#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/79/4327986.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_4327986
loop_
_publ_author_name
'Michael I. Webb'
'Ryan A. Chard'
'Yaser M. Al-Jobory'
'Michael R. Jones'
'Edwin W. Y. Wong'
'Charles J. Walsby'
_publ_contact_author_address
; 
Walsby, Charles J.
Department of Chemistry
Simon Fraser University
Burnaby, British Columbia
Canada         V5A 1S6
;
_publ_contact_author_email       cwalsby@sfu.ca
_publ_contact_author_fax         +1-778-782-3765
_publ_contact_author_name        'Charles J. Walsby'
_publ_contact_author_phone       +1-778-782-4607
_publ_section_title
;
 Pyridine Analogues of the Antimetastatic Ru(III) Complex NAMI-A Targeting
 Non-Covalent Interactions with Albumin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              954
_journal_page_last               966
_journal_paper_doi               10.1021/ic202029e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C18 H24 Cl4 N2 Na1 O5 Ru1 S1'
_chemical_formula_sum            'C18 H24 Cl4 N2 Na O5 Ru S'
_chemical_formula_weight         646.34
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                99.8050(10)
_cell_angle_beta                 90.6560(10)
_cell_angle_gamma                96.2220(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9223(2)
_cell_length_b                   9.7239(2)
_cell_length_c                   14.8391(4)
_cell_measurement_reflns_used    5879
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.30
_cell_volume                     1260.57(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution
; 
SIR92 (Altomare et al, 1994)
CRYSTALS (Watkin, 1988) 
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.773
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9585
_diffrn_reflns_theta_full        25.207
_diffrn_reflns_theta_max         25.721
_diffrn_reflns_theta_min         1.393
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6515
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0504
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2654
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0009493
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.418 0.483 0.398 0.215 0.884E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0453
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0284
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2773
_reflns_number_total             3708
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.35
_oxford_diffrn_Wilson_scale      85.71
_oxford_refine_ls_r_factor_ref   0.0348
_oxford_refine_ls_scale          0.10936(12)
_oxford_reflns_number_all        3708
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic202029e_si_002_7.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C18 H24 Cl4 N2 Na1 O5 Ru1 S1'
_cod_database_code               4327986
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
Ru1 Ru 0.16424(5) 0.83017(5) 0.66294(3) 0.0258 1.0000 Uani .
Cl1 Cl 0.02957(16) 0.69580(14) 0.75940(9) 0.0402 1.0000 Uani .
Cl2 Cl 0.01241(17) 0.71696(16) 0.53725(9) 0.0461 1.0000 Uani .
Cl3 Cl 0.30850(16) 0.96164(14) 0.57000(8) 0.0384 1.0000 Uani .
Cl4 Cl 0.32101(14) 0.93919(14) 0.79043(8) 0.0323 1.0000 Uani .
Na1 Na 0.0817(2) 0.9160(2) 0.90642(13) 0.0408 1.0000 Uani .
S1 S 0.00563(16) 0.99870(14) 0.70276(8) 0.0349 1.0000 Uani .
O1 O 0.7497(5) 0.1549(5) 0.9824(3) 0.0584 1.0000 Uani .
O2 O 0.9017(5) 0.3453(5) 0.9960(3) 0.0597 1.0000 Uani .
O21 O -0.0283(4) 1.0291(4) 0.8009(2) 0.0412 1.0000 Uani .
O31 O 0.1397(4) 1.1368(4) 1.0082(2) 0.0437 1.0000 Uani .
O32 O 0.3262(5) 1.3084(4) 0.9941(3) 0.0573 1.0000 Uani .
N1 N 0.3092(4) 0.6699(4) 0.6348(2) 0.0235 1.0000 Uani .
N2 N 0.8028(6) 0.2607(6) 0.9544(3) 0.0446 1.0000 Uani .
C1 C 0.2547(6) 0.5353(5) 0.6136(3) 0.0295 1.0000 Uani .
C2 C 0.3471(6) 0.4282(5) 0.6002(3) 0.0326 1.0000 Uani .
C3 C 0.5012(6) 0.4595(5) 0.6108(3) 0.0284 1.0000 Uani .
C4 C 0.5559(6) 0.5993(5) 0.6302(3) 0.0317 1.0000 Uani .
C5 C 0.4591(6) 0.7025(5) 0.6429(3) 0.0286 1.0000 Uani .
