#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/37/7003736.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_7003736
loop_
_publ_author_name
'Drew, Michael G. B.'
'Nag, Samik'
'Datta, Dipankar'
_publ_section_title
;
 Use of HNO3 as the source of NO to prepare a nitric oxide complex of
 ruthenium
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2298
_journal_page_last               2302
_journal_paper_doi               10.1039/b719134k
_journal_year                    2008
_chemical_formula_sum            'C20 H32 N6 O8 Ru'
_chemical_formula_weight         585.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.170(3)
_cell_length_b                   11.896(2)
_cell_length_c                   10.1839(14)
_cell_measurement_temperature    150(2)
_cell_volume                     2443.5(6)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16354
_diffrn_reflns_theta_full        30.15
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1.245
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5647
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0578P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                3411
_reflns_number_total             5647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719134k.txt
_cod_data_source_block           2
_cod_original_cell_volume        2443.6(7)
_cod_original_sg_symbol_H-M      Pna21
_cod_original_formula_sum        'C20 H32 N6 O8 Ru '
_cod_database_code               7003736
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.2884(2) 0.8129(3) 0.6324(4) 0.0199(9) Uani 1 1 d . . .
C13 C 0.3123(2) 0.7952(4) 0.4893(5) 0.0257(10) Uani 1 1 d . . .
H13A H 0.3163 0.8666 0.4441 0.031 Uiso 1 1 calc R . .
H13B H 0.3551 0.7578 0.4879 0.031 Uiso 1 1 calc R . .
O14 O 0.26088(18) 0.7239(3) 0.4265(4) 0.0263(9) Uani 1 1 d . . .
C15 C 0.2139(2) 0.7153(4) 0.5165(5) 0.0197(9) Uani 1 1 d . . .
C16 C 0.1532(2) 0.6537(4) 0.4893(5) 0.0195(9) Uani 1 1 d . . .
O17 O 0.14860(16) 0.5897(3) 0.3835(3) 0.0248(7) Uani 1 1 d . . .
C18 C 0.0799(2) 0.5507(4) 0.3855(5) 0.0320(12) Uani 1 1 d . . .
H18A H 0.0777 0.4707 0.3675 0.038 Uiso 1 1 calc R . .
H18B H 0.0538 0.5903 0.3203 0.038 Uiso 1 1 calc R . .
C19 C 0.0545(2) 0.5762(4) 0.5242(5) 0.0242(10) Uani 1 1 d . . .
C32 C 0.0751(2) 0.9815(4) 0.5777(4) 0.0241(10) Uani 1 1 d . . .
C33 C 0.0847(2) 1.1050(4) 0.6182(5) 0.0318(11) Uani 1 1 d . . .
H33A H 0.1188 1.1405 0.5653 0.038 Uiso 1 1 calc R . .
H33B H 0.0437 1.1468 0.6086 0.038 Uiso 1 1 calc R . .
O34 O 0.10504(15) 1.0996(2) 0.7574(4) 0.0291(7) Uani 1 1 d . . .
C35 C 0.1204(2) 0.9913(3) 0.7771(4) 0.0193(10) Uani 1 1 d . . .
C36 C 0.1472(2) 0.9494(3) 0.9001(4) 0.0194(9) Uani 1 1 d . . .
O37 O 0.15866(16) 1.0167(3) 1.0018(3) 0.0277(7) Uani 1 1 d . . .
C39 C 0.1808(2) 0.8242(4) 1.0480(4) 0.0226(9) Uani 1 1 d . . .
C121 C 0.33048(18) 0.7449(4) 0.7310(7) 0.0321(11) Uani 1 1 d . . .
H12A H 0.3319 0.6676 0.7042 0.048 Uiso 1 1 calc R . .
H12B H 0.3110 0.7501 0.8168 0.048 Uiso 1 1 calc R . .
H12C H 0.3747 0.7748 0.7334 0.048 Uiso 1 1 calc R . .
C122 C 0.2850(2) 0.9357(4) 0.6693(5) 0.0332(12) Uani 1 1 d . . .
H12D H 0.2587 0.9754 0.6059 0.050 Uiso 1 1 calc R . .
H12E H 0.3289 0.9667 0.6708 0.050 Uiso 1 1 calc R . .
H12F H 0.2652 0.9432 0.7546 0.050 Uiso 1 1 calc R . .
C191 C 0.0578(2) 0.4736(4) 0.6128(5) 0.0310(11) Uani 1 1 d . . .
H19A H 0.0421 0.4931 0.6988 0.046 Uiso 1 1 calc R . .
H19B H 0.1028 0.4478 0.6185 0.046 Uiso 1 1 calc R . .
H19C H 0.0305 0.4150 0.5770 0.046 Uiso 1 1 calc R . .
