#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:29:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179898 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/94/7019478.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_7019478
loop_
_publ_author_name
'Merkle, Anna C.'
'McQuarters, Ashley B.'
'Lehnert, Nicolai'
_publ_section_title
;
 Synthesis, spectroscopic analysis and photolabilization of water-soluble
 ruthenium(iii)-nitrosyl complexes.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8047
_journal_page_last               8059
_journal_paper_doi               10.1039/c2dt30464c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C18 H18 N6 O3 Ru, 2(F6 P)'
_chemical_formula_sum            'C18 H18 F12 N6 O3 P2 Ru'
_chemical_formula_weight         757.39
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.313(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3726(3)
_cell_length_b                   9.9439(2)
_cell_length_c                   17.3570(12)
_cell_measurement_reflns_used    32688
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      2.80
_cell_volume                     2575.2(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn744+ CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39910
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         3.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.272
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0303P)²+15.0335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                4482
_reflns_number_total             4645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30464c.txt
_cod_data_source_block           am163
_cod_original_cell_volume        2575.2(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7019478
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ru1 Ru 0.292383(18) 0.35843(3) 0.106350(18) 0.02238(7) Uani 1 1 d .
P1 P 0.64514(6) 0.20354(10) 0.05809(6) 0.0238(2) Uani 1 1 d .
P2 P 0.49955(6) 0.88951(10) 0.35253(6) 0.0238(2) Uani 1 1 d .
F1 F 0.55988(16) 0.1369(3) -0.01531(16) 0.0380(7) Uani 1 1 d .
F2 F 0.70115(14) 0.0677(2) 0.06453(15) 0.0317(6) Uani 1 1 d .
F3 F 0.67854(16) 0.2614(3) -0.01026(14) 0.0359(6) Uani 1 1 d .
F4 F 0.73109(15) 0.2672(3) 0.13235(14) 0.0332(6) Uani 1 1 d .
F5 F 0.58914(17) 0.3368(3) 0.05172(18) 0.0404(6) Uani 1 1 d .
F6 F 0.61386(15) 0.1434(3) 0.12793(15) 0.0354(6) Uani 1 1 d .
F7 F 0.45479(17) 0.7489(3) 0.35395(16) 0.0383(6) Uani 1 1 d .
F8 F 0.46364(18) 0.8820(3) 0.25189(15) 0.0389(7) Uani 1 1 d .
F9 F 0.59023(16) 0.8152(3) 0.36225(17) 0.0431(7) Uani 1 1 d .
F10 F 0.54640(16) 1.0319(3) 0.35220(15) 0.0359(6) Uani 1 1 d .
F11 F 0.53821(17) 0.8998(3) 0.45376(15) 0.0389(6) Uani 1 1 d .
F12 F 0.41143(16) 0.9663(3) 0.34447(19) 0.0464(7) Uani 1 1 d .
N1 N 0.2365(2) 0.5138(3) 0.0989(2) 0.0281(8) Uani 1 1 d .
N2 N 0.2998(3) 0.3791(5) 0.2812(3) 0.0501(11) Uani 1 1 d .
N3 N 0.1851(2) 0.2288(3) 0.0449(2) 0.0263(7) Uani 1 1 d .
N4 N 0.3686(3) 0.1788(4) 0.1168(3) 0.0340(11) Uani 1 1 d .
N5 N 0.4227(2) 0.4277(3) 0.17132(19) 0.0235(7) Uani 1 1 d .
N6 N 0.2965(2) 0.3658(3) -0.0124(2) 0.0242(7) Uani 1 1 d .
O1 O 0.2056(2) 0.6168(3) 0.0943(2) 0.0368(8) Uani 1 1 d .
O2 O 0.2941(2) 0.2974(3) 0.21859(18) 0.0373(7) Uani 1 1 d .
O3 O 0.3008(2) 0.4953(4) 0.2672(2) 0.0544(10) Uani 1 1 d .
C1 C 0.1010(3) 0.2639(5) -0.0033(2) 0.0289(9) Uani 1 1 d .
H1A H 0.0835 0.3554 -0.0053 0.035 Uiso 1 1 calc R
C2 C 0.0395(3) 0.1707(5) -0.0500(3) 0.0320(10) Uani 1 1 d .