C6 C 0.5801(6) 0.2171(5) 0.7367(4) 0.0335 1.0000 Uani .
C7 C 0.6286(6) 0.1976(5) 0.8225(3) 0.0336 1.0000 Uani .
C8 C 0.7480(6) 0.2835(5) 0.8656(3) 0.0290 1.0000 Uani .
C9 C 0.8207(6) 0.3915(6) 0.8276(4) 0.0389 1.0000 Uani .
C10 C 0.7728(6) 0.4068(6) 0.7406(4) 0.0393 1.0000 Uani .
C11 C 0.6534(6) 0.3215(5) 0.6951(3) 0.0326 1.0000 Uani .
C12 C 0.6032(6) 0.3432(6) 0.6012(3) 0.0366 1.0000 Uani .
C21 C -0.1677(7) 0.9619(8) 0.6425(4) 0.0750 1.0000 Uani .
C22 C 0.0722(9) 1.1616(6) 0.6718(4) 0.0762 1.0000 Uani .
C31 C 0.3436(9) 1.4548(7) 0.8793(5) 0.0698 1.0000 Uani .
C32 C 0.2532(8) 1.3301(7) 0.9095(4) 0.0633 1.0000 Uani .
C33 C 0.2555(7) 1.2091(7) 1.0364(4) 0.0467 1.0000 Uani .
C34 C 0.3392(8) 1.2006(8) 1.1227(4) 0.0737 1.0000 Uani .
H11 H 0.1498 0.5131 0.6073 0.029(4) 1.0000 Uiso R
H21 H 0.3057 0.3344 0.5845 0.030(4) 1.0000 Uiso R
H41 H 0.6601 0.6247 0.6355 0.031(4) 1.0000 Uiso R
H51 H 0.4988 0.7972 0.6573 0.026(4) 1.0000 Uiso R
H61 H 0.4978 0.1592 0.7068 0.034(4) 1.0000 Uiso R
H71 H 0.5802 0.1265 0.8499 0.035(4) 1.0000 Uiso R
H91 H 0.9000 0.4516 0.8590 0.040(4) 1.0000 Uiso R
H101 H 0.8222 0.4767 0.7127 0.040(4) 1.0000 Uiso R
H121 H 0.6912 0.3693 0.5672 0.036(4) 1.0000 Uiso R
H122 H 0.5476 0.2563 0.5696 0.036(4) 1.0000 Uiso R
H211 H -0.1514 0.9414 0.5780 0.111(12) 1.0000 Uiso R
H212 H -0.2239 1.0414 0.6555 0.111(12) 1.0000 Uiso R
H213 H -0.2233 0.8820 0.6613 0.111(12) 1.0000 Uiso R
H221 H 0.0961 1.1479 0.6083 0.111(12) 1.0000 Uiso R
H222 H -0.0034 1.2251 0.6827 0.111(12) 1.0000 Uiso R
H223 H 0.1613 1.2002 0.7083 0.111(12) 1.0000 Uiso R
H311 H 0.4439 1.4328 0.8662 0.08(2) 1.0000 Uiso R
H312 H 0.3484 1.5336 0.9282 0.11(3) 1.0000 Uiso R
H313 H 0.2969 1.4780 0.8265 0.155(15) 1.0000 Uiso R
H321 H 0.1501 1.3503 0.9210 0.132(15) 1.0000 Uiso R
H322 H 0.2541 1.2468 0.8632 0.133(15) 1.0000 Uiso R
H341 H 0.4364 1.2552 1.1240 0.159(15) 1.0000 Uiso R
H342 H 0.2815 1.2370 1.1735 0.159(15) 1.0000 Uiso R
H343 H 0.3515 1.1039 1.1231 0.159(15) 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928
5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Ru1 Cl2 . 90.93(6) yes
Cl1 . Ru1 Cl3 . 177.37(6) yes
Cl2 . Ru1 Cl3 . 90.88(6) yes
Cl1 . Ru1 Cl4 . 88.52(5) yes
Cl2 . Ru1 Cl4 . 178.45(6) yes
Cl3 . Ru1 Cl4 . 89.63(5) yes
Cl1 . Ru1 S1 . 88.07(5) yes
Cl2 . Ru1 S1 . 93.30(5) yes
Cl3 . Ru1 S1 . 93.74(5) yes
Cl4 . Ru1 S1 . 88.13(5) yes
