#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180007 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/01/7030145.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_7030145
loop_
_publ_author_name
'Delgado, Patricia'
'González-Prieto, Rodrigo'
'Jiménez-Aparicio, Reyes'
'Perles, Josefina'
'Priego, José L'
'Torres, Rosario M.'
_publ_section_title
;
 Comparative study of different methods for the preparation of
 tetraamidato- and tetracarboxylatodiruthenium compounds. Structural and
 magnetic characterization.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11866
_journal_page_last               11874
_journal_paper_doi               10.1039/c2dt30939d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C32 H28 Cl O8 Ru2'
_chemical_formula_weight         778.13
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.277(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.817(2)
_cell_length_b                   11.084(2)
_cell_length_c                   21.847(4)
_cell_measurement_reflns_used    1559
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.4555
_cell_measurement_theta_min      3.2123
_cell_volume                     3071.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.916
_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  0.2025
_diffrn_reflns_av_sigmaI/netI    0.3121
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28138
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  0.9565
_exptl_absorpt_correction_T_min  0.7748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.3221
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.9208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.3155
_reflns_number_gt                2167
_reflns_number_total             7495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30939d.txt
_cod_data_source_block           pdm50
_cod_original_cell_volume        3071.2(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7030145
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C26 C 0.6501(12) 0.8115(11) 0.5623(6) 0.087(6) Uani 1 1 d G
C27 C 0.5960(8) 0.9205(15) 0.5556(7) 0.129(2) Uani 1 1 d G
H27 H 0.5243 0.9215 0.5407 0.155 Uiso 1 1 calc R
C28 C 0.6492(13) 1.0280(11) 0.5711(7) 0.129(2) Uani 1 1 d G
H28 H 0.6130 1.1009 0.5666 0.155 Uiso 1 1 calc R
C29 C 0.7564(13) 1.0265(11) 0.5933(7) 0.129(2) Uani 1 1 d G
H29 H 0.7919 1.0985 0.6036 0.155 Uiso 1 1 calc R
C30 C 0.8105(8) 0.9176(15) 0.6000(6) 0.093(6) Uani 1 1 d G
C31 C 0.7573(12) 0.8100(11) 0.5845(7) 0.129(2) Uani 1 1 d G
H31 H 0.7935 0.7371 0.5890 0.155 Uiso 1 1 calc R
C10 C 0.8523(12) 0.8164(10) 0.4361(6) 0.084(6) Uani 1 1 d G
C11 C 0.9090(9) 0.9227(14) 0.4482(7) 0.129(2) Uani 1 1 d G
H11 H 0.9803 0.9198 0.4642 0.155 Uiso 1 1 calc R
C12 C 0.8594(13) 1.0335(10) 0.4363(8) 0.129(2) Uani 1 1 d G
H12 H 0.8973 1.1046 0.4444 0.155 Uiso 1 1 calc R
C13 C 0.7529(13) 1.0379(11) 0.4124(7) 0.129(2) Uani 1 1 d G
H13 H 0.7197 1.1120 0.4044 0.155 Uiso 1 1 calc R
C14 C 0.6962(9) 0.9316(16) 0.4003(7) 0.134(5) Uani 1 1 d G
C15 C 0.7459(12) 0.8208(12) 0.4121(7) 0.129(2) Uani 1 1 d G
H15 H 0.7079 0.7497 0.4040 0.155 Uiso 1 1 calc R
C1 C 1.0191(15) 0.5896(17) 0.6149(8) 0.075(5) Uani 1 1 d .
C2 C 1.0296(14) 0.6376(15) 0.6753(7) 0.070(5) Uani 1 1 d .
C3 C 0.9482(17) 0.6228(17) 0.7107(8) 0.103(7) Uani 1 1 d .
H3 H 0.8886 0.5782 0.6955 0.123 Uiso 1 1 calc R
C4 C 0.957(2) 0.676(2) 0.7693(9) 0.122(8) Uani 1 1 d .
H4 H 0.9030 0.6674 0.7930 0.146 Uiso 1 1 calc R
C5 C 1.0466(19) 0.740(2) 0.7921(10) 0.103(7) Uani 1 1 d .