C192 C -0.0157(2) 0.6259(4) 0.5185(6) 0.0361(13) Uani 1 1 d . . .
H19D H -0.0160 0.6898 0.4610 0.054 Uiso 1 1 calc R . .
H19E H -0.0292 0.6487 0.6049 0.054 Uiso 1 1 calc R . .
H19F H -0.0460 0.5701 0.4859 0.054 Uiso 1 1 calc R . .
C321 C 0.0027(2) 0.9478(4) 0.5773(6) 0.0359(12) Uani 1 1 d . . .
H32A H -0.0163 0.9627 0.6620 0.054 Uiso 1 1 calc R . .
H32B H -0.0010 0.8691 0.5580 0.054 Uiso 1 1 calc R . .
H32C H -0.0205 0.9903 0.5117 0.054 Uiso 1 1 calc R . .
C381 C 0.1956(2) 0.9448(4) 1.0941(5) 0.0341(12) Uani 1 1 d . . .
H38A H 0.1804 0.9563 1.1834 0.041 Uiso 1 1 calc R . .
H38B H 0.2427 0.9604 1.0900 0.041 Uiso 1 1 calc R . .
C391 C 0.1211(2) 0.7727(4) 1.1203(5) 0.0283(12) Uani 1 1 d . . .
H39A H 0.1125 0.6989 1.0862 0.042 Uiso 1 1 calc R . .
H39B H 0.0829 0.8194 1.1074 0.042 Uiso 1 1 calc R . .
H39C H 0.1308 0.7677 1.2124 0.042 Uiso 1 1 calc R . .
C392 C 0.2419(3) 0.7493(4) 1.0611(5) 0.0309(13) Uani 1 1 d . . .
H39D H 0.2784 0.7827 1.0147 0.046 Uiso 1 1 calc R . .
H39E H 0.2326 0.6765 1.0247 0.046 Uiso 1 1 calc R . .
H39F H 0.2533 0.7414 1.1522 0.046 Uiso 1 1 calc R . .
O42 O 0.01574(14) 0.8307(3) 0.8818(3) 0.0297(8) Uani 1 1 d . . .
O43 O 0.00623(15) 0.6570(3) 0.8306(4) 0.0325(8) Uani 1 1 d . . .
O52 O 0.13442(17) 0.5630(3) 0.9250(4) 0.0309(8) Uani 1 1 d . . .
O53 O 0.20036(15) 0.5420(2) 0.7636(4) 0.0360(9) Uani 1 1 d . . .
N11 N 0.22065(15) 0.7611(3) 0.6294(3) 0.0172(7) Uani 1 1 d . . .
Ru1 Ru 0.130540(10) 0.75042(3) 0.74515(11) 0.01294(7) Uani 1 1 d . . .
N20 N 0.10537(16) 0.6607(3) 0.5726(4) 0.0171(7) Uani 1 1 d . . .
N41 N 0.04015(16) 0.7443(3) 0.8305(4) 0.0194(7) Uani 1 1 d . . .
N51 N 0.15753(18) 0.6005(3) 0.8199(4) 0.0210(8) Uani 1 1 d . . .
N31 N 0.10882(16) 0.9201(3) 0.6854(4) 0.0189(8) Uani 1 1 d . . .
N40 N 0.16121(17) 0.8450(3) 0.9074(3) 0.0186(8) Uani 1 1 d . . .
C322 C 0.1086(3) 0.9591(5) 0.4468(6) 0.0426(14) Uani 1 1 d . . .
H32D H 0.1542 0.9819 0.4515 0.064 Uiso 1 1 calc R . .
H32E H 0.0865 1.0009 0.3791 0.064 Uiso 1 1 calc R . .
H32F H 0.1063 0.8803 0.4271 0.064 Uiso 1 1 calc R . .
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'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 '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
N11 C12 C122 111.2(3) . . ?
N11 C12 C121 107.4(3) . . ?
C122 C12 C121 111.7(4) . . ?
N11 C12 C13 102.1(3) . . ?
C122 C12 C13 112.3(4) . . ?
C121 C12 C13 111.7(4) . . ?
O14 C13 C12 105.4(3) . . ?
C15 O14 C13 104.3(4) . . ?
N11 C15 O14 120.9(4) . . ?
N11 C15 C16 118.4(4) . . ?
O14 C15 C16 120.7(4) . . ?
N20 C16 O17 121.4(4) . . ?
N20 C16 C15 118.2(4) . . ?
O17 C16 C15 120.3(4) . . ?
C16 O17 C18 103.8(3) . . ?
O17 C18 C19 105.5(3) . . ?
N20 C19 C191 108.1(4) . . ?
N20 C19 C18 101.8(3) . . ?
