#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/01/4300109.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_4300109
loop_
_publ_author_name
'Dusan Hesek'
'Yoshihisa Inoue'
'Simon R. L. Everitt'
'Hitoshi Ishida'
'Mieko Kunieda'
'Michael G. B. Drew'
_publ_section_title
;
Novel Synthetic Routes to Several New, Differentially Substituted Ruthenium
Tris(4,4'-disubstituted-2,2-bipyridine) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              308
_journal_page_last               316
_journal_paper_doi               10.1021/ic990840i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C12 H11 Cl3 N3 Ru'
_chemical_formula_weight         404.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.640(10)
_cell_angle_beta                 88.380(10)
_cell_angle_gamma                86.390(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0930(10)
_cell_length_b                   12.9750(10)
_cell_length_c                   6.9140(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     723.72(15)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    'PLATON (Spek, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0085
_diffrn_reflns_av_sigmaI/netI    0.2437
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3618
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -0.22
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          1.131
_refine_ls_shift/su_mean         0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0720P)²+0.7577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2679
_reflns_number_total             3305
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.7577P] 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^)+(0.0720P)^2^+0.7577P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C12 H11 Cl3 N3 Ru              '
_cod_database_code               4300109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.13187(3) 0.22676(2) 0.81492(4) 0.02483(12) Uani 1 d . . .
Cl1 Cl 0.20729(12) 0.37073(8) 0.98151(14) 0.0332(2) Uani 1 d . . .
Cl2 Cl 0.04405(18) 0.08398(9) 0.66556(19) 0.0497(3) Uani 1 d . . .
Cl3 Cl 0.37318(13) 0.23264(9) 0.61325(16) 0.0420(3) Uani 1 d . . .
N11 N -0.0183(4) 0.3194(2) 0.6384(4) 0.0252(6) Uani 1 d . . .
C12 C 0.0215(5) 0.3550(3) 0.4585(5) 0.0284(7) Uani 1 d . . .
H12 H 0.1249 0.3353 0.4051 0.034 Uiso 1 calc R . .
C13 C -0.0854(5) 0.4194(3) 0.3506(6) 0.0336(8) Uani 1 d . . .
H13 H -0.0556 0.4417 0.2257 0.040 Uiso 1 calc R . .
C14 C -0.2380(6) 0.4504(4) 0.4315(7) 0.0440(11) Uani 1 d . . .
H14 H -0.3096 0.4972 0.3646 0.053 Uiso 1 calc R . .
C15 C -0.2827(5) 0.4108(4) 0.6127(7) 0.0430(10) Uani 1 d . . .
H15 H -0.3871 0.4278 0.6661 0.052 Uiso 1 calc R . .
C16 C -0.1712(5) 0.3459(3) 0.7141(6) 0.0304(8) Uani 1 d . . .
C17 C -0.2093(5) 0.2942(3) 0.9029(6) 0.0321(8) Uani 1 d . . .
C18 C -0.3616(5) 0.3064(4) 0.9998(7) 0.0432(10) Uani 1 d . . .
H18 H -0.4456 0.3503 0.9476 0.052 Uiso 1 calc R . .
C19 C -0.3879(5) 0.2532(4) 1.1735(7) 0.0442(11) Uani 1 d . . .
H19 H -0.4892 0.2608 1.2400 0.053 Uiso 1 calc R . .
C20 C -0.2607(6) 0.1886(4) 1.2465(7) 0.0457(11) Uani 1 d . . .
H20 H -0.2759 0.1514 1.3628 0.055 Uiso 1 calc R . .
C21 C -0.1106(6) 0.1793(4) 1.1464(6) 0.0404(10) Uani 1 d . . .
H21 H -0.0255 0.1356 1.1967 0.049 Uiso 1 calc R . .
N22 N -0.0847(4) 0.2322(3) 0.9773(5) 0.0299(7) Uani 1 d . . .
N100 N 0.2605(4) 0.1295(3) 1.0078(5) 0.0344(7) Uani 1 d . . .
C101 C 0.3160(6) 0.0747(4) 1.1222(7) 0.0409(10) Uani 1 d . . .
C102 C 0.3813(7) 0.0036(5) 1.2728(8) 0.0575(14) Uani 1 d . . .
H10A H 0.3429 -0.0638 1.2556 0.069 Uiso 1 calc R . .
H10B H 0.3441 0.0275 1.3972 0.069 Uiso 1 calc R . .
H10C H 0.5001 0.0003 1.2652 0.069 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 0 1
1 -2 1
1 2 1
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 Ru1 N22 79.32(13) . . ?
N11 Ru1 N100 174.01(13) . . ?
N22 Ru1 N100 94.90(14) . . ?
N11 Ru1 Cl2 88.96(10) . . ?
N22 Ru1 Cl2 88.83(10) . . ?
N100 Ru1 Cl2 89.38(11) . . ?
N11 Ru1 Cl1 91.13(9) . . ?
N22 Ru1 Cl1 87.59(10) . . ?
N100 Ru1 Cl1 90.15(11) . . ?
Cl2 Ru1 Cl1 176.34(4) . . ?
N11 Ru1 Cl3 96.26(9) . . ?
N22 Ru1 Cl3 175.34(10) . . ?
N100 Ru1 Cl3 89.56(10) . . ?
Cl2 Ru1 Cl3 92.57(5) . . ?
Cl1 Ru1 Cl3 91.06(4) . . ?
C12 N11 C16 118.7(3) . . ?
C12 N11 Ru1 126.0(3) . . ?
C16 N11 Ru1 115.3(2) . . ?
N11 C12 C13 122.4(4) . . ?
C12 C13 C14 118.8(4) . . ?
C15 C14 C13 119.1(4) . . ?
C16 C15 C14 119.5(4) . . ?
N11 C16 C15 121.2(4) . . ?
N11 C16 C17 114.5(3) . . ?
C15 C16 C17 124.1(4) . . ?
N22 C17 C18 121.1(4) . . ?
N22 C17 C16 115.2(3) . . ?
C18 C17 C16 123.6(4) . . ?
C19 C18 C17 119.8(4) . . ?
C18 C19 C20 118.5(4) . . ?
C19 C20 C21 119.8(4) . . ?
N22 C21 C20 121.5(4) . . ?
C21 N22 C17 119.2(4) . . ?
C21 N22 Ru1 125.6(3) . . ?
C17 N22 Ru1 115.2(3) . . ?
C101 N100 Ru1 173.1(4) . . ?
N100 C101 C102 177.8(5) . . ?
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 N11 2.047(3) . ?
Ru1 N22 2.054(3) . ?
Ru1 N100 2.057(3) . ?
Ru1 Cl2 2.3170(12) . ?
Ru1 Cl1 2.3556(11) . ?
Ru1 Cl3 2.3707(10) . ?
N11 C12 1.346(5) . ?
N11 C16 1.359(5) . ?
C12 C13 1.377(5) . ?
C13 C14 1.384(6) . ?
C14 C15 1.382(6) . ?
C15 C16 1.381(6) . ?
C16 C17 1.477(5) . ?
C17 N22 1.349(5) . ?
C17 C18 1.390(6) . ?
C18 C19 1.378(6) . ?
C19 C20 1.380(7) . ?
C20 C21 1.382(6) . ?
C21 N22 1.348(5) . ?
N100 C101 1.125(5) . ?
C101 C102 1.450(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660688