H5 H 1.0518 0.7753 0.8310 0.123 Uiso 1 1 calc R
C6 C 1.126(2) 0.752(2) 0.7585(13) 0.134(5) Uani 1 1 d .
C7 C 1.120(2) 0.705(2) 0.6971(13) 0.129(2) Uani 1 1 d .
H7 H 1.1728 0.7189 0.6729 0.155 Uiso 1 1 calc R
C8 C 1.225(2) 0.830(3) 0.7854(14) 0.206(8) Uani 1 1 d .
H8A H 1.2371 0.8910 0.7558 0.308 Uiso 1 1 calc R
H8B H 1.2860 0.7793 0.7936 0.308 Uiso 1 1 calc R
H8C H 1.2122 0.8685 0.8231 0.308 Uiso 1 1 calc R
C9 C 0.8997(15) 0.6972(17) 0.4577(7) 0.069(5) Uani 1 1 d .
C16 C 0.578(2) 0.947(3) 0.3788(14) 0.206(8) Uani 1 1 d .
H16A H 0.5388 0.9011 0.4052 0.308 Uiso 1 1 calc R
H16B H 0.5606 0.9190 0.3370 0.308 Uiso 1 1 calc R
H16C H 0.5592 1.0308 0.3809 0.308 Uiso 1 1 calc R
C17 C 0.5521(13) 0.5495(14) 0.3901(6) 0.054(4) Uani 1 1 d .
C18 C 0.5913(14) 0.5864(14) 0.3337(7) 0.066(5) Uani 1 1 d .
C19 C 0.6859(19) 0.543(2) 0.3229(12) 0.129(2) Uani 1 1 d .
H19 H 0.7232 0.4875 0.3497 0.155 Uiso 1 1 calc R
C20 C 0.727(2) 0.585(2) 0.2681(11) 0.129(2) Uani 1 1 d .
H20 H 0.7920 0.5588 0.2592 0.155 Uiso 1 1 calc R
C21 C 0.6682(19) 0.662(2) 0.2306(11) 0.129(2) Uani 1 1 d .
H21 H 0.6939 0.6855 0.1948 0.155 Uiso 1 1 calc R
C22 C 0.575(2) 0.708(2) 0.2407(12) 0.134(5) Uani 1 1 d .
C23 C 0.5310(19) 0.663(2) 0.2944(11) 0.129(2) Uani 1 1 d .
H23 H 0.4638 0.6849 0.3015 0.155 Uiso 1 1 calc R
C24 C 0.507(2) 0.790(3) 0.1979(14) 0.206(8) Uani 1 1 d .
H24A H 0.5508 0.8492 0.1817 0.308 Uiso 1 1 calc R
H24B H 0.4576 0.8297 0.2199 0.308 Uiso 1 1 calc R
H24C H 0.4704 0.7438 0.1645 0.308 Uiso 1 1 calc R
C25 C 0.5992(15) 0.7006(15) 0.5400(7) 0.062(5) Uani 1 1 d .
C32 C 0.918(2) 0.922(3) 0.6270(14) 0.206(8) Uani 1 1 d .
H32A H 0.9539 0.9820 0.6066 0.308 Uiso 1 1 calc R
H32B H 0.9496 0.8443 0.6225 0.308 Uiso 1 1 calc R
H32C H 0.9222 0.9409 0.6701 0.308 Uiso 1 1 calc R
Cl1 Cl 0.7568(3) 0.3426(4) 0.53208(19) 0.0680(12) Uani 1 1 d .
O1 O 0.9385(9) 0.5281(10) 0.5926(5) 0.069(3) Uani 1 1 d .
O2 O 0.9060(7) 0.3907(9) 0.4199(4) 0.064(3) Uani 1 1 d .
O3 O 0.8471(8) 0.6078(11) 0.4729(5) 0.072(3) Uani 1 1 d .
O4 O 0.9994(10) 0.3069(9) 0.5395(5) 0.074(3) Uani 1 1 d .
O5 O 0.6129(8) 0.4832(9) 0.4284(4) 0.057(3) Uani 1 1 d .
O6 O 0.5354(8) 0.4091(8) 0.5969(4) 0.057(3) Uani 1 1 d .
