#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:56:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179270 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/90/4319061.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_4319061
loop_
_publ_author_name
'Chayan Das'
'Amit K. Ghosh'
'Chen-Hsiung Hung'
'Gene-Hsiang Lee'
'Shie-Ming Peng'
'Sreebrata Goswami'
_publ_section_title
;
 Metal-Promoted Aromatic Ring Amination and Deamination Reactions at a
 Diazo Ligand Coordinated to Rhodium and Ruthenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7125
_journal_page_last               7135
_journal_paper_doi               10.1021/ic020421c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C28 H22 Cl N7 Ru'
_chemical_formula_weight         593.05
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.83(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.481(7)
_cell_length_b                   14.377(9)
_cell_length_c                   13.543(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2624(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4470
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.730
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.950
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.544
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0398P)²+12.2275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2000
_refine_ls_wR_factor_obs         0.1151
_reflns_number_observed          3072
_reflns_number_total             4027
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020421c_4.cif
_cod_data_source_block           '[RuCl(pap)(L1a)],(5a)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+12.2275P] 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^)+(0.0398P)^2^+12.2275P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2623.4(25)
_cod_database_code               4319061
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru Ru 0.00414(4) 0.79799(3) 0.29359(4) 0.0422(2) Uani 1 d . .
N6 N 0.0303(4) 0.6008(4) 0.3080(4) 0.0472(13) Uani 1 d . .
N3 N -0.1020(4) 0.8592(3) 0.3608(4) 0.0424(12) Uani 1 d . .
N4 N -0.0965(4) 0.8101(4) 0.1788(4) 0.0487(13) Uani 1 d . .
N5 N 0.1130(4) 0.7198(4) 0.2285(4) 0.0499(14) Uani 1 d . .
N2 N -0.0939(4) 0.8835(4) 0.4541(4) 0.0462(13) Uani 1 d . .
N7 N -0.0256(4) 0.6717(3) 0.3317(4) 0.0415(12) Uani 1 d . .
N1 N 0.0693(4) 0.8285(4) 0.4316(4) 0.0481(13) Uani 1 d . .
Cl Cl 0.07366(14) 0.94143(12) 0.23923(14) 0.0638(5) Uani 1 d . .
C1 C 0.1630(5) 0.8210(5) 0.4665(6) 0.061(2) Uani 1 d . .
H1A H 0.2108(5) 0.7970(5) 0.4255(6) 0.073 Uiso 1 calc R .
C2 C 0.1909(6) 0.8476(6) 0.5601(6) 0.071(2) Uani 1 d . .
H2A H 0.2566(6) 0.8413(6) 0.5822(6) 0.085 Uiso 1 calc R .
C3 C 0.1214(6) 0.8835(5) 0.6215(6) 0.067(2) Uani 1 d . .
H3A H 0.1393(6) 0.9014(5) 0.6856(6) 0.080 Uiso 1 calc R .
C4 C 0.0261(5) 0.8927(5) 0.5871(5) 0.058(2) Uani 1 d . .
H4A H -0.0219(5) 0.9165(5) 0.6280(5) 0.070 Uiso 1 calc R .
C5 C 0.0000(5) 0.8662(4) 0.4901(5) 0.0463(15) Uani 1 d . .
C6 C -0.1868(4) 0.8794(4) 0.3062(5) 0.0456(15) Uani 1 d . .
C7 C -0.2712(5) 0.9203(5) 0.3452(5) 0.055(2) Uani 1 d . .
H7A H -0.2729(5) 0.9350(5) 0.4120(5) 0.066 Uiso 1 calc R .
C8 C -0.3503(5) 0.9383(5) 0.2842(6) 0.066(2) Uani 1 d . .
H8A H -0.4068(5) 0.9662(5) 0.3085(6) 0.079 Uiso 1 calc R .
C9 C -0.3464(5) 0.9145(5) 0.1836(6) 0.063(2) Uani 1 d . .
H9A H -0.4014(5) 0.9261(5) 0.1424(6) 0.076 Uiso 1 calc R .
C10 C -0.2646(5) 0.8750(5) 0.1447(5) 0.057(2) Uani 1 d . .
H10A H -0.2640(5) 0.8615(5) 0.0776(5) 0.068 Uiso 1 calc R .
C11 C -0.1799(5) 0.8542(4) 0.2064(5) 0.048(2) Uani 1 d . .
