#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/30/7013094.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_7013094
loop_
_publ_author_name
'Daniel Dönnecke'
'Wolfgang Imhof'
_publ_section_title
;
 The formation of cis- and trans-[Ru(CN)2(CNtBu)4] by reductive
 cleavage of isocyanide ligands; isomer separation by supramolecular
 interactions with various solvents
;
_journal_issue                   13
_journal_name_full               'Dalton Trans.'
_journal_page_first              2737
_journal_page_last               2744
_journal_paper_doi               10.1039/b304199a
_journal_year                    2003
_chemical_formula_sum            'C11.75 H19.5 N3 O0.25 Ru0.5'
_chemical_formula_weight         257.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.64(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3896(3)
_cell_length_b                   9.6085(3)
_cell_length_c                   14.8321(5)
_cell_measurement_temperature    173(2)
_cell_volume                     1480.06(8)
_computing_cell_refinement       XP
_computing_data_collection       COLLECT
_computing_data_reduction        XP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       KAPPA-CCD
_diffrn_measurement_method       'phi-scan, omega-scan'
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5908
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.550
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       quader
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.921
_refine_ls_goodness_of_fit_obs   0.947
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_restrained_S_obs      0.947
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_obs          0.0401
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0717P)²+3.0901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1372
_refine_ls_wR_factor_obs         0.1131
_reflns_number_observed          2780
_reflns_number_total             3370
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b304199a.txt
_cod_data_source_block           tt1721
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+3.0901P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+3.0901P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2/n
_cod_original_formula_sum        'C11.75 H19.50 N3 O0.25 Ru0.50'
_cod_database_code               7013094
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.0000 0.5000 0.0000 0.02660(13) Uani 1 d S .
C2 C 0.0022(3) 0.5485(3) 0.1317(2) 0.0300(6) Uani 1 d . .
C1 C 0.1669(3) 0.3851(3) 0.0181(2) 0.0338(7) Uani 1 d . .
N3 N -0.1608(3) 0.2299(3) 0.0383(2) 0.0399(6) Uani 1 d . .
N2 N 0.0017(3) 0.5762(3) 0.2068(2) 0.0331(6) Uani 1 d . .
N1 N 0.2602(3) 0.3215(3) 0.0277(2) 0.0465(7) Uani 1 d . .
C7 C -0.1033(3) 0.3288(3) 0.0248(2) 0.0323(6) Uani 1 d . .
C3 C -0.0050(3) 0.6097(3) 0.3029(2) 0.0332(7) Uani 1 d . .
C8 C -0.2307(3) 0.0997(3) 0.0525(3) 0.0483(9) Uani 1 d . .
C4 C -0.0644(4) 0.7540(4) 0.3114(3) 0.0549(10) Uani 1 d . .
H4A H -0.1502(12) 0.7544(9) 0.2823(18) 0.077(5) Uiso 1 calc R .
H4B H -0.0097(15) 0.8226(6) 0.2820(18) 0.077(5) Uiso 1 calc R .
H4C H -0.0714(27) 0.7778(14) 0.3753(3) 0.077(5) Uiso 1 calc R .
C5 C 0.1321(4) 0.6108(5) 0.3422(3) 0.0532(10) Uani 1 d . .
H5A H 0.1708(11) 0.5187(10) 0.3348(20) 0.077(5) Uiso 1 calc R .
H5B H 0.1307(5) 0.6342(34) 0.4065(6) 0.077(5) Uiso 1 calc R .
H5C H 0.1831(9) 0.6803(24) 0.3106(15) 0.077(5) Uiso 1 calc R .
C6 C -0.0852(6) 0.4984(4) 0.3466(3) 0.0645(14) Uani 1 d . .
H6A H -0.0431(16) 0.4078(7) 0.3402(19) 0.077(5) Uiso 1 calc R .
H6B H -0.1708(11) 0.4955(22) 0.3172(15) 0.077(5) Uiso 1 calc R .
H6C H -0.0936(26) 0.5197(18) 0.4108(6) 0.077(5) Uiso 1 calc R .
