#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:31:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179382 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/79/4327984.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_4327984
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_absolute_configuration ad
_chemical_formula_moiety
'C5.25 H9 Cl3 N0.75 Na0.75 O1.12 Ru0.75 S0.75'
_chemical_formula_sum
'C5.25 H9 Cl3 N0.75 Na0.75 O1.12 Ru0.75 S0.75'
_chemical_formula_weight         324.09
_chemical_name_systematic        ?
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            8
_cell_length_a                   13.1432(12)
_cell_length_b                   13.1432(12)
_cell_length_c                   19.6099(18)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.74
_cell_volume                     2933.6(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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_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  0.083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34617
_diffrn_reflns_theta_full        27.435
_diffrn_reflns_theta_max         28.578
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.32
_refine_diff_density_min         -0.84
_refine_ls_abs_structure_details 'Flack (1983), 6555 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0358
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.0008398
_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: 
 0.838 0.531 0.605 0.112 0.841E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0807
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0663
_reflns_limit_h_max              8
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3946
_reflns_number_total             4776
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      98.33
_oxford_refine_ls_r_factor_ref   0.0637
_oxford_refine_ls_scale          0.1187(3)
_oxford_reflns_number_all        4776
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic202029e_si_002_5.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 31 2 1 '
_cod_database_code               4327984
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z+1/3
-x+y,-x,z+2/3
y,x,-z
x-y,-y,-z+2/3
-x,-x+y,-z+1/3
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
Ru1 Ru -0.46643(5) -0.38856(5) -0.80725(3) 0.0203 1.0000 Uani . . .
Cl1 Cl -0.58169(17) -0.33202(16) -0.74345(9) 0.0262 1.0000 Uani . . .
Cl2 Cl -0.61562(17) -0.58638(17) -0.80095(9) 0.0287 1.0000 Uani . . .
Cl3 Cl -0.34898(16) -0.44442(18) -0.86920(10) 0.0306 1.0000 Uani . . .
Cl4 Cl -0.31626(18) -0.19116(17) -0.80831(10) 0.0316 1.0000 Uani . . .
Na1 Na -0.5559(3) -0.6416(3) -0.93187(14) 0.0227 1.0000 Uani . . .
S1 S -0.5407(2) -0.37208(17) -0.90980(9) 0.0282 1.0000 Uani . . .
O1 O -0.5849(5) -0.4772(5) -0.9545(3) 0.0268 1.0000 Uani . . .
O20 O -0.7531(9) -0.7279(9) -0.9875(7) 0.0299 0.5000 Uani . . .
N1 N -0.4125(15) -0.4228(10) -0.7103(7) 0.0248 0.336(16) Uani D P 1
N11 N -0.3869(8) -0.4053(7) -0.7169(4) 0.0248 0.664(16) Uani D P 2
C6 C -0.4372(17) -0.2491(9) -0.9584(5) 0.0722 1.0000 Uani . . .
C7 C -0.6585(15) -0.3427(15) -0.9021(6) 0.0704 1.0000 Uani . . .
C10 C -0.4905(15) -0.4778(9) -0.6586(8) 0.0280 0.336(16) Uani D P 1
C11 C -0.4550(9) -0.4610(6) -0.6615(4) 0.0280 0.664(16) Uani D P 2
C20 C -0.452(2) -0.4944(10) -0.5968(7) 0.0392 0.336(16) Uani D P 1
C21 C -0.4057(11) -0.4734(7) -0.6026(4) 0.0392 0.664(16) Uani D P 2
C30 C -0.335(2) -0.4552(12) -0.5869(7) 0.0327 0.336(16) Uani D P 1
C31 C -0.2868(11) -0.4293(7) -0.5996(4) 0.0327 0.664(16) Uani D P 2
C40 C -0.2567(17) -0.3999(11) -0.6386(9) 0.0316 0.336(16) Uani D P 1
C41 C -0.2181(9) -0.3735(7) -0.6555(5) 0.0316 0.664(16) Uani D P 2
C50 C -0.2952(17) -0.3834(10) -0.7004(8) 0.0294 0.336(16) Uani D P 1
C51 C -0.2698(10) -0.3623(7) -0.7136(4) 0.0294 0.664(16) Uani D P 2
H61 H -0.4722 -0.2463 -1.0003 0.090(12) 1.0000 Uiso R . .
H62 H -0.3702 -0.2565 -0.9675 0.090(12) 1.0000 Uiso R . .
H63 H -0.4142 -0.1790 -0.9335 0.090(12) 1.0000 Uiso R . .
H71 H -0.6854 -0.3368 -0.9461 0.075(12) 1.0000 Uiso R . .
H72 H -0.7209 -0.4049 -0.8776 0.075(12) 1.0000 Uiso R . .
H73 H -0.6321 -0.2709 -0.8782 0.075(12) 1.0000 Uiso R . .
H101 H -0.5703 -0.5056 -0.6646 0.041(12) 0.336(16) Uiso R P 1
H111 H -0.5358 -0.4916 -0.6636 0.041(12) 0.664(16) Uiso R P 2
H201 H -0.5045 -0.5316 -0.5610 0.052(12) 0.336(16) Uiso R P 1
H202 H -0.7820 -0.8035 -1.0072 0.043(12) 0.5000 Uiso R . .