C12 C -0.0785(5) 0.7924(5) 0.0778(5) 0.052(2) Uani 1 d . .
C13 C -0.0817(6) 0.8620(6) 0.0076(6) 0.076(2) Uani 1 d . .
H13A H -0.0957(6) 0.9229(6) 0.0258(6) 0.091 Uiso 1 calc R .
C14 C -0.0638(8) 0.8407(8) -0.0902(7) 0.097(3) Uani 1 d . .
H14A H -0.0675(8) 0.8875(8) -0.1376(7) 0.117 Uiso 1 calc R .
C15 C -0.0415(8) 0.7540(9) -0.1175(7) 0.099(3) Uani 1 d . .
H15A H -0.0312(8) 0.7409(9) -0.1836(7) 0.119 Uiso 1 calc R .
C16 C -0.0334(7) 0.6842(7) -0.0483(7) 0.088(3) Uani 1 d . .
H16A H -0.0161(7) 0.6242(7) -0.0668(7) 0.105 Uiso 1 calc R .
C17 C -0.0516(5) 0.7046(5) 0.0492(6) 0.063(2) Uani 1 d . .
H17A H -0.0455(5) 0.6578(5) 0.0964(6) 0.076 Uiso 1 calc R .
C18 C 0.1839(5) 0.7468(6) 0.1679(6) 0.069(2) Uani 1 d . .
H18A H 0.1905(5) 0.8098(6) 0.1540(6) 0.083 Uiso 1 calc R .
C19 C 0.2471(6) 0.6852(6) 0.1255(6) 0.077(2) Uani 1 d . .
H19A H 0.2939(6) 0.7061(6) 0.0818(6) 0.093 Uiso 1 calc R .
C20 C 0.2408(6) 0.5928(6) 0.1479(6) 0.073(2) Uani 1 d . .
H20A H 0.2850(6) 0.5505(6) 0.1217(6) 0.087 Uiso 1 calc R .
C21 C 0.1692(5) 0.5634(5) 0.2091(5) 0.063(2) Uani 1 d . .
H21A H 0.1632(5) 0.5005(5) 0.2238(5) 0.076 Uiso 1 calc R .
C22 C 0.1053(5) 0.6269(5) 0.2492(5) 0.0468(15) Uani 1 d . .
C23 C -0.1051(4) 0.6436(4) 0.3926(5) 0.0428(15) Uani 1 d . .
C24 C -0.0842(6) 0.6004(5) 0.4816(5) 0.062(2) Uani 1 d . .
H24A H -0.0188(6) 0.5914(5) 0.5037(5) 0.074 Uiso 1 calc R .
C25 C -0.1611(8) 0.5712(6) 0.5369(6) 0.084(3) Uani 1 d . .
H25A H -0.1477(8) 0.5416(6) 0.5969(6) 0.101 Uiso 1 calc R .
C26 C -0.2563(8) 0.5843(6) 0.5063(8) 0.086(3) Uani 1 d . .
H26A H -0.3078(8) 0.5639(6) 0.5450(8) 0.103 Uiso 1 calc R .
C27 C -0.2767(6) 0.6275(6) 0.4185(7) 0.077(2) Uani 1 d . .
H27A H -0.3424(6) 0.6365(6) 0.3975(7) 0.092 Uiso 1 calc R .
C28 C -0.2015(5) 0.6581(5) 0.3602(6) 0.056(2) Uani 1 d . .
H28A H -0.2156(5) 0.6879(5) 0.3004(6) 0.068 Uiso 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'
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
N3 Ru N7 98.0(2) . . y
N3 Ru N4 80.5(2) . . y
N7 Ru N4 98.3(2) . . y
N3 Ru N5 174.0(2) . . y
N7 Ru N5 76.1(2) . . y
N4 Ru N5 100.7(2) . . y
N3 Ru N1 77.3(2) . . y
N7 Ru N1 92.5(2) . . y
N4 Ru N1 156.4(2) . . y
N5 Ru N1 102.2(2) . . y
N3 Ru Cl 93.2(2) . . y
N7 Ru Cl 168.24(14) . . y
N4 Ru Cl 87.1(2) . . y
N5 Ru Cl 92.7(2) . . y
N1 Ru Cl 86.37(15) . . y
N7 N6 C22 111.8(5) . . ?
N2 N3 C6 120.4(5) . . ?
N2 N3 Ru 122.3(4) . . ?
C6 N3 Ru 117.3(4) . . ?
C11 N4 C12 121.2(6) . . ?
