#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:16:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179053 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/15/4301507.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_4301507
loop_
_publ_author_name
'Sofia Derossi'
'Lee Brammer'
'Christopher A. Hunter'
'Michael D. Ward'
_publ_contact_author
; 
        Prof. Mike Ward
        Department of Chemistry
        University of Sheffield
        SHEFFIELD
        S3 7HF
;
_publ_contact_author_email       m.d.ward@sheffield.ac.uk
_publ_contact_author_fax         '0114 2229346'
_publ_section_title
;
Halogen Bonded Supramolecular Assemblies of [Ru(bipy)(CN)4]2- Anions
and N-Methyl-Halopyridinium Cations in the Solid State and in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1666
_journal_page_last               1677
_journal_paper_doi               10.1021/ic8021529
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C26 H20 I4 N8 Ru'
_chemical_formula_weight         1053.17
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.435(5)
_cell_angle_beta                 90.038(5)
_cell_angle_gamma                100.223(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3350(8)
_cell_length_b                   13.1418(12)
_cell_length_c                   13.7330(13)
_cell_measurement_temperature    100(2)
_cell_volume                     1516.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24579
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    4.620
_exptl_absorpt_correction_T_max  0.7381
_exptl_absorpt_correction_T_min  0.5252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.129
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0549
_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)+(0.1080P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                4815
_reflns_number_total             6411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8021529_si_002_4.cif
_cod_data_source_block           imw1133
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4301507
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.72911(7) 0.78345(5) 0.26579(5) 0.01379(17) Uani 1 1 d . . .
C1 C 0.9008(9) 0.8626(6) 0.2129(6) 0.0154(16) Uani 1 1 d . . .
C2 C 0.5557(9) 0.6940(7) 0.3064(7) 0.0173(17) Uani 1 1 d . . .
C3 C 0.5993(9) 0.8140(7) 0.1705(6) 0.0169(17) Uani 1 1 d . . .
C4 C 0.7721(9) 0.6400(7) 0.1552(7) 0.0167(17) Uani 1 1 d . . .
N1 N 0.9975(8) 0.9003(6) 0.1780(6) 0.0242(16) Uani 1 1 d . . .
N2 N 0.4580(8) 0.6388(6) 0.3279(6) 0.0228(16) Uani 1 1 d . . .
N3 N 0.5246(7) 0.8425(6) 0.1221(6) 0.0204(15) Uani 1 1 d . . .
N4 N 0.8073(7) 0.5585(6) 0.0965(6) 0.0197(15) Uani 1 1 d . . .
N11 N 0.8643(7) 0.7810(6) 0.3872(6) 0.0183(15) Uani 1 1 d . . .
C12 C 0.8702(8) 0.8685(7) 0.4838(6) 0.0168(17) Uani 1 1 d . . .
C13 C 0.9595(8) 0.8787(7) 0.5709(7) 0.0181(17) Uani 1 1 d . . .
H13A H 0.9658 0.9421 0.6369 0.022 Uiso 1 1 calc R . .
C14 C 1.0376(9) 0.7958(7) 0.5594(7) 0.0203(18) Uani 1 1 d . . .
H14A H 1.0993 0.8016 0.6172 0.024 Uiso 1 1 calc R . .
C15 C 1.0253(9) 0.7035(8) 0.4622(7) 0.0227(19) Uani 1 1 d . . .
H15A H 1.0757 0.6440 0.4535 0.027 Uiso 1 1 calc R . .
C16 C 0.9399(9) 0.6993(7) 0.3794(7) 0.0207(18) Uani 1 1 d . . .
H16A H 0.9330 0.6360 0.3132 0.025 Uiso 1 1 calc R . .
N21 N 0.7091(7) 0.9343(6) 0.3969(5) 0.0174(15) Uani 1 1 d . . .
C22 C 0.7835(8) 0.9540(7) 0.4898(7) 0.0168(17) Uani 1 1 d . . .
C23 C 0.7758(9) 1.0469(7) 0.5831(7) 0.0191(18) Uani 1 1 d . . .
H23A H 0.8262 1.0575 0.6475 0.023 Uiso 1 1 calc R . .
C24 C 0.6928(9) 1.1249(7) 0.5810(7) 0.0221(19) Uani 1 1 d . . .
H24A H 0.6862 1.1894 0.6438 0.027 Uiso 1 1 calc R . .
C25 C 0.6213(9) 1.1063(7) 0.4868(7) 0.0191(18) Uani 1 1 d . . .
H25A H 0.5657 1.1589 0.4834 0.023 Uiso 1 1 calc R . .
C26 C 0.6296(9) 1.0118(7) 0.3971(7) 0.0191(18) Uani 1 1 d . . .
H26A H 0.5780 1.0001 0.3328 0.023 Uiso 1 1 calc R . .
N31 N 0.4805(7) 0.3584(6) 0.1342(6) 0.0190(15) Uani 1 1 d . . .
C32 C 0.3813(9) 0.2632(7) 0.1191(7) 0.0186(17) Uani 1 1 d . . .