H203 H -0.8134 -0.7270 -0.9612 0.043(12) 0.5000 Uiso R . .
H211 H -0.4520 -0.5105 -0.5647 0.052(12) 0.664(16) Uiso R P 2
H301 H -0.3076 -0.4660 -0.5454 0.044(12) 0.336(16) Uiso R P 1
H311 H -0.2527 -0.4383 -0.5603 0.044(12) 0.664(16) Uiso R P 2
H401 H -0.1771 -0.3725 -0.6327 0.042(12) 0.336(16) Uiso R P 1
H411 H -0.1374 -0.3430 -0.6540 0.042(12) 0.664(16) Uiso R P 2
H501 H -0.2427 -0.3460 -0.7361 0.041(12) 0.336(16) Uiso R P 1
H511 H -0.2228 -0.3251 -0.7514 0.041(12) 0.664(16) Uiso R P 2
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 . 90.50(7) yes
Cl1 . Ru1 Cl3 . 178.92(7) yes
Cl2 . Ru1 Cl3 . 89.80(7) yes
Cl1 . Ru1 Cl4 . 88.51(7) yes
Cl2 . Ru1 Cl4 . 177.46(8) yes
Cl3 . Ru1 Cl4 . 91.15(7) yes
Cl1 . Ru1 S1 . 93.72(7) yes
Cl2 . Ru1 S1 . 89.52(7) yes
Cl3 . Ru1 S1 . 87.32(7) yes
Cl4 . Ru1 S1 . 92.88(8) yes
Cl1 . Ru1 N1 . 85.9(4) yes
Cl2 . Ru1 N1 . 84.4(4) yes
Cl3 . Ru1 N1 . 93.1(4) yes
Cl4 . Ru1 N1 . 93.2(4) yes
S1 . Ru1 N1 . 173.9(4) yes
Na1 6_453 Cl1 Ru1 . 104.51(9) yes
Ru1 . Cl2 Na1 . 92.87(8) yes
Ru1 . Cl3 Na1 . 91.66(8) yes
Ru1 . Cl4 Na1 6_453 98.59(9) yes
O1 4_553 Na1 Cl1 6_443 85.85(16) yes
O1 4_553 Na1 Na1 4_553 46.77(14) yes
Cl1 6_443 Na1 Na1 4_553 129.50(14) yes
O1 4_553 Na1 O20 4_553 74.0(3) yes
Cl1 6_443 Na1 O20 4_553 110.9(2) yes
Na1 4_553 Na1 O20 4_553 48.5(3) yes
O1 4_553 Na1 Cl2 . 150.92(19) yes
Cl1 6_443 Na1 Cl2 . 113.52(11) yes
Na1 4_553 Na1 Cl2 . 116.86(14) yes
O20 4_553 Na1 Cl2 . 115.1(3) yes
O1 4_553 Na1 Cl3 . 92.84(17) yes
Cl1 6_443 Na1 Cl3 . 82.88(9) yes
Na1 4_553 Na1 Cl3 . 111.18(7) yes
O20 4_553 Na1 Cl3 . 159.6(3) yes
Cl2 . Na1 Cl3 . 69.68(8) yes
O1 4_553 Na1 Cl4 6_443 133.49(18) yes
Cl1 6_443 Na1 Cl4 6_443 68.22(8) yes
Na1 4_553 Na1 Cl4 6_443 128.23(7) yes
O20 4_553 Na1 Cl4 6_443 80.1(3) yes
Cl2 . Na1 Cl4 6_443 75.37(8) yes
O1 4_553 Na1 O1 . 77.8(2) yes
Cl1 6_443 Na1 O1 . 153.38(19) yes
Na1 4_553 Na1 O1 . 46.69(13) yes
O20 4_553 Na1 O1 . 84.8(3) yes
Cl2 . Na1 O1 . 75.76(15) yes
O1 4_553 Na1 O20 . 85.6(3) yes
Cl1 6_443 Na1 O20 . 125.4(3) yes
Na1 4_553 Na1 O20 . 49.5(3) yes
O20 4_553 Na1 O20 . 17.2(5) yes
Cl2 . Na1 O20 . 98.7(3) yes
Cl3 . Na1 Cl4 6_443 119.76(11) yes
Cl3 . Na1 O1 . 77.17(16) yes
Cl4 6_443 Na1 O1 . 137.57(19) yes
Cl3 . Na1 O20 . 151.4(3) yes
Cl4 6_443 Na1 O20 . 79.8(3) yes
O1 . Na1 O20 . 74.6(3) yes
Ru1 . S1 O1 . 114.6(2) yes
Ru1 . S1 C6 . 112.8(5) yes
O1 . S1 C6 . 107.1(4) yes
Ru1 . S1 C7 . 113.8(4) yes
O1 . S1 C7 . 105.9(5) yes
C6 . S1 C7 . 101.6(8) yes
Na1 4_553 O1 Na1 . 86.5(2) yes
Na1 4_553 O1 S1 . 146.7(3) yes
Na1 . O1 S1 . 124.0(3) yes
Na1 . O20 Na1 4_553 82.0(3) yes
Na1 . O20 H202 4_553 140.3 no
Na1 4_553 O20 H202 4_553 130.4 no
Na1 . O20 H202 . 115.6 no