O7 O 0.6479(8) 0.6006(10) 0.5443(4) 0.059(3) Uani 1 1 d .
O8 O 0.4998(9) 0.7043(8) 0.5181(4) 0.061(3) Uani 1 1 d .
Ru1 Ru 0.92077(10) 0.45753(12) 0.50671(6) 0.0558(5) Uani 1 1 d .
Ru2 Ru 0.57667(10) 0.44755(11) 0.51289(5) 0.0507(5) 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'
O O 0.0106 0.0060 '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
C27 C26 C31 120.0 . .
C27 C26 C25 120.7(14) . .
C31 C26 C25 119.0(14) . .
C28 C27 C26 120.0 . .
C28 C27 H27 120.0 . .
C26 C27 H27 120.0 . .
C27 C28 C29 120.0 . .
C27 C28 H28 120.0 . .
C29 C28 H28 120.0 . .
C30 C29 C28 120.0 . .
C30 C29 H29 120.0 . .
C28 C29 H29 120.0 . .
C31 C30 C29 120.0 . .
C31 C30 C32 122.7(16) . .
C29 C30 C32 117.2(16) . .
C30 C31 C26 120.0 . .
C30 C31 H31 120.0 . .
C26 C31 H31 120.0 . .
C11 C10 C15 120.0 . .
C11 C10 C9 120.6(13) . .
C15 C10 C9 118.7(13) . .
C10 C11 C12 120.0 . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C13 C12 C11 120.0 . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 120.0 . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C13 C14 C15 120.0 . .
C13 C14 C16 115.6(15) . .
C15 C14 C16 124.3(15) . .
C14 C15 C10 120.0 . .
C14 C15 H15 120.0 . .
C10 C15 H15 120.0 . .
O1 C1 O2 118.9(15) . 3_766
O1 C1 C2 121.5(16) . .
O2 C1 C2 119.7(18) 3_766 .
C3 C2 C7 121.4(19) . .
C3 C2 C1 119.7(19) . .
C7 C2 C1 118.8(18) . .
C2 C3 C4 119(2) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C5 C4 C3 120(2) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C6 C5 C4 121(2) . .
C6 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
C5 C6 C7 122(3) . .
C5 C6 C8 119(3) . .
C7 C6 C8 119(3) . .
C2 C7 C6 116(2) . .
C2 C7 H7 121.9 . .
C6 C7 H7 121.9 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O3 C9 O4 121.9(16) . 3_766
O3 C9 C10 124.2(16) . .
O4 C9 C10 113.9(16) 3_766 .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O6 C17 O5 121.8(12) 3_666 .
O6 C17 C18 120.5(14) 3_666 .
O5 C17 C18 117.4(14) . .
C19 C18 C23 123.5(19) . .
C19 C18 C17 118.2(17) . .
C23 C18 C17 118.3(17) . .
C18 C19 C20 118(2) . .
C18 C19 H19 121.1 . .
C20 C19 H19 121.1 . .
C21 C20 C19 118(2) . .
C21 C20 H20 120.9 . .
C19 C20 H20 120.9 . .
C20 C21 C22 125(3) . .
C20 C21 H21 117.4 . .
C22 C21 H21 117.4 . .
C21 C22 C23 117(2) . .
C21 C22 C24 125(3) . .
C23 C22 C24 117(2) . .
C18 C23 C22 118(2) . .
C18 C23 H23 121.0 . .
C22 C23 H23 121.0 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
O7 C25 O8 120.1(15) . .
O7 C25 C26 121.6(17) . .
O8 C25 C26 118.1(16) . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
Ru2 Cl1 Ru1 118.82(15) . .
C1 O1 Ru1 122.7(10) . .
C1 O2 Ru1 120.1(11) 3_766 .
C9 O3 Ru1 120.4(11) . .
C9 O4 Ru1 119.4(11) 3_766 .
C17 O5 Ru2 120.8(9) . .
C17 O6 Ru2 118.4(9) 3_666 .
C25 O7 Ru2 121.3(10) . .
C25 O8 Ru2 120.2(10) . 3_666
O3 Ru1 O1 90.3(4) . .
O3 Ru1 O2 89.0(4) . .
O1 Ru1 O2 178.2(4) . .
