#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:40:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179072 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/34/4303419.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_4303419
loop_
_publ_author_name
'József S. Pap'
'Jamie L. Snyder'
'Paula M. B. Piccoli'
'John F. Berry'
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison
WI
53706
;
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       6082627534
_publ_section_title
;
Chloro and Azido Diruthenium Complexes Bearing
Electron-Rich N,N',N''-Triphenylguanidinate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9846
_journal_page_last               9852
_journal_paper_doi               10.1021/ic901419w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         Ru2(C19N3H16)4Cl,(CH2Cl2)4
_chemical_formula_sum            'C80 H72 Cl9 N12 Ru2'
_chemical_formula_weight         1722.69
_chemical_name_common            Ru2(TPG)4Cl,(CH2Cl2)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-08-13 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.409(5)
_cell_length_b                   18.409(5)
_cell_length_c                   11.110(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.41
_cell_volume                     3765.1(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46706
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.8605
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4122
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0472P)²+2.3587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                3617
_reflns_number_total             4122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901419w_si_001_3.cif
_cod_data_source_block           berry55m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_original_cell_volume        3764.7(17)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4303419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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 0.2500 0.2500 0.01698(3) 0.01237(10) Uani 1 4 d S . .
Ru2 Ru 0.2500 0.2500 0.22435(3) 0.01218(10) Uani 1 4 d S . .
N1 N 0.28855(10) 0.02985(9) 0.12758(14) 0.0170(3) Uani 1 1 d . . .
H1A H 0.3019 0.0106 0.0585 0.020 Uiso 1 1 calc R . .
N2 N 0.25502(9) 0.13631(9) 0.02626(14) 0.0154(3) Uani 1 1 d . . .
N3 N 0.14538(9) 0.20953(9) 0.22502(14) 0.0149(3) Uani 1 1 d . . .
C1 C 0.27759(11) 0.10427(11) 0.12676(17) 0.0155(4) Uani 1 1 d . . .
C11 C 0.28119(11) -0.01933(11) 0.22429(17) 0.0168(4) Uani 1 1 d . . .
C12 C 0.31324(11) -0.08759(11) 0.21247(19) 0.0208(4) Uani 1 1 d . . .
H12A H 0.3403 -0.0990 0.1422 0.025 Uiso 1 1 calc R . .
C13 C 0.30565(12) -0.13906(11) 0.3033(2) 0.0245(5) Uani 1 1 d . . .
H13A H 0.3267 -0.1858 0.2940 0.029 Uiso 1 1 calc R . .
C14 C 0.26755(13) -0.12254(12) 0.4075(2) 0.0254(5) Uani 1 1 d . . .
H14A H 0.2634 -0.1573 0.4703 0.031 Uiso 1 1 calc R . .
C15 C 0.23565(12) -0.05480(12) 0.41880(19) 0.0219(4) Uani 1 1 d . . .
H15A H 0.2091 -0.0434 0.4896 0.026 Uiso 1 1 calc R . .
C16 C 0.24190(11) -0.00312(11) 0.32818(18) 0.0178(4) Uani 1 1 d . . .
H16A H 0.2195 0.0431 0.3370 0.021 Uiso 1 1 calc R . .
C21 C 0.22871(11) 0.09007(10) -0.06827(18) 0.0158(4) Uani 1 1 d . . .
C22 C 0.27030(11) 0.07862(11) -0.17168(18) 0.0191(4) Uani 1 1 d . . .
H22A H 0.3159 0.1021 -0.1805 0.023 Uiso 1 1 calc R . .
C23 C 0.24482(13) 0.03294(11) -0.26134(18) 0.0223(4) Uani 1 1 d . . .
H23A H 0.2729 0.0257 -0.3321 0.027 Uiso 1 1 calc R . .
C24 C 0.17886(13) -0.00219(11) -0.24874(19) 0.0231(4) Uani 1 1 d . . .
H24A H 0.1623 -0.0343 -0.3098 0.028 Uiso 1 1 calc R . .
C25 C 0.13682(12) 0.00952(12) -0.1463(2) 0.0238(4) Uani 1 1 d . . .
H25A H 0.0912 -0.0140 -0.1378 0.029 Uiso 1 1 calc R . .
C26 C 0.16183(11) 0.05569(11) -0.05677(19) 0.0205(4) Uani 1 1 d . . .
H26A H 0.1331 0.0639 0.0129 0.025 Uiso 1 1 calc R . .
C31 C 0.12237(10) 0.15869(11) 0.31242(18) 0.0164(4) Uani 1 1 d . . .