C9 C -0.1504(6) -0.0009(6) 0.1042(6) 0.052(2) Uani 0.669(8) d P 1
H9A H -0.1344(34) 0.0343(21) 0.1655(10) 0.058(7) Uiso 0.669(8) calc PR 1
H9B H -0.0682(18) -0.0135(34) 0.0745(16) 0.058(7) Uiso 0.669(8) calc PR 1
H9C H -0.1954(19) -0.0904(14) 0.1070(25) 0.058(7) Uiso 0.669(8) calc PR 1
C10 C -0.2550(6) 0.0375(6) -0.0479(5) 0.055(2) Uani 0.669(8) d P 1
H10A H -0.3020(32) -0.0507(20) -0.0442(5) 0.058(7) Uiso 0.669(8) calc PR 1
H10B H -0.1721(6) 0.0215(37) -0.0760(10) 0.058(7) Uiso 0.669(8) calc PR 1
H10C H -0.3057(31) 0.1040(18) -0.0843(9) 0.058(7) Uiso 0.669(8) calc PR 1
C11 C -0.3593(6) 0.1322(6) 0.0894(6) 0.061(2) Uani 0.669(8) d P 1
H11A H -0.3478(6) 0.1818(37) 0.1468(14) 0.058(7) Uiso 0.669(8) calc PR 1
H11B H -0.4064(16) 0.0454(7) 0.0993(26) 0.058(7) Uiso 0.669(8) calc PR 1
H11C H -0.4081(16) 0.1907(35) 0.0465(13) 0.058(7) Uiso 0.669(8) calc PR 1
C9X C -0.1386(19) -0.0142(18) 0.0468(15) 0.074(5) Uiso 0.331(8) d P 2
H9D H -0.1012(79) -0.0145(69) -0.0131(28) 0.079(18) Uiso 0.331(8) calc PR 2
H9E H -0.1826(27) -0.1028(20) 0.0568(73) 0.079(18) Uiso 0.331(8) calc PR 2
H9F H -0.0700(56) -0.0017(62) 0.0928(49) 0.079(18) Uiso 0.331(8) calc PR 2
C10X C -0.2503(12) 0.1137(13) 0.1694(8) 0.051(3) Uiso 0.331(8) d P 2
H10D H -0.1673(22) 0.0983(101) 0.2009(9) 0.079(18) Uiso 0.331(8) calc PR 2
H10E H -0.3123(72) 0.0437(68) 0.1888(13) 0.079(18) Uiso 0.331(8) calc PR 2
H10F H -0.2822(89) 0.2068(36) 0.1837(11) 0.079(18) Uiso 0.331(8) calc PR 2
C11X C -0.3522(5) 0.1026(6) 0.0229(4) 0.073(4) Uiso 0.331(8) d P 2
H11D H -0.3787(6) 0.0089(6) 0.0039(7) 0.079(18) Uiso 0.331(8) calc PR 2
H11E H -0.3607(5) 0.1665(7) -0.0284(5) 0.079(18) Uiso 0.331(8) calc PR 2
H11F H -0.4072(5) 0.1344(9) 0.0714(4) 0.079(18) Uiso 0.331(8) calc PR 2
C12 C -0.2498(5) -0.1010(8) -0.2505(5) 0.043(2) Uani 0.50 d SPR .
C13 C 0.1326(5) 0.1798(8) 0.2539(4) 0.043(2) Uani 0.50 d PR .
H13A H 0.0599(5) 0.1164(9) 0.2616(4) 0.070(16) Uiso 0.50 calc PR .
H13B H 0.1199(5) 0.2320(7) 0.1976(5) 0.070(16) Uiso 0.50 calc PR .
H13C H 0.1380(5) 0.2448(8) 0.3047(5) 0.070(16) Uiso 0.50 calc PR .
O1 O -0.2500 0.0277(9) -0.2500 0.164(9) Uani 0.50 d SP .
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'
O O 0.0106 0.0060 '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
C7 Ru1 C7 180.0 . 3_565 ?
C7 Ru1 C2 89.83(12) . 3_565 ?
C7 Ru1 C2 90.17(12) 3_565 3_565 ?
C7 Ru1 C2 90.17(12) . . ?
C7 Ru1 C2 89.83(12) 3_565 . ?
C2 Ru1 C2 180.0 3_565 . ?
C7 Ru1 C1 89.40(12) . . ?
C7 Ru1 C1 90.60(12) 3_565 . ?
C2 Ru1 C1 89.36(12) 3_565 . ?
C2 Ru1 C1 90.64(13) . . ?
C7 Ru1 C1 90.60(12) . 3_565 ?
C7 Ru1 C1 89.40(12) 3_565 3_565 ?
C2 Ru1 C1 90.64(13) 3_565 3_565 ?
C2 Ru1 C1 89.36(12) . 3_565 ?
