#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:21:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179839 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/35/7013572.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_7013572
loop_
_publ_author_name
'Bonnet, Sylvestre'
'Collin, Jean-Paul'
'Gruber, Nathalie'
'Sauvage, Jean-Pierre'
'Schofield, Emma R.'
_publ_section_title
;
 Photochemical and thermal synthesis and characterization of
 polypyridine ruthenium(ii) complexes containing different monodentate
 ligandsElectronic supplementary information (ESI) available: View of
 the dimeric units of 8 and proton indexation used in the 1H NMR data.
 See http://www.rsc.org/suppdata/dt/b3/b310198c/
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4654
_journal_paper_doi               10.1039/b310198c
_journal_year                    2003
_chemical_formula_moiety         'C31 H25 Cl F6 N7 P Ru'
_chemical_formula_structural     '[Ru(terpy)(phen)(Cl][PF6]'
_chemical_formula_sum            'C31 H25 Cl F6 N7 P Ru'
_chemical_formula_weight         777.08
_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'
_cell_angle_alpha                80.973(8)
_cell_angle_beta                 80.067(8)
_cell_angle_gamma                85.708(8)
_cell_formula_units_Z            2
_cell_length_a                   8.8775(4)
_cell_length_b                   12.0354(5)
_cell_length_c                   15.3203(6)
_cell_measurement_reflns_used    7235
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1590.46(13)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
7235 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  2.0 deg 1 scans of   20 sec per frame.
Data collection was divided into  5 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.40 Omega =    0.00 Kappa =    0.00   91 frames
Set 2 Theta =   -3.40 Kappa = -172.00 Phi   =    0.00   22 frames
Set 3 Theta =   -5.50 Kappa = -167.00 Phi   =    0.00   20 frames
Set 4 Theta =   -6.40 Kappa =  112.00 Phi   =    0.00   14 frames
Set 5 Theta =   -6.40 Kappa =  -74.00 Phi   =    0.00   29 frames
Friedel pairs were averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7235
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.700
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.124
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                5225
_reflns_number_total             7235
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            b310198c.txt
_cod_data_source_block           st532
_cod_original_cell_volume        1590.5(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013572
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
RU 0.32302(3) 0.06609(2) 0.79408(2) 0.0198(1) Uani ? ? Ru
CL 0.38164(9) 0.12318(6) 0.92844(5) 0.0267(3) Uani ? ? Cl
N1 0.4288(3) 0.2036(2) 0.7097(2) 0.022(1) Uani ? ? N
C1 0.4994(3) 0.2868(2) 0.7315(2) 0.027(2) Uani ? ? C
C2 0.5671(4) 0.3734(2) 0.6663(2) 0.031(2) Uani ? ? C
C3 0.5621(4) 0.3732(2) 0.5779(2) 0.029(2) Uani ? ? C
C4 0.4870(3) 0.2863(2) 0.5528(2) 0.026(1) Uani ? ? C
C5 0.4718(4) 0.2786(3) 0.4617(2) 0.035(2) Uani ? ? C
C6 0.3996(4) 0.1917(3) 0.4420(2) 0.036(2) Uani ? ? C
C7 0.3348(4) 0.1055(3) 0.5112(2) 0.031(2) Uani ? ? C
C8 0.2588(4) 0.0123(3) 0.4959(2) 0.038(2) Uani ? ? C