H2A H -0.0205 0.1978 -0.0831 0.038 Uiso 1 1 calc R
C3 C 0.0632(3) 0.0380(4) -0.0497(3) 0.0299(9) Uani 1 1 d .
H3A H 0.0209 -0.0264 -0.0836 0.036 Uiso 1 1 calc R
C4 C 0.1511(3) 0.0003(4) 0.0016(3) 0.0327(9) Uani 1 1 d .
H4A H 0.1692 -0.0910 0.0043 0.039 Uiso 1 1 calc R
C5 C 0.2122(3) 0.0989(4) 0.0491(2) 0.0260(9) Uani 1 1 d .
C6 C 0.3058(3) 0.0671(4) 0.1107(3) 0.0289(9) Uani 1 1 d .
H6A H 0.3063 0.0504 0.1671 0.035 Uiso 1 1 calc R
H6B H 0.3263 -0.0159 0.0926 0.035 Uiso 1 1 calc R
C7 C 0.4510(3) 0.5570(4) 0.1789(3) 0.0285(9) Uani 1 1 d .
H7A H 0.4092 0.6260 0.1509 0.034 Uiso 1 1 calc R
C8 C 0.5400(3) 0.5905(5) 0.2268(3) 0.0306(10) Uani 1 1 d .
H8A H 0.5591 0.6816 0.2319 0.037 Uiso 1 1 calc R
C9 C 0.6001(3) 0.4895(5) 0.2669(3) 0.0326(10) Uani 1 1 d .
H9A H 0.6612 0.5104 0.3003 0.039 Uiso 1 1 calc R
C10 C 0.5712(3) 0.3581(5) 0.2583(3) 0.0323(10) Uani 1 1 d .
H10A H 0.6123 0.2876 0.2852 0.039 Uiso 1 1 calc R
C11 C 0.4830(3) 0.3300(4) 0.2107(2) 0.0264(9) Uani 1 1 d .
C12 C 0.4460(3) 0.1889(4) 0.1989(3) 0.0289(9) Uani 1 1 d .
H12A H 0.4929 0.1242 0.2011 0.035 Uiso 1 1 calc R
H12B H 0.4275 0.1666 0.2449 0.035 Uiso 1 1 calc R
C13 C 0.2473(3) 0.4486(4) -0.0756(3) 0.0281(9) Uani 1 1 d .
H13A H 0.2174 0.5227 -0.0640 0.034 Uiso 1 1 calc R
C14 C 0.2394(3) 0.4280(5) -0.1572(3) 0.0342(10) Uani 1 1 d .
H14A H 0.2045 0.4877 -0.2012 0.041 Uiso 1 1 calc R
C15 C 0.2833(3) 0.3183(5) -0.1747(3) 0.0345(10) Uani 1 1 d .
H15A H 0.2780 0.3017 -0.2305 0.041 Uiso 1 1 calc R
C16 C 0.3342(3) 0.2357(5) -0.1088(3) 0.0294(9) Uani 1 1 d .
H16A H 0.3649 0.1611 -0.1186 0.035 Uiso 1 1 calc R
C17 C 0.3406(2) 0.2617(4) -0.0273(2) 0.0205(8) Uani 1 1 d .
C18 C 0.3998(2) 0.1821(4) 0.0469(2) 0.0251(9) Uani 1 1 d .