C1 Ru1 C1 180.0 . 3_565 ?
N2 C2 Ru1 179.0(3) . . ?
N1 C1 Ru1 179.5(3) . . ?
C7 N3 C8 177.3(3) . . ?
C2 N2 C3 177.5(3) . . ?
N3 C7 Ru1 178.9(3) . . ?
N2 C3 C6 107.6(3) . . ?
N2 C3 C4 108.1(3) . . ?
C6 C3 C4 112.2(3) . . ?
N2 C3 C5 107.7(3) . . ?
C6 C3 C5 111.2(4) . . ?
C4 C3 C5 109.8(3) . . ?
C11X C8 N3 114.0(4) . . ?
C11X C8 C9X 128.1(8) . . ?
N3 C8 C9X 107.7(8) . . ?
N3 C8 C9 111.0(3) . . ?
N3 C8 C11 109.1(3) . . ?
C9 C8 C11 116.4(5) . . ?
N3 C8 C10 104.4(3) . . ?
C9 C8 C10 107.9(5) . . ?
C11 C8 C10 107.3(5) . . ?
C11X C8 C10X 100.9(5) . . ?
N3 C8 C10X 98.6(5) . . ?
C9X C8 C10X 102.1(10) . . ?
C3 C4 H4A 109.5(2) . . ?
C3 C4 H4B 109.5(2) . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5(2) . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5(2) . . ?
C3 C5 H5B 109.5(2) . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5(2) . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5(2) . . ?
C3 C6 H6B 109.5(3) . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5(2) . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C9 H9A 109.5(4) . . ?
C8 C9 H9B 109.5(3) . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5(3) . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5(3) . . ?
C8 C10 H10B 109.5(3) . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5(3) . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5(4) . . ?
C8 C11 H11B 109.5(3) . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5(3) . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C9X H9D 109.5(9) . . ?
C8 C9X H9E 109.5(8) . . ?
H9D C9X H9E 109.5 . . ?
C8 C9X H9F 109.5(8) . . ?
H9D C9X H9F 109.5 . . ?
H9E C9X H9F 109.5 . . ?
C8 C10X H10D 109.5(4) . . ?
C8 C10X H10E 109.5(4) . . ?
H10D C10X H10E 109.5 . . ?
C8 C10X H10F 109.5(4) . . ?
H10D C10X H10F 109.5 . . ?
H10E C10X H10F 109.5 . . ?
C8 C11X H11D 109.5(3) . . ?
C8 C11X H11E 109.5(3) . . ?
H11D C11X H11E 109.5 . . ?
C8 C11X H11F 109.5(3) . . ?
H11D C11X H11F 109.5 . . ?
H11E C11X H11F 109.5 . . ?
O1 C12 C13 122.0(8) . 3 ?
O1 C12 C13 121.6(5) . 4 ?
C13 C12 C13 116.5(11) 3 4 ?
C12 C13 H13A 109.5(6) 3 . ?
C12 C13 H13B 109.5(5) 3 . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5(5) 3 . ?
H13A C13 H13C 109.47(13) . . ?
H13B C13 H13C 109.5(2) . . ?
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 C7 2.004(3) . ?
Ru1 C7 2.004(3) 3_565 ?
Ru1 C2 2.007(3) 3_565 ?
Ru1 C2 2.007(3) . ?
Ru1 C1 2.067(4) . ?
Ru1 C1 2.067(4) 3_565 ?
C2 N2 1.147(4) . ?
C1 N1 1.151(5) . ?
N3 C7 1.143(4) . ?
N3 C8 1.465(4) . ?
N2 C3 1.465(4) . ?
C3 C6 1.513(5) . ?
C3 C4 1.524(5) . ?
C3 C5 1.523(5) . ?
C8 C11X 1.325(6) . ?
C8 C9X 1.46(2) . ?
C8 C9 1.478(7) . ?
C8 C11 1.491(7) . ?
C8 C10 1.618(8) . ?
C8 C10X 1.757(13) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C9X H9D 0.98 . ?
C9X H9E 0.98 . ?
C9X H9F 0.98 . ?
C10X H10D 0.98 . ?
C10X H10E 0.98 . ?
C10X H10F 0.98 . ?
C11X H11D 0.98 . ?
C11X H11E 0.98 . ?
C11X H11F 0.98 . ?
C12 O1 1.237(11) . ?
C12 C13 1.436(10) 3 ?
C12 C13 1.441(7) 4 ?
C13 C12 1.436(13) 3 ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