C32 C 0.08516(11) 0.09475(11) 0.28238(19) 0.0204(4) Uani 1 1 d . . .
H32A H 0.0735 0.0849 0.2007 0.024 Uiso 1 1 calc R . .
C33 C 0.06545(12) 0.04592(13) 0.3714(2) 0.0257(5) Uani 1 1 d . . .
H33A H 0.0394 0.0032 0.3501 0.031 Uiso 1 1 calc R . .
C34 C 0.08296(12) 0.05824(13) 0.4906(2) 0.0274(5) Uani 1 1 d . . .
H34A H 0.0691 0.0243 0.5508 0.033 Uiso 1 1 calc R . .
C35 C 0.12094(12) 0.12068(13) 0.52162(19) 0.0249(5) Uani 1 1 d . . .
H35A H 0.1340 0.1292 0.6032 0.030 Uiso 1 1 calc R . .
C36 C 0.13996(11) 0.17092(11) 0.43321(19) 0.0193(4) Uani 1 1 d . . .
H36A H 0.1651 0.2140 0.4552 0.023 Uiso 1 1 calc R . .
Cl3 Cl 0.2500 0.2500 -0.20208(8) 0.01691(19) Uani 1 4 d S . .
C1S C 0.3664(3) -0.1139(3) -0.1872(5) 0.0398(15) Uani 0.682(13) 1 d PD A 1
H1SA H 0.3470 -0.0927 -0.2627 0.048 Uiso 0.682(13) 1 calc PR A 1
H1SB H 0.3989 -0.1547 -0.2088 0.048 Uiso 0.682(13) 1 calc PR A 1
Cl4 Cl 0.4168(3) -0.0458(3) -0.1060(6) 0.0308(7) Uani 0.682(13) 1 d PD A 1
Cl5 Cl 0.29423(16) -0.1462(2) -0.0984(2) 0.0323(8) Uani 0.682(13) 1 d PD A 1
C1SA C 0.3916(5) -0.1339(5) -0.1317(10) 0.030(3) Uani 0.318(13) 1 d PD A 2
H1SC H 0.4022 -0.1508 -0.2145 0.036 Uiso 0.318(13) 1 calc PR A 2
H1SD H 0.4203 -0.1637 -0.0748 0.036 Uiso 0.318(13) 1 calc PR A 2
Cl4A Cl 0.4159(8) -0.0396(6) -0.1164(14) 0.046(3) Uani 0.318(13) 1 d PD A 2
Cl5A Cl 0.2967(5) -0.1438(7) -0.1004(8) 0.062(3) Uani 0.318(13) 1 d PD A 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ru1 N2 174.36(9) 2 . ?
N2 Ru1 N2 89.862(4) 2 3 ?
N2 Ru1 N2 89.861(4) . 3 ?
N2 Ru1 N2 89.862(4) 2 4 ?
N2 Ru1 N2 89.861(4) . 4 ?
N2 Ru1 N2 174.36(9) 3 4 ?
N2 Ru1 Ru2 87.18(4) 2 . ?
N2 Ru1 Ru2 87.18(4) . . ?
N2 Ru1 Ru2 87.18(4) 3 . ?
N2 Ru1 Ru2 87.18(4) 4 . ?
N2 Ru1 Cl3 92.82(4) 2 . ?
N2 Ru1 Cl3 92.82(4) . . ?
N2 Ru1 Cl3 92.82(4) 3 . ?
N2 Ru1 Cl3 92.82(4) 4 . ?
Ru2 Ru1 Cl3 180.0 . . ?
N3 Ru2 N3 90.0 2 4 ?
N3 Ru2 N3 179.59(9) 2 . ?
N3 Ru2 N3 89.999(1) 4 . ?
N3 Ru2 N3 90.0 2 3 ?
N3 Ru2 N3 179.59(9) 4 3 ?
N3 Ru2 N3 90.0 . 3 ?
N3 Ru2 Ru1 90.21(4) 2 . ?
N3 Ru2 Ru1 90.21(4) 4 . ?
N3 Ru2 Ru1 90.21(4) . . ?
N3 Ru2 Ru1 90.21(4) 3 . ?
C1 N1 C11 128.73(17) . . ?
C1 N1 H1A 115.6 . . ?
C11 N1 H1A 115.6 . . ?
C1 N2 C21 117.18(17) . . ?
C1 N2 Ru1 119.85(13) . . ?
C21 N2 Ru1 122.73(12) . . ?
