#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:49:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179492 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/89/4338959.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_4338959
loop_
_publ_author_name
'Singh, Priti'
'Fiedler, Jan'
'Zális, Stanislav'
'Duboc, Carole'
'Niemeyer, Mark'
'Lissner, Falk'
'Schleid, Thomas'
'Kaim, Wolfgang'
_publ_section_title
;
 Spectroelectrochemistry and DFT analysis of a new {RuNO}n redox system
 with multifrequency EPR suggesting conformational isomerism in the
 {RuNO}7 state.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9254
_journal_page_last               9261
_journal_paper_doi               10.1021/ic701206a
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C23 H17 F6 N8 O2 P Ru'
_chemical_formula_weight         683.49
_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                 95.216(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9165(17)
_cell_length_b                   15.8829(19)
_cell_length_c                   19.321(3)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      5.1
_cell_volume                     2724.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5651
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.6544
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0534
_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)+(0.0593P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                2898
_reflns_number_total             5303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701206a-file004.cif
_cod_data_source_block           sin02
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4338959
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
Ru Ru 1.38464(6) -0.21106(3) 1.09950(2) 0.02452(15) Uani 1 1 d .
N1 N 1.2904(6) -0.1898(3) 1.0012(2) 0.0303(13) Uani 1 1 d .
O1 O 1.2020(5) -0.1285(3) 0.9884(2) 0.0372(11) Uani 1 1 d .
O2 O 1.3262(6) -0.2336(3) 0.9518(2) 0.0475(14) Uani 1 1 d .
N2 N 1.4109(6) -0.0887(3) 1.1140(2) 0.0261(12) Uani 1 1 d .
N3 N 1.1836(6) -0.1835(3) 1.1413(2) 0.0245(12) Uani 1 1 d .
N4 N 1.5910(6) -0.1913(3) 1.0613(3) 0.0313(13) Uani 1 1 d .
N5 N 1.4751(6) -0.2439(3) 1.1983(2) 0.0271(12) Uani 1 1 d .
N6 N 1.3592(6) -0.3419(3) 1.0983(3) 0.0315(14) Uani 1 1 d .
N7 N 1.4989(7) -0.3573(3) 1.2798(3) 0.0365(14) Uani 1 1 d .
N8 N 1.3596(7) -0.4597(3) 1.1771(3) 0.0413(15) Uani 1 1 d .
C1 C 1.2988(8) -0.0458(4) 1.1426(3) 0.0280(15) Uani 1 1 d .
C2 C 1.3162(8) 0.0400(4) 1.1554(3) 0.0352(17) Uani 1 1 d .
H2A H 1.2412 0.0707 1.1765 0.047(5) Uiso 1 1 calc R
C3 C 1.4443(9) 0.0797(4) 1.1368(3) 0.0411(18) Uani 1 1 d .
H3A H 1.4574 0.1383 1.1452 0.047(5) Uiso 1 1 calc R
C4 C 1.5509(9) 0.0359(4) 1.1070(3) 0.0398(18) Uani 1 1 d .
H4A H 1.6390 0.0635 1.0945 0.047(5) Uiso 1 1 calc R
C5 C 1.5314(8) -0.0501(4) 1.0945(3) 0.0317(16) Uani 1 1 d .
C6 C 1.1677(7) -0.1001(4) 1.1582(3) 0.0267(14) Uani 1 1 d .
C7 C 1.0468(8) -0.0707(4) 1.1885(3) 0.0346(16) Uani 1 1 d .
H7A H 1.0380 -0.0123 1.1979 0.047(5) Uiso 1 1 calc R
C8 C 0.9371(9) -0.1256(5) 1.2057(4) 0.0448(19) Uani 1 1 d .
H8A H 0.8537 -0.1065 1.2287 0.047(5) Uiso 1 1 calc R
C9 C 0.9518(8) -0.2104(5) 1.1883(3) 0.0425(17) Uani 1 1 d .
H9A H 0.8764 -0.2499 1.1979 0.047(5) Uiso 1 1 calc R
C10 C 1.0770(8) -0.2363(4) 1.1569(3) 0.0325(16) Uani 1 1 d .