H32A H 0.3175 0.2270 0.0560 0.022 Uiso 1 1 calc R . .
C33 C 0.3734(9) 0.2193(7) 0.1952(8) 0.024(2) Uani 1 1 d . . .
C34 C 0.4620(10) 0.2738(8) 0.2885(8) 0.028(2) Uani 1 1 d . . .
H34A H 0.4527 0.2467 0.3433 0.033 Uiso 1 1 calc R . .
C35 C 0.5677(9) 0.3715(8) 0.3013(7) 0.0239(19) Uani 1 1 d . . .
C36 C 0.5716(9) 0.4107(7) 0.2217(7) 0.0218(19) Uani 1 1 d . . .
H36A H 0.6407 0.4764 0.2295 0.026 Uiso 1 1 calc R . .
C37 C 0.4802(10) 0.4125(7) 0.0589(7) 0.025(2) Uani 1 1 d . . .
H37A H 0.5586 0.4796 0.0818 0.038 Uiso 1 1 calc R . .
H37B H 0.3860 0.4349 0.0568 0.038 Uiso 1 1 calc R . .
H37C H 0.4960 0.3591 -0.0123 0.038 Uiso 1 1 calc R . .
I1 I 1.18463(6) 0.47826(4) 0.24371(4) 0.01930(16) Uani 1 1 d . . .
I2 I 0.69356(6) 0.06053(5) 0.13046(5) 0.02118(16) Uani 1 1 d . . .
N41 N 0.8527(7) 0.2923(6) -0.0110(6) 0.0179(15) Uani 1 1 d . . .
C42 C 0.7741(8) 0.2097(7) 0.0130(7) 0.0172(17) Uani 1 1 d . . .
H42A H 0.6931 0.1593 -0.0335 0.021 Uiso 1 1 calc R . .
C43 C 0.8116(9) 0.1988(7) 0.1045(7) 0.0205(18) Uani 1 1 d . . .
C44 C 0.9266(9) 0.2730(7) 0.1749(7) 0.0206(18) Uani 1 1 d . . .
H44A H 0.9517 0.2662 0.2388 0.025 Uiso 1 1 calc R . .
C45 C 1.0053(9) 0.3593(7) 0.1480(6) 0.0168(17) Uani 1 1 d . . .
C46 C 0.9687(8) 0.3650(7) 0.0534(7) 0.0171(17) Uani 1 1 d . . .
H46A H 1.0251 0.4202 0.0333 0.021 Uiso 1 1 calc R . .
C47 C 0.8158(10) 0.3050(8) -0.1092(7) 0.0244(19) Uani 1 1 d . . .
H47A H 0.8839 0.3690 -0.1130 0.037 Uiso 1 1 calc R . .
H47B H 0.7160 0.3187 -0.1090 0.037 Uiso 1 1 calc R . .
H47C H 0.8230 0.2358 -0.1710 0.037 Uiso 1 1 calc R . .
I3 I 0.20932(6) 0.07938(5) 0.17794(5) 0.02384(17) Uani 1 1 d . . .
I4 I 0.70685(8) 0.45485(6) 0.43811(6) 0.0408(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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Ru1 C4 96.2(3) . . ?
C3 Ru1 C2 91.1(3) . . ?
C4 Ru1 C2 90.4(3) . . ?
C3 Ru1 C1 87.3(3) . . ?
C4 Ru1 C1 85.3(3) . . ?
C2 Ru1 C1 175.3(3) . . ?
C3 Ru1 N11 169.4(3) . . ?
C4 Ru1 N11 94.2(3) . . ?
C2 Ru1 N11 90.5(3) . . ?
C1 Ru1 N11 91.9(3) . . ?
C3 Ru1 N21 92.0(3) . . ?
C4 Ru1 N21 171.6(3) . . ?
C2 Ru1 N21 91.2(3) . . ?
C1 Ru1 N21 93.3(3) . . ?
N11 Ru1 N21 77.5(3) . . ?
N1 C1 Ru1 175.6(7) . . ?
N2 C2 Ru1 177.4(7) . . ?
N3 C3 Ru1 173.4(7) . . ?
N4 C4 Ru1 174.3(7) . . ?
C16 N11 C12 117.7(7) . . ?
C16 N11 Ru1 126.6(6) . . ?
C12 N11 Ru1 115.7(5) . . ?
N11 C12 C13 121.4(8) . . ?
N11 C12 C22 116.1(7) . . ?
C13 C12 C22 122.4(8) . . ?
C14 C13 C12 119.2(8) . . ?
C14 C13 H13A 120.4 . . ?
C12 C13 H13A 120.4 . . ?
C13 C14 C15 119.2(8) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
C16 C15 C14 119.1(8) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
N11 C16 C15 123.2(8) . . ?
N11 C16 H16A 118.4 . . ?
C15 C16 H16A 118.4 . . ?
C22 N21 C26 117.5(7) . . ?
C22 N21 Ru1 115.7(5) . . ?
C26 N21 Ru1 126.8(6) . . ?
N21 C22 C23 122.0(7) . . ?
N21 C22 C12 114.9(7) . . ?