C9 0.2061(4) -0.0669(2) 0.5659(2) 0.036(2) Uani ? ? C
C10 0.2214(4) -0.0546(2) 0.6529(2) 0.030(2) Uani ? ? C
N2 0.2903(3) 0.0334(2) 0.6714(2) 0.023(1) Uani ? ? N
C11 0.3468(3) 0.1125(2) 0.6000(2) 0.025(1) Uani ? ? C
C12 0.4219(3) 0.2038(2) 0.6210(2) 0.024(1) Uani ? ? C
N3 0.5079(3) -0.0500(2) 0.7940(2) 0.023(1) Uani ? ? N
C13 0.6567(3) -0.0333(2) 0.7579(2) 0.028(2) Uani ? ? C
C14 0.7687(4) -0.1206(3) 0.7593(2) 0.033(2) Uani ? ? C
C15 0.7285(4) -0.2275(3) 0.7988(2) 0.037(2) Uani ? ? C
C16 0.5782(4) -0.2457(2) 0.8375(2) 0.034(2) Uani ? ? C
C17 0.4685(4) -0.1558(2) 0.8345(2) 0.026(1) Uani ? ? C
C18 0.3057(3) -0.1661(2) 0.8729(2) 0.023(1) Uani ? ? C
C19 0.2350(4) -0.2633(2) 0.9167(2) 0.029(2) Uani ? ? C
C20 0.0775(4) -0.2584(2) 0.9468(2) 0.031(2) Uani ? ? C
C21 -0.0077(4) -0.1570(2) 0.9343(2) 0.028(1) Uani ? ? C
C22 0.0673(3) -0.0610(2) 0.8904(2) 0.022(1) Uani ? ? C
N4 0.2216(3) -0.0680(2) 0.8611(2) 0.022(1) Uani ? ? N
C23 -0.0017(3) 0.0531(2) 0.8696(2) 0.022(1) Uani ? ? C
N5 0.0993(3) 0.1320(2) 0.8232(1) 0.022(1) Uani ? ? N
C24 0.0449(3) 0.2392(2) 0.8045(2) 0.026(1) Uani ? ? C
C25 -0.1062(4) 0.2723(2) 0.8293(2) 0.031(2) Uani ? ? C
C26 -0.2090(4) 0.1940(3) 0.8740(2) 0.032(2) Uani ? ? C
C27 -0.1562(3) 0.0822(2) 0.8948(2) 0.027(1) Uani ? ? C
P 0.1279(1) -0.41288(6) 0.70599(6) 0.0329(4) Uani ? ? P
F1 0.1984(3) -0.5348(2) 0.6998(3) 0.083(2) Uani ? ? F
F2 0.0598(3) -0.2897(2) 0.7113(2) 0.078(2) Uani ? ? F
F3 0.2825(3) -0.3789(2) 0.7306(2) 0.071(1) Uani ? ? F
F4 -0.0271(3) -0.4461(2) 0.6806(2) 0.073(1) Uani ? ? F
F5 0.1953(3) -0.3764(3) 0.6029(2) 0.067(2) Uani ? ? F
F6 0.0575(3) -0.4460(2) 0.8079(2) 0.074(2) Uani ? ? F
C28 0.0228(5) 0.3339(3) 0.5544(3) 0.057(2) Uani ? ? C
C29 -0.0425(4) 0.2264(3) 0.5944(2) 0.045(2) Uani ? ? C
N6 -0.0938(4) 0.1431(3) 0.6251(2) 0.060(2) Uani ? ? N
C30 0.2828(5) -0.5858(3) 0.9532(3) 0.054(2) Uani ? ? C
C31 0.4446(4) -0.5649(3) 0.9204(2) 0.044(2) Uani ? ? C
N7 0.5689(4) -0.5485(3) 0.8952(2) 0.060(2) Uani ? ? N
H1 0.5045 0.2880 0.7928 0.0354 Uiso calc C1 H
H2 0.6160 0.4317 0.6842 0.0412 Uiso calc C2 H
H3 0.6084 0.4305 0.5338 0.0406 Uiso calc C3 H
H4 0.5128 0.3348 0.4147 0.0488 Uiso calc C5 H
H5 0.3920 0.1882 0.3814 0.0492 Uiso calc C6 H
H6 0.2449 0.0053 0.4369 0.0498 Uiso calc C8 H
H7 0.1587 -0.1307 0.5554 0.0464 Uiso calc C9 H
H8 0.1819 -0.1101 0.7009 0.0384 Uiso calc C10 H
H9 0.6852 0.0403 0.7309 0.0363 Uiso calc C13 H
H10 0.8719 -0.1066 0.7333 0.0432 Uiso calc C14 H
H11 0.8035 -0.2881 0.7993 0.0486 Uiso calc C15 H
H12 0.5495 -0.3187 0.8660 0.0444 Uiso calc C16 H
H13 0.2933 -0.3323 0.9260 0.0390 Uiso calc C19 H
H14 0.0281 -0.3247 0.9759 0.0407 Uiso calc C20 H
H15 -0.1148 -0.1532 0.9553 0.0365 Uiso calc C21 H
H16 0.1138 0.2942 0.7730 0.0344 Uiso calc C24 H
H17 -0.1397 0.3489 0.8155 0.0407 Uiso calc C25 H
H18 -0.3139 0.2156 0.8905 0.0417 Uiso calc C26 H
H19 -0.2248 0.0268 0.9257 0.0348 Uiso calc C27 H
H20 0.1036 0.3469 0.5843 0.0730 Uiso calc C28 H
H21 0.0615 0.3320 0.4928 0.0730 Uiso calc C28 H
H22 -0.0543 0.3927 0.5600 0.0730 Uiso calc C28 H
H23 0.2677 -0.6640 0.9584 0.0746 Uiso calc C30 H
H24 0.2535 -0.5618 1.0102 0.0746 Uiso calc C30 H
H25 0.2222 -0.5450 0.9123 0.0746 Uiso calc C30 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1
Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL RU N1 93.51(7) . . . ?