C1 N3 C31 120.26(16) 4 . ?
C1 N3 Ru2 117.18(13) 4 . ?
C31 N3 Ru2 121.39(12) . . ?
N2 C1 N3 119.06(18) . 3 ?
N2 C1 N1 119.34(17) . . ?
N3 C1 N1 121.60(17) 3 . ?
C12 C11 C16 119.36(18) . . ?
C12 C11 N1 117.76(18) . . ?
C16 C11 N1 122.86(18) . . ?
C13 C12 C11 120.19(19) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C15 C14 C13 119.2(2) . . ?
C15 C14 H14A 120.4 . . ?
C13 C14 H14A 120.4 . . ?
C14 C15 C16 121.0(2) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C15 C16 C11 119.74(19) . . ?
C15 C16 H16A 120.1 . . ?
C11 C16 H16A 120.1 . . ?
C26 C21 C22 119.50(18) . . ?
C26 C21 N2 120.09(18) . . ?
C22 C21 N2 120.41(18) . . ?
C23 C22 C21 119.83(19) . . ?
C23 C22 H22A 120.1 . . ?
C21 C22 H22A 120.1 . . ?
C24 C23 C22 120.6(2) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 119.9(2) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 H25A 120.1 . . ?
C24 C25 H25A 120.1 . . ?
C25 C26 C21 120.5(2) . . ?
C25 C26 H26A 119.8 . . ?
C21 C26 H26A 119.8 . . ?
C36 C31 C32 118.46(18) . . ?
C36 C31 N3 118.89(18) . . ?
C32 C31 N3 122.59(18) . . ?
C33 C32 C31 120.2(2) . . ?
C33 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C34 C33 C32 121.1(2) . . ?
C34 C33 H33A 119.4 . . ?
C32 C33 H33A 119.4 . . ?
C33 C34 C35 119.4(2) . . ?
C33 C34 H34A 120.3 . . ?
C35 C34 H34A 120.3 . . ?
C34 C35 C36 120.1(2) . . ?
C34 C35 H35A 120.0 . . ?
C36 C35 H35A 120.0 . . ?
C35 C36 C31 120.7(2) . . ?
C35 C36 H36A 119.6 . . ?
C31 C36 H36A 119.6 . . ?
Cl5 C1S Cl4 110.1(3) . . ?
Cl5 C1S H1SA 109.6 . . ?
Cl4 C1S H1SA 109.6 . . ?
Cl5 C1S H1SB 109.6 . . ?
Cl4 C1S H1SB 109.6 . . ?
H1SA C1S H1SB 108.2 . . ?
Cl5A C1SA Cl4A 108.8(7) . . ?
Cl5A C1SA H1SC 109.9 . . ?
Cl4A C1SA H1SC 109.9 . . ?
Cl5A C1SA H1SD 109.9 . . ?
Cl4A C1SA H1SD 109.9 . . ?
H1SC C1SA H1SD 108.3 . . ?
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 N2 2.0975(17) 2 ?
Ru1 N2 2.0975(17) . ?
Ru1 N2 2.0975(17) 3 ?
Ru1 N2 2.0975(17) 4 ?
Ru1 Ru2 2.3039(7) . ?
Ru1 Cl3 2.4336(11) . ?
Ru2 N3 2.0649(17) 2 ?
Ru2 N3 2.0649(17) 4 ?
Ru2 N3 2.0649(17) . ?
Ru2 N3 2.0649(17) 3 ?
N1 C1 1.385(3) . ?
N1 C11 1.411(2) . ?
N1 H1A 0.8800 . ?
N2 C1 1.329(2) . ?
N2 C21 1.436(2) . ?
N3 C1 1.349(2) 4 ?
N3 C31 1.414(2) . ?
C1 N3 1.349(2) 3 ?
C11 C12 1.394(3) . ?
C11 C16 1.394(3) . ?
C12 C13 1.392(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.387(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.384(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.390(3) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C21 C26 1.390(3) . ?
C21 C22 1.397(3) . ?
C22 C23 1.386(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.383(3) . ?
C23 H23A 0.9500 . ?
C24 C25 1.393(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.387(3) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C31 C36 1.399(3) . ?
C31 C32 1.402(3) . ?
C32 C33 1.385(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.382(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.389(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.394(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C1S Cl5 1.758(5) . ?
C1S Cl4 1.802(6) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1SA Cl5A 1.791(8) . ?
C1SA Cl4A 1.802(9) . ?
C1SA H1SC 0.9900 . ?
C1SA H1SD 0.9900 . ?