C191 C19 C18 111.9(4) . . ?
N20 C19 C192 112.4(4) . . ?
C191 C19 C192 111.8(4) . . ?
C18 C19 C192 110.4(4) . . ?
N31 C32 C322 111.0(4) . . ?
N31 C32 C321 108.3(4) . . ?
C322 C32 C321 112.4(4) . . ?
N31 C32 C33 102.4(3) . . ?
C322 C32 C33 110.3(4) . . ?
C321 C32 C33 112.0(4) . . ?
O34 C33 C32 104.5(3) . . ?
C35 O34 C33 104.5(3) . . ?
N31 C35 O34 118.9(4) . . ?
N31 C35 C36 118.0(4) . . ?
O34 C35 C36 123.1(4) . . ?
N40 C36 O37 120.2(4) . . ?
N40 C36 C35 117.8(4) . . ?
O37 C36 C35 122.0(4) . . ?
C36 O37 C381 103.6(3) . . ?
N40 C39 C381 100.8(4) . . ?
N40 C39 C392 113.0(4) . . ?
C381 C39 C392 111.2(4) . . ?
N40 C39 C391 108.4(4) . . ?
C381 C39 C391 112.1(4) . . ?
C392 C39 C391 111.0(4) . . ?
O37 C381 C39 104.4(4) . . ?
C15 N11 C12 106.8(3) . . ?
C15 N11 Ru1 112.0(3) . . ?
C12 N11 Ru1 141.0(3) . . ?
N51 Ru1 N41 92.84(16) . . ?
N51 Ru1 N40 95.63(15) . . ?
N41 Ru1 N40 86.92(15) . . ?
N51 Ru1 N20 86.09(14) . . ?
N41 Ru1 N20 97.05(14) . . ?
N40 Ru1 N20 175.61(14) . . ?
N51 Ru1 N31 172.71(15) . . ?
N41 Ru1 N31 88.37(14) . . ?
N40 Ru1 N31 77.25(13) . . ?
N20 Ru1 N31 100.91(14) . . ?
N51 Ru1 N11 91.75(14) . . ?
N41 Ru1 N11 172.44(15) . . ?
N40 Ru1 N11 98.61(13) . . ?
N20 Ru1 N11 77.27(13) . . ?
N31 Ru1 N11 87.83(13) . . ?
C16 N20 C19 104.5(4) . . ?
C16 N20 Ru1 113.6(3) . . ?
C19 N20 Ru1 139.9(3) . . ?
O43 N41 O42 118.0(3) . . ?
O43 N41 Ru1 121.7(3) . . ?
O42 N41 Ru1 120.3(3) . . ?
O53 N51 O52 116.9(4) . . ?
O53 N51 Ru1 120.5(3) . . ?
O52 N51 Ru1 122.6(3) . . ?
C35 N31 C32 107.3(3) . . ?
C35 N31 Ru1 112.1(3) . . ?
C32 N31 Ru1 139.8(3) . . ?
C36 N40 C39 105.9(4) . . ?
C36 N40 Ru1 114.3(3) . . ?
C39 N40 Ru1 137.7(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
C12 N11 1.500(5) . ?
C12 C122 1.510(6) . ?
C12 C121 1.544(7) . ?
C12 C13 1.549(6) . ?
C13 O14 1.485(5) . ?
O14 C15 1.322(5) . ?
C15 N11 1.280(6) . ?
C15 C16 1.454(6) . ?
C16 N20 1.288(6) . ?
C16 O17 1.322(5) . ?
O17 C18 1.461(5) . ?
C18 C19 1.533(6) . ?
C19 N20 1.518(5) . ?
C19 C191 1.519(6) . ?
C19 C192 1.536(6) . ?
C32 N31 1.483(5) . ?
C32 C322 1.517(7) . ?
C32 C321 1.514(6) . ?
C32 C33 1.539(6) . ?
C33 O34 1.477(6) . ?
O34 C35 1.341(5) . ?
C35 N31 1.283(5) . ?
C35 C36 1.452(6) . ?
C36 N40 1.276(5) . ?
C36 O37 1.329(5) . ?
O37 C381 1.473(6) . ?
C39 N40 1.506(5) . ?
C39 C381 1.538(6) . ?
C39 C392 1.527(6) . ?
C39 C391 1.538(6) . ?
O42 N41 1.254(4) . ?
O43 N41 1.244(4) . ?
O52 N51 1.250(5) . ?
O53 N51 1.248(4) . ?
N11 Ru1 2.170(3) . ?
Ru1 N51 2.014(4) . ?
Ru1 N41 2.021(3) . ?
Ru1 N40 2.092(4) . ?
Ru1 N20 2.118(4) . ?
Ru1 N31 2.153(3) . ?