H18A H 0.4610 0.2207 0.0689 0.030 Uiso 1 1 calc R
H18B H 0.4033 0.0888 0.0285 0.030 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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 O2 97.67(15)
N1 Ru1 N5 97.73(14)
O2 Ru1 N5 88.45(12)
N1 Ru1 N3 101.62(14)
O2 Ru1 N3 88.95(13)
N5 Ru1 N3 160.66(13)
N1 Ru1 N6 97.03(15)
O2 Ru1 N6 164.43(13)
N5 Ru1 N6 94.62(12)
N3 Ru1 N6 83.09(12)
N1 Ru1 N4 175.82(16)
O2 Ru1 N4 83.82(16)
N5 Ru1 N4 78.38(14)
N3 Ru1 N4 82.29(14)
N6 Ru1 N4 81.87(15)
F5 P1 F1 90.04(14)
F5 P1 F4 90.97(14)
F1 P1 F4 178.83(15)
F5 P1 F3 90.68(15)
F1 P1 F3 90.63(14)
F4 P1 F3 89.95(13)
F5 P1 F2 179.50(15)
F1 P1 F2 89.61(13)
F4 P1 F2 89.38(13)
F3 P1 F2 89.68(14)
F5 P1 F6 90.52(15)
F1 P1 F6 90.11(14)
F4 P1 F6 89.29(13)
F3 P1 F6 178.58(14)
F2 P1 F6 89.12(14)
F7 P2 F12 90.93(15)
F7 P2 F8 90.66(14)
F12 P2 F8 90.81(16)
F7 P2 F9 90.33(15)
F12 P2 F9 178.44(16)
F8 P2 F9 90.09(15)
F7 P2 F11 90.89(14)
F12 P2 F11 90.03(16)
F8 P2 F11 178.23(16)
F9 P2 F11 89.04(15)
F7 P2 F10 179.17(15)
F12 P2 F10 89.65(15)
F8 P2 F10 89.92(14)
F9 P2 F10 89.08(15)
F11 P2 F10 88.52(14)
O1 N1 Ru1 175.7(3)
O3 N2 O2 115.6(4)
C1 N3 C5 120.9(3)
C1 N3 Ru1 126.5(3)
C5 N3 Ru1 111.9(2)
C12 N4 C6 114.5(4)
C12 N4 C18 109.7(4)
C6 N4 C18 114.5(4)
C12 N4 Ru1 105.3(3)
C6 N4 Ru1 104.8(3)
C18 N4 Ru1 107.1(3)
C11 N5 C7 118.9(3)
C11 N5 Ru1 114.1(3)
C7 N5 Ru1 126.9(3)
C13 N6 C17 120.3(4)
C13 N6 Ru1 125.0(3)
C17 N6 Ru1 113.5(3)
N2 O2 Ru1 124.8(3)
N3 C1 C2 121.0(4)
C1 C2 C3 120.8(4)
C2 C3 C4 118.4(4)
C3 C4 C5 119.1(4)
N3 C5 C4 119.7(3)
N3 C5 C6 117.1(3)
C4 C5 C6 123.0(4)
N4 C6 C5 111.5(3)
N5 C7 C8 121.3(4)
C9 C8 C7 118.8(4)
C10 C9 C8 119.7(4)
C11 C10 C9 119.4(4)
N5 C11 C10 121.9(4)
N5 C11 C12 115.5(3)
C10 C11 C12 122.6(4)
N4 C12 C11 109.5(3)
N6 C13 C14 121.1(4)
C13 C14 C15 119.7(4)
C16 C15 C14 118.1(4)
C15 C16 C17 119.9(4)
N6 C17 C16 120.9(3)
N6 C17 C18 117.1(3)
C16 C17 C18 122.0(4)
C17 C18 N4 113.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 N1 1.772(3)
Ru1 O2 2.030(3)
Ru1 N5 2.078(3)
Ru1 N3 2.083(3)
Ru1 N6 2.091(4)
Ru1 N4 2.143(4)
P1 F5 1.589(3)
P1 F1 1.596(2)
P1 F4 1.597(2)
P1 F3 1.604(3)
P1 F2 1.610(3)
P1 F6 1.613(3)
P2 F7 1.583(3)
P2 F12 1.587(3)
P2 F8 1.599(3)
P2 F9 1.604(3)
P2 F11 1.607(3)
P2 F10 1.612(3)
N1 O1 1.131(4)
N2 O3 1.182(6)
N2 O2 1.329(5)
N3 C1 1.332(5)
N3 C5 1.357(5)
N4 C12 1.470(5)
N4 C6 1.486(6)
N4 C18 1.498(6)
N5 C11 1.353(5)
N5 C7 1.355(5)
N6 C13 1.342(5)
N6 C17 1.346(5)
C1 C2 1.362(6)
C2 C3 1.375(6)
C3 C4 1.396(6)
C4 C5 1.401(6)
C5 C6 1.497(5)
C7 C8 1.389(5)
C8 C9 1.377(6)
C9 C10 1.377(7)
C10 C11 1.366(6)
C11 C12 1.507(6)
C13 C14 1.384(6)
C14 C15 1.407(7)
C15 C16 1.376(6)
C16 C17 1.399(6)
C17 C18 1.482(5)
