7)
N2 C1 H1 119
C2 C1 H1 119
N4 C15 C14 120.8(7)
N4 C15 H15 119.6
C14 C15 H15 119.6
C11 C12 C13 119.7(7)
C11 C12 H12 120.1
C13 C12 H12 120.1
C12 C13 C14 119.7(7)
C12 C13 H13 120.2
C14 C13 H13 120.2
C2 C3 C4 119.2(7)
C2 C3 H3 120.4
C4 C3 H3 120.4
C20 C19 C24 121.6(10)
C20 C19 C18 129.4(10)
C24 C19 C18 109.0(7)
C22 C21 C20 122.8(10)
C22 C21 H21 118.6
C20 C21 H21 118.6
C24 C23 C22 120.1(10)
C24 C23 H23 120
C22 C23 H23 120
C23 C22 C21 118.5(10)
C23 C22 H22 120.7
C21 C22 H22 120.7
C19 C20 C21 117.1(11)
C19 C20 H20 121.4
C21 C20 H20 121.4
O1 N1 Ru1 179.5(6)
C17 C16 C29 119.8(8)
C17 C16 H16 120.1
C29 C16 H16 120.1
C25 C26 C27 117.5(8)
C25 C26 H26 121.2
C27 C26 H26 121.2
C16 C17 C25 119.8(8)
C16 C17 C18 128.6(9)
C25 C17 C18 111.5(7)
C29 C27 C26 121.5(8)
C29 C27 H27 119.3
C26 C27 H27 119.3
C26 C25 C17 122.8(7)
C26 C25 C24 126.7(8)
C17 C25 C24 110.4(7)
C17 C18 C19 102.3(8)
C17 C18 H18A 111.3
C19 C18 H18A 111.3
C17 C18 H18B 111.3
C19 C18 H18B 111.3
H18A C18 H18B 109.2
O2 C28 H28A 109.5
O2 C28 H28B 109.5
H28A C28 H28B 109.5
O2 C28 H28C 109.5
H28A C28 H28C 109.5
H28B C28 H28C 109.5
C28' O2' H2' 109.5
O2' C28' H28D 109.5
O2' C28' H28E 109.5
H28D C28' H28E 109.5
O2' C28' H28F 109.5
H28D C28' H28F 109.5
H28E C28' H28F 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 N1 1.759(6)
Ru1 N3 2.001(5)
Ru1 N4 2.073(6)
Ru1 N2 2.081(6)
Ru1 Cl2 2.3478(18)
Ru1 Cl1 2.3642(18)
P1 F6 1.585(7)
P1 F4 1.599(7)
P1 F2 1.604(6)
P1 F3 1.612(8)
P1 F5 1.626(7)
P1 F1 1.629(7)
N3 C10 1.350(8)
N3 C6 1.353(8)
C6 C7 1.384(9)
C6 C5 1.468(10)
C5 N2 1.355(8)
C5 C4 1.368(10)
N4 C15 1.344(8)
N4 C11 1.363(8)
C29 C27 1.345(11)
C29 C16 1.418(11)
C29 C8 1.487(9)
C24 C23 1.382(12)
C24 C19 1.440(13)
C24 C25 1.482(10)
N2 C1 1.360(9)
C2 C1 1.368(10)
C2 C3 1.369(11)
C2 H2 0.95
C10 C9 1.372(9)
C10 C11 1.473(9)
C9 C8 1.409(10)
C9 H9 0.95
C14 C13 1.381(11)
C14 C15 1.403(11)
C14 H14 0.95
C11 C12 1.362(10)
C8 C7 1.386(10)
C4 C3 1.389(11)
C4 H4 0.95
C7 H7 0.95
C1 H1 0.95
C15 H15 0.95
C12 C13 1.380(10)
C12 H12 0.95
C13 H13 0.95
C3 H3 0.95
C19 C20 1.366(13)
C19 C18 1.559(13)
C21 C22 1.409(15)
C21 C20 1.410(14)
C21 H21 0.95
C23 C22 1.397(11)
C23 H23 0.95
C22 H22 0.95
C20 H20 0.95
N1 O1 1.132(7)
C16 C17 1.368(10)
C16 H16 0.95
C26 C25 1.326(11)
C26 C27 1.443(11)
C26 H26 0.95
C17 C25 1.377(12)
C17 C18 1.496(12)
C27 H27 0.95
C18 H18A 0.99
C18 H18B 0.99
O2 C28 1.27(2)
O2 H2A 0.84
C28 H28A 0.98
C28 H28B 0.98
C28 H28C 0.98
O2' C28' 1.28(2)
O2' H2' 0.84
C28' H28D 0.98
C28' H28E 0.98
C28' H28F 0.98