Cl1 . Ru1 N1 . 88.56(11) yes
Cl2 . Ru1 N1 . 88.67(11) yes
Cl3 . Ru1 N1 . 89.58(11) yes
Cl4 . Ru1 N1 . 89.86(11) yes
S1 . Ru1 N1 . 176.12(11) yes
Ru1 . Cl1 Na1 . 90.85(6) yes
Ru1 . Cl4 Na1 . 90.79(6) yes
O31 2_577 Na1 O1 2_667 92.74(15) yes
O31 2_577 Na1 Cl4 . 171.31(13) yes
O1 2_667 Na1 Cl4 . 89.45(12) yes
O31 2_577 Na1 Cl1 . 98.59(12) yes
O1 2_667 Na1 Cl1 . 108.08(13) yes
Cl4 . Na1 Cl1 . 72.74(6) yes
O31 2_577 Na1 Na1 2_577 45.05(10) yes
O1 2_667 Na1 Na1 2_577 84.95(12) yes
Cl4 . Na1 Na1 2_577 143.61(12) yes
Cl1 . Na1 Na1 2_577 142.84(11) yes
O31 2_577 Na1 O21 . 98.46(15) yes
O1 2_667 Na1 O21 . 165.27(18) yes
Cl4 . Na1 O21 . 80.90(10) yes
Cl1 . Na1 O21 . 79.76(11) yes
Na1 2_577 Na1 O21 . 96.20(12) yes
O31 2_577 Na1 O31 . 90.27(15) yes
O1 2_667 Na1 O31 . 80.08(15) yes
Cl4 . Na1 O31 . 98.40(12) yes
Cl1 . Na1 O31 . 167.51(13) yes
Na1 2_577 Na1 O31 . 45.22(10) yes
O21 . Na1 O31 . 90.29(15) yes
Ru1 . S1 O21 . 115.64(15) yes
Ru1 . S1 C21 . 113.2(2) yes
O21 . S1 C21 . 106.8(3) yes
Ru1 . S1 C22 . 113.0(2) yes
O21 . S1 C22 . 106.2(3) yes
C21 . S1 C22 . 100.7(4) yes
Na1 2_667 O1 N2 . 112.6(4) yes
Na1 . O21 S1 . 121.1(2) yes
Na1 . O31 Na1 2_577 89.73(15) yes
Na1 . O31 C33 . 134.4(4) yes
Na1 2_577 O31 C33 . 127.5(4) yes
C32 . O32 C33 . 116.1(5) yes
Ru1 . N1 C1 . 121.4(3) yes
Ru1 . N1 C5 . 120.1(3) yes
C1 . N1 C5 . 118.5(4) yes
O1 . N2 O2 . 123.1(5) yes
O1 . N2 C8 . 118.0(5) yes
O2 . N2 C8 . 118.9(5) yes
N1 . C1 C2 . 122.4(5) yes
N1 . C1 H11 . 118.2 no
C2 . C1 H11 . 119.4 no
C1 . C2 C3 . 120.0(5) yes
C1 . C2 H21 . 120.6 no
C3 . C2 H21 . 119.4 no
C2 . C3 C4 . 116.8(5) yes
C2 . C3 C12 . 120.6(5) yes
C4 . C3 C12 . 122.6(5) yes
C3 . C4 C5 . 121.0(5) yes
C3 . C4 H41 . 119.3 no
C5 . C4 H41 . 119.7 no
C4 . C5 N1 . 121.3(5) yes
C4 . C5 H51 . 119.6 no
N1 . C5 H51 . 119.1 no
C7 . C6 C11 . 120.5(5) yes
C7 . C6 H61 . 119.7 no
C11 . C6 H61 . 119.8 no
C6 . C7 C8 . 119.1(5) yes
C6 . C7 H71 . 120.3 no
C8 . C7 H71 . 120.5 no
N2 . C8 C7 . 119.4(5) yes
N2 . C8 C9 . 118.6(5) yes
C7 . C8 C9 . 122.0(5) yes
C8 . C9 C10 . 117.8(5) yes
C8 . C9 H91 . 120.9 no
C10 . C9 H91 . 121.2 no
C9 . C10 C11 . 121.6(5) yes
C9 . C10 H101 . 119.4 no
C11 . C10 H101 . 119.0 no
C6 . C11 C10 . 118.9(5) yes
C6 . C11 C12 . 121.2(5) yes
C10 . C11 C12 . 119.9(5) yes
C3 . C12 C11 . 109.7(4) yes
C3 . C12 H121 . 109.3 no
C11 . C12 H121 . 109.3 no