C23 C22 C12 123.0(8) . . ?
C22 C23 C24 119.2(8) . . ?
C22 C23 H23A 120.4 . . ?
C24 C23 H23A 120.4 . . ?
C25 C24 C23 118.6(8) . . ?
C25 C24 H24A 120.7 . . ?
C23 C24 H24A 120.7 . . ?
C24 C25 C26 120.2(8) . . ?
C24 C25 H25A 119.9 . . ?
C26 C25 H25A 119.9 . . ?
N21 C26 C25 122.5(8) . . ?
N21 C26 H26A 118.7 . . ?
C25 C26 H26A 118.7 . . ?
C36 N31 C32 121.2(7) . . ?
C36 N31 C37 118.1(7) . . ?
C32 N31 C37 120.5(7) . . ?
N31 C32 C33 120.0(8) . . ?
N31 C32 H32A 120.0 . . ?
C33 C32 H32A 120.0 . . ?
C32 C33 C34 120.2(8) . . ?
C32 C33 I3 120.1(7) . . ?
C34 C33 I3 119.2(6) . . ?
C33 C34 C35 118.7(8) . . ?
C33 C34 H34A 120.7 . . ?
C35 C34 H34A 120.7 . . ?
C36 C35 C34 118.3(8) . . ?
C36 C35 I4 121.2(6) . . ?
C34 C35 I4 120.5(7) . . ?
N31 C36 C35 121.5(8) . . ?
N31 C36 H36A 119.3 . . ?
C35 C36 H36A 119.3 . . ?
N31 C37 H37A 109.5 . . ?
N31 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N31 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C45 I1 N2 166.4(3) . 1_655 ?
C43 I2 N3 169.0(3) . 1_545 ?
C43 I2 C3 163.3(3) . 1_545 ?
N3 I2 C3 18.99(18) 1_545 1_545 ?
C46 N41 C42 121.4(7) . . ?
C46 N41 C47 117.7(7) . . ?
C42 N41 C47 120.9(7) . . ?
N41 C42 C43 119.8(8) . . ?
N41 C42 H42A 120.1 . . ?
C43 C42 H42A 120.1 . . ?
C42 C43 C44 121.2(8) . . ?
C42 C43 I2 117.5(6) . . ?
C44 C43 I2 121.2(6) . . ?
C43 C44 C45 117.4(8) . . ?
C43 C44 H44A 121.3 . . ?
C45 C44 H44A 121.3 . . ?
C46 C45 C44 119.9(8) . . ?
C46 C45 I1 117.2(6) . . ?
C44 C45 I1 122.9(6) . . ?
N41 C46 C45 120.2(7) . . ?
N41 C46 H46A 119.9 . . ?
C45 C46 H46A 119.9 . . ?
N41 C47 H47A 109.5 . . ?
N41 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N41 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C33 I3 N1 174.0(3) . 1_445 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C3 1.982(9) . ?
Ru1 C4 2.003(8) . ?
Ru1 C2 2.040(8) . ?
Ru1 C1 2.046(8) . ?
Ru1 N11 2.104(7) . ?
Ru1 N21 2.121(7) . ?
C1 N1 1.149(11) . ?
C2 N2 1.175(10) . ?
C3 N3 1.165(11) . ?
C4 N4 1.159(10) . ?
N11 C16 1.357(10) . ?
N11 C12 1.360(10) . ?
C12 C13 1.405(11) . ?
C12 C22 1.475(12) . ?
C13 C14 1.374(12) . ?
C13 H13A 0.9500 . ?
C14 C15 1.389(12) . ?
C14 H14A 0.9500 . ?
C15 C16 1.366(12) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
N21 C22 1.360(11) . ?
N21 C26 1.362(10) . ?
C22 C23 1.387(12) . ?
C23 C24 1.398(12) . ?
C23 H23A 0.9500 . ?
C24 C25 1.367(12) . ?
C24 H24A 0.9500 . ?
C25 C26 1.372(12) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
N31 C36 1.332(11) . ?
N31 C32 1.360(10) . ?
N31 C37 1.469(11) . ?
C32 C33 1.377(12) . ?
C32 H32A 0.9500 . ?
C33 C34 1.378(13) . ?
C33 I3 2.106(8) . ?
C34 C35 1.423(12) . ?
C34 H34A 0.9500 . ?
C35 C36 1.379(12) . ?
C35 I4 2.067(9) . ?
C36 H36A 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
I1 C45 2.100(8) . ?
I1 N2 2.906(7) 1_655 ?
I2 C43 2.109(8) . ?
I2 N3 2.974(7) 1_545 ?
I2 C3 3.461(8) 1_545 ?
N41 C46 1.351(10) . ?
N41 C42 1.352(10) . ?
N41 C47 1.471(11) . ?
C42 C43 1.372(12) . ?
C42 H42A 0.9500 . ?
C43 C44 1.384(12) . ?
C44 C45 1.415(11) . ?
C44 H44A 0.9500 . ?
C45 C46 1.377(12) . ?
C46 H46A 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
I3 N1 2.793(7) 1_445 ?