CL RU N2 172.82(7) . . . ?
CL RU N3 89.41(7) . . . ?
CL RU N4 92.56(7) . . . ?
CL RU N5 90.01(7) . . . ?
N1 RU N2 79.38(9) . . . ?
N1 RU N3 99.9(1) . . . ?
N1 RU N4 173.90(9) . . . ?
N1 RU N5 101.17(9) . . . ?
N2 RU N3 90.8(1) . . . ?
N2 RU N4 94.5(1) . . . ?
N2 RU N5 92.3(1) . . . ?
N3 RU N4 79.5(1) . . . ?
N3 RU N5 158.9(1) . . . ?
N4 RU N5 79.5(1) . . . ?
N1 RU N2 79.38(9) . . . ?
N1 RU N3 99.9(1) . . . ?
N1 RU N4 173.90(9) . . . ?
N1 RU N5 101.17(9) . . . ?
N2 RU N3 90.8(1) . . . ?
N2 RU N4 94.5(1) . . . ?
N2 RU N5 92.3(1) . . . ?
N3 RU N4 79.5(1) . . . ?
N3 RU N5 158.9(1) . . . ?
N4 RU N5 79.5(1) . . . ?
RU N1 C1 128.8(2) . . . ?
RU N1 C12 113.2(2) . . . ?
C1 N1 C12 118.0(3) . . . ?
N1 C1 C2 122.1(3) . . . ?
C1 C2 C3 120.0(3) . . . ?
C2 C3 C4 119.1(3) . . . ?
C3 C4 C5 124.1(3) . . . ?
C3 C4 C12 117.7(3) . . . ?
C5 C4 C12 118.3(3) . . . ?
C4 C5 C6 121.0(3) . . . ?
C5 C6 C7 121.3(3) . . . ?
C6 C7 C8 124.5(3) . . . ?
C6 C7 C11 118.4(3) . . . ?
C8 C7 C11 117.0(3) . . . ?
C7 C8 C9 119.9(3) . . . ?
C8 C9 C10 120.1(3) . . . ?
C9 C10 N2 122.4(3) . . . ?
RU N2 C10 128.1(2) . . . ?
RU N2 C11 114.6(2) . . . ?
C10 N2 C11 117.3(3) . . . ?
C7 C11 N2 123.2(3) . . . ?
C7 C11 C12 120.5(3) . . . ?
N2 C11 C12 116.3(3) . . . ?
N1 C12 C4 123.1(3) . . . ?
N1 C12 C11 116.4(3) . . . ?
C4 C12 C11 120.5(3) . . . ?
RU N3 C13 128.1(2) . . . ?
RU N3 C17 113.4(2) . . . ?
C13 N3 C17 118.5(3) . . . ?
N3 C13 C14 122.1(3) . . . ?
C13 C14 C15 119.4(3) . . . ?
C14 C15 C16 119.4(3) . . . ?
C15 C16 C17 119.6(3) . . . ?
N3 C17 C16 121.0(3) . . . ?
N3 C17 C18 115.0(3) . . . ?
C16 C17 C18 124.0(3) . . . ?
C17 C18 C19 126.9(3) . . . ?
C17 C18 N4 113.3(2) . . . ?
C19 C18 N4 119.8(3) . . . ?