C11 N4 Ru 111.6(4) . . ?
C12 N4 Ru 126.1(4) . . ?
C18 N5 C22 118.0(6) . . ?
C18 N5 Ru 129.4(5) . . ?
C22 N5 Ru 112.6(4) . . ?
N3 N2 C5 110.1(5) . . ?
N6 N7 C23 111.5(5) . . ?
N6 N7 Ru 122.6(4) . . ?
C23 N7 Ru 125.8(4) . . ?
C1 N1 C5 119.1(6) . . ?
C1 N1 Ru 131.7(5) . . ?
C5 N1 Ru 109.2(4) . . ?
N1 C1 C2 122.3(7) . . ?
C1 C2 C3 119.6(7) . . ?
C4 C3 C2 119.0(7) . . ?
C3 C4 C5 120.0(7) . . ?
N1 C5 N2 120.9(6) . . ?
N1 C5 C4 119.9(6) . . ?
N2 C5 C4 119.1(6) . . ?
N3 C6 C11 112.6(5) . . ?
N3 C6 C7 124.0(6) . . ?
C11 C6 C7 123.4(6) . . ?
C8 C7 C6 119.0(7) . . ?
C7 C8 C9 119.4(7) . . ?
C10 C9 C8 122.2(7) . . ?
C9 C10 C11 120.3(7) . . ?
N4 C11 C6 117.9(6) . . ?
N4 C11 C10 126.4(6) . . ?
C6 C11 C10 115.7(6) . . ?
C17 C12 C13 118.4(7) . . ?
C17 C12 N4 119.5(6) . . ?
C13 C12 N4 122.0(7) . . ?
C12 C13 C14 119.6(9) . . ?
C15 C14 C13 121.2(9) . . ?
C14 C15 C16 120.3(9) . . ?
C15 C16 C17 118.9(9) . . ?
C12 C17 C16 121.4(8) . . ?
N5 C18 C19 122.4(7) . . ?
C20 C19 C18 119.6(7) . . ?
C21 C20 C19 119.2(7) . . ?
C20 C21 C22 119.9(7) . . ?
N6 C22 N5 116.9(5) . . ?
N6 C22 C21 122.2(6) . . ?
N5 C22 C21 120.9(6) . . ?
C24 C23 C28 120.9(6) . . ?
C24 C23 N7 119.7(6) . . ?
C28 C23 N7 119.4(6) . . ?
C25 C24 C23 118.7(8) . . ?
C26 C25 C24 121.4(8) . . ?
C25 C26 C27 119.6(8) . . ?
C28 C27 C26 121.0(8) . . ?
C27 C28 C23 118.3(7) . . ?
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
Ru N3 1.933(5) . y
Ru N7 1.933(5) . y
Ru N4 2.038(6) . y
Ru N5 2.068(5) . y
Ru N1 2.086(6) . y
Ru Cl 2.391(2) . y
N6 N7 1.314(7) . ?
N6 C22 1.360(8) . ?
N3 N2 1.312(7) . ?
N3 C6 1.372(8) . ?
N4 C11 1.353(8) . ?
N4 C12 1.421(8) . ?
N5 C18 1.338(8) . ?
N5 C22 1.368(8) . ?
N2 C5 1.364(8) . ?
N7 C23 1.432(7) . ?
N1 C1 1.338(8) . ?
N1 C5 1.357(8) . ?
C1 C2 1.365(11) . ?
C2 C3 1.374(11) . ?
C3 C4 1.359(10) . ?
C4 C5 1.402(9) . ?
C6 C11 1.406(9) . ?
C6 C7 1.400(8) . ?
C7 C8 1.353(10) . ?
C8 C9 1.407(11) . ?
C9 C10 1.362(10) . ?
C10 C11 1.425(9) . ?
C12 C17 1.372(10) . ?
C12 C13 1.380(10) . ?
C13 C14 1.388(12) . ?
C14 C15 1.337(14) . ?
C15 C16 1.375(14) . ?
C16 C17 1.382(11) . ?
C18 C19 1.367(10) . ?
C19 C20 1.366(11) . ?
C20 C21 1.359(10) . ?
C21 C22 1.379(9) . ?
C23 C24 1.378(9) . ?
C23 C28 1.374(9) . ?
C24 C25 1.365(11) . ?
C25 C26 1.349(13) . ?
C26 C27 1.363(13) . ?
C27 C28 1.377(10) . ?