C3 . C12 H122 . 109.3 no
C11 . C12 H122 . 108.7 no
H121 . C12 H122 . 110.6 no
S1 . C21 H211 . 109.9 no
S1 . C21 H212 . 109.6 no
H211 . C21 H212 . 109.5 no
S1 . C21 H213 . 108.9 no
H211 . C21 H213 . 109.5 no
H212 . C21 H213 . 109.5 no
S1 . C22 H221 . 109.7 no
S1 . C22 H222 . 110.0 no
H221 . C22 H222 . 109.5 no
S1 . C22 H223 . 108.7 no
H221 . C22 H223 . 109.5 no
H222 . C22 H223 . 109.5 no
C32 . C31 H311 . 109.4 no
C32 . C31 H312 . 108.7 no
H311 . C31 H312 . 108.8 no
C32 . C31 H313 . 110.5 no
H311 . C31 H313 . 110.2 no
H312 . C31 H313 . 109.2 no
C31 . C32 O32 . 106.8(5) yes
C31 . C32 H321 . 110.0 no
O32 . C32 H321 . 110.0 no
C31 . C32 H322 . 110.3 no
O32 . C32 H322 . 109.6 no
H321 . C32 H322 . 110.2 no
O32 . C33 O31 . 124.5(5) yes
O32 . C33 C34 . 110.6(6) yes
O31 . C33 C34 . 124.9(6) yes
C33 . C34 H341 . 108.8 no
C33 . C34 H342 . 108.4 no
H341 . C34 H342 . 110.6 no
C33 . C34 H343 . 108.2 no
H341 . C34 H343 . 110.2 no
H342 . C34 H343 . 110.6 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 Cl1 . 2.3528(14) yes
Ru1 Cl2 . 2.3335(15) yes
Ru1 Cl3 . 2.3404(14) yes
Ru1 Cl4 . 2.3652(14) yes
Ru1 S1 . 2.2868(14) yes
Ru1 N1 . 2.123(4) yes
Cl1 Na1 . 2.780(2) yes
Cl4 Na1 . 2.772(2) yes
Na1 O31 2_577 2.414(4) yes
Na1 O1 2_667 2.453(4) yes
Na1 Na1 2_577 3.402(4) yes
Na1 O21 . 2.326(4) yes
Na1 O31 . 2.407(4) yes
S1 O21 . 1.477(3) yes
S1 C21 . 1.749(6) yes
S1 C22 . 1.767(6) yes
O1 N2 . 1.225(6) yes
O2 N2 . 1.223(6) yes
O31 C33 . 1.212(7) yes
O32 C32 . 1.464(7) yes
O32 C33 . 1.345(7) yes
N1 C1 . 1.329(6) yes
N1 C5 . 1.339(6) yes
N2 C8 . 1.460(6) yes
C1 C2 . 1.387(6) yes
C1 H11 . 0.937 no
C2 C3 . 1.377(7) yes
C2 H21 . 0.936 no
C3 C4 . 1.374(7) yes
C3 C12 . 1.516(6) yes
C4 C5 . 1.384(6) yes
C4 H41 . 0.935 no
C5 H51 . 0.938 no
C6 C7 . 1.390(7) yes
C6 C11 . 1.385(7) yes
C6 H61 . 0.933 no
C7 C8 . 1.361(7) yes
C7 H71 . 0.930 no
C8 C9 . 1.380(7) yes
C9 C10 . 1.392(7) yes
C9 H91 . 0.932 no
C10 C11 . 1.371(7) yes
C10 H101 . 0.929 no
C11 C12 . 1.514(7) yes
C12 H121 . 0.972 no
C12 H122 . 0.973 no
C21 H211 . 0.960 no
C21 H212 . 0.960 no
C21 H213 . 0.960 no
C22 H221 . 0.960 no
C22 H222 . 0.960 no
C22 H223 . 0.960 no
C31 C32 . 1.518(9) yes
C31 H311 . 0.957 no
C31 H312 . 0.959 no
C31 H313 . 0.955 no
C32 H321 . 0.972 no
C32 H322 . 0.970 no
C33 C34 . 1.494(8) yes
C34 H341 . 0.965 no
C34 H342 . 0.957 no
C34 H343 . 0.960 no