H10A H 1.0871 -0.2943 1.1462 0.047(5) Uiso 1 1 calc R
C11 C 1.6360(8) -0.1083(4) 1.0622(3) 0.0370(17) Uani 1 1 d .
C12 C 1.7674(8) -0.0823(5) 1.0340(4) 0.046(2) Uani 1 1 d .
H12A H 1.7956 -0.0246 1.0346 0.047(5) Uiso 1 1 calc R
C13 C 1.8552(9) -0.1421(6) 1.0053(4) 0.057(2) Uani 1 1 d .
H13A H 1.9444 -0.1254 0.9856 0.047(5) Uiso 1 1 calc R
C14 C 1.8140(8) -0.2266(5) 1.0049(4) 0.048(2) Uani 1 1 d .
H14A H 1.8749 -0.2682 0.9858 0.047(5) Uiso 1 1 calc R
C15 C 1.6818(8) -0.2486(5) 1.0330(3) 0.0406(18) Uani 1 1 d .
H15A H 1.6531 -0.3062 1.0325 0.047(5) Uiso 1 1 calc R
C16 C 1.4570(7) -0.3254(4) 1.2171(3) 0.0274(15) Uani 1 1 d .
C17 C 1.5478(8) -0.1930(4) 1.2473(3) 0.0334(16) Uani 1 1 d .
H17A H 1.5648 -0.1356 1.2364 0.047(5) Uiso 1 1 calc R
C18 C 1.5970(8) -0.2232(4) 1.3122(3) 0.0360(16) Uani 1 1 d .
H18A H 1.6478 -0.1877 1.3463 0.047(5) Uiso 1 1 calc R
C19 C 1.5698(7) -0.3070(4) 1.3259(3) 0.0328(16) Uani 1 1 d .
H19A H 1.6037 -0.3291 1.3703 0.047(5) Uiso 1 1 calc R
C20 C 1.3881(8) -0.3798(4) 1.1613(3) 0.0297(15) Uani 1 1 d .
C21 C 1.3022(8) -0.3927(4) 1.0461(3) 0.0387(17) Uani 1 1 d .
H21A H 1.2833 -0.3703 1.0006 0.047(5) Uiso 1 1 calc R
C22 C 1.2713(10) -0.4756(4) 1.0573(4) 0.053(2) Uani 1 1 d .
H22A H 1.2309 -0.5108 1.0205 0.047(5) Uiso 1 1 calc R
C23 C 1.3005(11) -0.5064(5) 1.1236(4) 0.059(2) Uani 1 1 d .
H23A H 1.2776 -0.5638 1.1320 0.047(5) Uiso 1 1 calc R
P P 1.8392(3) -0.46298(12) 1.14866(11) 0.0474(5) Uani 1 1 d .
F1 F 1.8888(6) -0.4100(3) 1.0846(2) 0.0755(15) Uani 1 1 d .
F2 F 1.7528(6) -0.3854(3) 1.1746(3) 0.0884(18) Uani 1 1 d .
F3 F 1.6895(7) -0.4890(5) 1.1055(3) 0.136(3) Uani 1 1 d .
F4 F 1.7932(7) -0.5148(3) 1.2130(3) 0.106(2) Uani 1 1 d .
F5 F 1.9174(9) -0.5405(3) 1.1181(4) 0.146(3) Uani 1 1 d .