O3 Ru1 O4 178.1(4) . .
O1 Ru1 O4 90.4(4) . .
O2 Ru1 O4 90.2(4) . .
O3 Ru1 Ru1 89.5(3) . 3_766
O1 Ru1 Ru1 88.6(3) . 3_766
O2 Ru1 Ru1 89.7(3) . 3_766
O4 Ru1 Ru1 88.8(3) . 3_766
O3 Ru1 Cl1 97.7(3) . .
O1 Ru1 Cl1 88.7(3) . .
O2 Ru1 Cl1 93.0(3) . .
O4 Ru1 Cl1 84.1(3) . .
Ru1 Ru1 Cl1 172.37(13) 3_766 .
O7 Ru2 O5 89.7(4) . .
O7 Ru2 O8 178.0(4) . 3_666
O5 Ru2 O8 91.2(4) . 3_666
O7 Ru2 O6 91.9(4) . .
O5 Ru2 O6 178.0(4) . .
O8 Ru2 O6 87.2(4) 3_666 .
O7 Ru2 Ru2 89.2(3) . 3_666
O5 Ru2 Ru2 88.7(3) . 3_666
O8 Ru2 Ru2 89.0(3) 3_666 3_666
O6 Ru2 Ru2 90.2(3) . 3_666
O7 Ru2 Cl1 88.5(3) . .
O5 Ru2 Cl1 85.3(3) . .
O8 Ru2 Cl1 93.4(3) 3_666 .
O6 Ru2 Cl1 95.9(3) . .
Ru2 Ru2 Cl1 173.59(12) 3_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C26 C27 1.3900 .
C26 C31 1.3900 .
C26 C25 1.443(18) .
C27 C28 1.3900 .
C27 H27 0.9300 .
C28 C29 1.3900 .
C28 H28 0.9300 .
C29 C30 1.3900 .
C29 H29 0.9300 .
C30 C31 1.3900 .
C30 C32 1.42(3) .
C31 H31 0.9300 .
C10 C11 1.3900 .
C10 C15 1.3900 .
C10 C9 1.502(19) .
C11 C12 1.3900 .
C11 H11 0.9300 .
C12 C13 1.3900 .
C12 H12 0.9300 .
C13 C14 1.3900 .
C13 H13 0.9300 .
C14 C15 1.3900 .
C14 C16 1.53(3) .
C15 H15 0.9300 .
C1 O1 1.274(19) .
C1 O2 1.326(18) 3_766
C1 C2 1.41(2) .
C2 C3 1.40(2) .
C2 C7 1.40(3) .
C3 C4 1.40(2) .
C3 H3 0.9300 .
C4 C5 1.38(3) .
C4 H4 0.9300 .
C5 C6 1.34(3) .
C5 H5 0.9300 .
C6 C7 1.43(3) .
C6 C8 1.58(4) .
C7 H7 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 O3 1.270(18) .
C9 O4 1.287(18) 3_766
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 O6 1.282(17) 3_666
C17 O5 1.288(16) .
C17 C18 1.454(19) .
C18 C19 1.36(2) .
C18 C23 1.36(2) .
C19 C20 1.45(3) .
C19 H19 0.9300 .
C20 C21 1.34(3) .
C20 H20 0.9300 .
C21 C22 1.35(3) .
C21 H21 0.9300 .
C22 C23 1.46(3) .
C22 C24 1.49(3) .
C23 H23 0.9300 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 O7 1.269(17) .
C25 O8 1.295(18) .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
Cl1 Ru2 2.565(4) .
Cl1 Ru1 2.585(4) .
O1 Ru1 2.016(11) .
O2 C1 1.326(18) 3_766
O2 Ru1 2.018(10) .
O3 Ru1 2.002(12) .
O4 C9 1.287(18) 3_766
O4 Ru1 2.027(11) .
O5 Ru2 2.006(9) .
O6 C17 1.282(17) 3_666
O6 Ru2 2.027(9) .
O7 Ru2 2.001(10) .
O8 Ru2 2.015(10) 3_666
Ru1 Ru1 2.295(2) 3_766
Ru2 O8 2.015(10) 3_666
Ru2 Ru2 2.283(3) 3_666