Na1 4_553 O20 H202 . 115.5 no
H202 4_553 O20 H202 . 36.0 no
Na1 . O20 H203 . 116.0 no
Na1 4_553 O20 H203 . 116.2 no
H202 4_553 O20 H203 . 73.8 no
H202 . O20 H203 . 109.5 no
Ru1 . N1 C10 . 121.9(9) yes
Ru1 . N1 C50 . 118.1(9) yes
C10 . N1 C50 . 119.9(6) yes
Ru1 . N11 C11 . 119.7(5) yes
Ru1 . N11 C51 . 121.0(6) yes
C11 . N11 C51 . 119.3(6) yes
S1 . C6 H61 . 109.4 no
S1 . C6 H62 . 109.5 no
H61 . C6 H62 . 109.5 no
S1 . C6 H63 . 109.4 no
H61 . C6 H63 . 109.5 no
H62 . C6 H63 . 109.5 no
S1 . C7 H71 . 109.9 no
S1 . C7 H72 . 109.1 no
H71 . C7 H72 . 109.5 no
S1 . C7 H73 . 109.4 no
H71 . C7 H73 . 109.5 no
H72 . C7 H73 . 109.5 no
N1 . C10 C20 . 120.2(7) yes
N1 . C10 H101 . 121.0 no
C20 . C10 H101 . 118.9 no
N11 . C11 C21 . 120.8(6) yes
N11 . C11 H111 . 119.8 no
C21 . C11 H111 . 119.4 no
C10 . C20 C30 . 119.9(7) yes
C10 . C20 H201 . 121.0 no
C30 . C20 H201 . 119.1 no
C11 . C21 C31 . 119.4(6) yes
C11 . C21 H211 . 120.7 no
C31 . C21 H211 . 119.8 no
C20 . C30 C40 . 120.0(6) yes
C20 . C30 H301 . 121.0 no
C40 . C30 H301 . 119.0 no
C21 . C31 C41 . 119.9(5) yes
C21 . C31 H311 . 120.2 no
C41 . C31 H311 . 119.9 no
C30 . C40 C50 . 120.0(7) yes
C30 . C40 H401 . 121.1 no
C50 . C40 H401 . 118.9 no
C31 . C41 C51 . 119.4(6) yes
C31 . C41 H411 . 120.6 no
C51 . C41 H411 . 120.0 no
N1 . C50 C40 . 119.9(8) yes
N1 . C50 H501 . 119.3 no
C40 . C50 H501 . 120.8 no
C41 . C51 N11 . 121.2(6) yes
C41 . C51 H511 . 118.9 no
N11 . C51 H511 . 119.9 no
H202 4_553 H202 O20 . 46.6 no
H202 4_553 H202 O20 4_553 97.4 no
O20 . H202 O20 4_553 51.9 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 . 2.3534(18) yes
Ru1 Cl2 . 2.3499(19) yes
Ru1 Cl3 . 2.3519(18) yes
Ru1 Cl4 . 2.347(2) yes
Ru1 S1 . 2.2923(19) yes
Ru1 N1 . 2.154(12) yes
Cl1 Na1 6_453 2.815(3) yes
Cl2 Na1 . 2.882(3) yes
Cl3 Na1 . 2.928(4) yes
Cl4 Na1 6_453 3.026(3) yes
Na1 O1 4_553 2.412(6) yes
Na1 Na1 4_553 3.308(6) yes
Na1 O20 4_553 2.539(13) yes
Na1 O1 . 2.415(6) yes
Na1 O20 . 2.502(11) yes
S1 O1 . 1.488(5) yes
S1 C6 . 1.781(13) yes
S1 C7 . 1.779(11) yes
O20 H202 4_553 0.696 no
O20 H202 . 0.950 no
O20 H203 . 0.950 no
N1 C10 . 1.365(9) yes
N1 C50 . 1.372(17) yes
N11 C11 . 1.365(8) yes
N11 C51 . 1.351(12) yes
C6 H61 . 0.950 no
C6 H62 . 0.950 no
C6 H63 . 0.950 no
C7 H71 . 0.950 no
C7 H72 . 0.950 no
C7 H73 . 0.950 no
C10 C20 . 1.371(9) yes
C10 H101 . 0.929 no
C11 C21 . 1.373(8) yes
C11 H111 . 0.929 no
C20 C30 . 1.371(8) yes
C20 H201 . 0.931 no
C21 C31 . 1.369(7) yes
C21 H211 . 0.929 no
C30 C40 . 1.367(8) yes
C30 H301 . 0.930 no
C31 C41 . 1.375(7) yes
C31 H311 . 0.929 no
C40 C50 . 1.371(9) yes
C40 H401 . 0.928 no
C41 C51 . 1.371(8) yes
C41 H411 . 0.928 no
C50 H501 . 0.931 no
C51 H511 . 0.932 no
H202 H202 4_553 0.563 no