F6 F 1.9889(6) -0.4331(5) 1.1888(3) 0.107(2) Uani 1 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'
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
N2 Ru N1 90.18(19)
N2 Ru N4 78.7(2)
N1 Ru N4 87.0(2)
N2 Ru N5 94.93(19)
N1 Ru N5 174.8(2)
N4 Ru N5 94.7(2)
N2 Ru N3 80.4(2)
N1 Ru N3 91.8(2)
N4 Ru N3 159.01(19)
N5 Ru N3 88.41(19)
N2 Ru N6 172.50(19)
N1 Ru N6 96.8(2)
N4 Ru N6 104.2(2)
N5 Ru N6 78.0(2)
N3 Ru N6 96.7(2)
O2 N1 O1 118.6(5)
O2 N1 Ru 120.7(4)
O1 N1 Ru 120.6(4)
C5 N2 C1 121.9(5)
C5 N2 Ru 120.3(5)
C1 N2 Ru 117.8(4)
C10 N3 C6 117.7(6)
C10 N3 Ru 128.2(4)
C6 N3 Ru 114.0(4)
C15 N4 C11 117.5(6)
C15 N4 Ru 128.4(5)
C11 N4 Ru 114.1(5)
C16 N5 C17 116.1(5)
C16 N5 Ru 116.2(4)
C17 N5 Ru 127.7(4)
C21 N6 C20 115.4(5)
C21 N6 Ru 129.4(4)
C20 N6 Ru 114.7(4)
C19 N7 C16 117.5(5)
C20 N8 C23 114.7(6)
N2 C1 C2 119.0(6)
N2 C1 C6 113.9(5)
C2 C1 C6 127.0(6)
C3 C2 C1 118.9(7)
C4 C3 C2 120.5(6)
C3 C4 C5 119.8(7)
N2 C5 C4 119.7(7)
N2 C5 C11 112.9(6)
C4 C5 C11 127.4(7)
C7 C6 N3 122.5(6)
C7 C6 C1 123.5(6)
N3 C6 C1 114.0(6)
C6 C7 C8 119.9(6)
C7 C8 C9 118.0(7)
C10 C9 C8 119.3(7)
N3 C10 C9 122.6(6)
N4 C11 C12 122.0(7)
N4 C11 C5 114.0(6)
C12 C11 C5 123.9(7)
C13 C12 C11 118.7(7)
C12 C13 C14 120.5(7)
C15 C14 C13 118.3(7)
N4 C15 C14 123.0(7)
N7 C16 N5 125.1(6)
N7 C16 C20 120.5(6)
N5 C16 C20 114.4(5)
N5 C17 C18 121.2(6)
C17 C18 C19 117.6(6)
N7 C19 C18 122.5(6)
N8 C20 N6 126.9(6)
N8 C20 C16 117.7(5)
N6 C20 C16 115.4(5)
N6 C21 C22 121.6(6)
C21 C22 C23 117.9(6)
N8 C23 C22 123.3(7)
F6 P F5 92.1(4)
F6 P F2 91.4(4)
F5 P F2 176.0(4)
F6 P F3 176.9(4)
F5 P F3 88.8(5)
F2 P F3 87.6(4)
F6 P F4 92.3(4)
F5 P F4 92.5(3)
F2 P F4 89.3(3)
F3 P F4 90.7(4)
F6 P F1 86.6(3)
F5 P F1 87.6(3)
F2 P F1 90.7(3)
F3 P F1 90.5(4)
F4 P F1 178.8(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru N2 1.975(5)
Ru N1 2.034(5)
Ru N4 2.068(5)
Ru N5 2.070(5)
Ru N3 2.079(5)
Ru N6 2.090(5)
N1 O2 1.246(6)
N1 O1 1.264(6)
N2 C5 1.321(8)
N2 C1 1.366(8)
N3 C10 1.322(8)
N3 C6 1.375(7)
N4 C15 1.365(8)
N4 C11 1.378(8)
N5 C16 1.359(7)
N5 C17 1.364(7)
N6 C21 1.354(7)
N6 C20 1.362(7)
N7 C19 1.314(8)
N7 C16 1.334(7)
N8 C20 1.336(7)
N8 C23 1.341(9)
C1 C2 1.391(8)
C1 C6 1.504(9)
C2 C3 1.380(9)
C3 C4 1.349(10)
C4 C5 1.395(9)
C5 C11 1.489(9)
C6 C7 1.356(9)
C7 C8 1.372(9)
C8 C9 1.397(10)
C9 C10 1.380(9)
C11 C12 1.399(9)
C12 C13 1.379(11)
C13 C14 1.392(11)
C14 C15 1.387(10)
C16 C20 1.471(8)
C17 C18 1.376(8)
C18 C19 1.383(8)
C21 C22 1.366(9)
C22 C23 1.374(10)
P F6 1.555(6)
P F5 1.557(6)
P F2 1.561(5)
P F3 1.564(6)
P F4 1.575(5)
P F1 1.592(5)