C18 C19 C20 119.3(3) . . . ?
C19 C20 C21 120.5(3) . . . ?
C20 C21 C22 118.7(3) . . . ?
C21 C22 N4 119.8(3) . . . ?
C21 C22 C23 127.2(3) . . . ?
N4 C22 C23 113.1(2) . . . ?
RU N4 C18 118.8(2) . . . ?
RU N4 C22 119.1(2) . . . ?
C18 N4 C22 122.0(2) . . . ?
C22 C23 N5 114.9(3) . . . ?
C22 C23 C27 123.8(3) . . . ?
N5 C23 C27 121.3(3) . . . ?
RU N5 C23 113.4(2) . . . ?
RU N5 C24 128.5(2) . . . ?
C23 N5 C24 118.1(3) . . . ?
N5 C24 C25 122.7(3) . . . ?
C24 C25 C26 119.8(3) . . . ?
C25 C26 C27 118.9(3) . . . ?
C23 C27 C26 119.2(3) . . . ?
F1 P F2 179.0(2) . . . ?
F1 P F3 89.6(2) . . . ?
F1 P F4 90.7(2) . . . ?
F1 P F5 89.7(2) . . . ?
F1 P F6 91.9(2) . . . ?
F2 P F3 89.7(2) . . . ?
F2 P F4 90.0(2) . . . ?
F2 P F5 89.6(2) . . . ?
F2 P F6 88.8(2) . . . ?
F3 P F4 179.5(2) . . . ?
F3 P F5 88.7(1) . . . ?
F3 P F6 92.0(2) . . . ?
F4 P F5 90.9(2) . . . ?
F4 P F6 88.4(1) . . . ?
F5 P F6 178.3(2) . . . ?
C28 C29 N6 179.5(4) . . . ?
C30 C31 N7 180(1) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
RU CL 2.4180(8) . . ?
RU N1 2.105(2) . . ?
RU N2 2.051(3) . . ?
RU N3 2.074(3) . . ?
RU N4 1.961(2) . . ?
RU N5 2.084(3) . . ?
RU N1 2.105(2) . . ?
RU N2 2.051(3) . . ?
RU N3 2.074(3) . . ?
RU N4 1.961(2) . . ?
RU N5 2.084(3) . . ?
N1 C1 1.334(4) . . ?
N1 C12 1.370(4) . . ?
C1 C2 1.417(4) . . ?
C2 C3 1.363(5) . . ?
C3 C4 1.416(4) . . ?
C4 C5 1.442(5) . . ?
C4 C12 1.402(4) . . ?
C5 C6 1.364(5) . . ?
C6 C7 1.437(5) . . ?
C7 C8 1.421(5) . . ?
C7 C11 1.398(4) . . ?
C8 C9 1.360(5) . . ?
C9 C10 1.394(5) . . ?
C10 N2 1.353(4) . . ?
N2 C11 1.382(4) . . ?
C11 C12 1.433(4) . . ?
N3 C13 1.358(4) . . ?
N3 C17 1.368(4) . . ?
C13 C14 1.391(5) . . ?
C14 C15 1.378(5) . . ?
C15 C16 1.382(5) . . ?
C16 C17 1.401(4) . . ?
C17 C18 1.470(4) . . ?
C18 C19 1.389(4) . . ?
C18 N4 1.354(4) . . ?
C19 C20 1.394(5) . . ?
C20 C21 1.391(5) . . ?
C21 C22 1.396(4) . . ?
C22 N4 1.367(4) . . ?
C22 C23 1.471(4) . . ?
C23 N5 1.380(4) . . ?
C23 C27 1.393(4) . . ?
N5 C24 1.349(4) . . ?
C24 C25 1.376(5) . . ?
C25 C26 1.379(5) . . ?
C26 C27 1.397(5) . . ?
P F1 1.562(3) . . ?
P F2 1.567(3) . . ?
P F3 1.582(3) . . ?
P F4 1.587(3) . . ?
P F5 1.594(3) . . ?
P F6 1.579(3) . . ?
C28 C29 1.457(6) . . ?
C29 N6 1.132(5) . . ?
C30 C31 1.465(6) . . ?
C31 N7 1.125(5) . . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
