#------------------------------------------------------------------------------
#$Date: 2019-11-21 09:57:43 +0200 (Thu, 21 Nov 2019) $
#$Revision: 231121 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/60/4346002.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_4346002
loop_
_publ_author_name
'Louise A. Berben'
'Mary C. Faia'
'Nathan R. M. Crawford'
'Jeffrey R. Long'
_publ_section_title
;
 Angle-Dependent Electronic Effects in 4,4'-Bipyridine-Bridged Ru3
 Triangle and Ru4 Square Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6378
_journal_page_last               6386
_journal_paper_doi               10.1021/ic060570l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety
;
'3(C8 H20 N4 Ru1 C10 H8 N2), Cl6, 31(H2 O), (C4 H8 O)'
;
_chemical_formula_sum            'C58 H154 Cl6 N18 O32 Ru3'
_chemical_formula_weight         2131.90
_space_group_IT_number           189
_space_group_name_Hall           'P -6 -2'
_space_group_name_H-M_alt        'P -6 2 m'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -6 2 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   19.0160(13)
_cell_length_b                   19.0160(13)
_cell_length_c                   8.9761(9)
_cell_measurement_reflns_used    595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.43
_cell_volume                     2811.0(4)
_computing_cell_refinement
;
  'SMART (Siemens, 1995), SAINT (Siemens, 1995)'
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  'SAINT (Siemens, 1995), XPREP (Siemens, 1995)'
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12600
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(9)
_refine_ls_extinction_coef       0.0058(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    construct
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_obs          0.0437
_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)+(0.0693P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1120
_refine_ls_wR_factor_obs         0.1083
_reflns_number_observed          1569
_reflns_number_total             1803
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic060570lsi20060602_120415.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-62m
_cod_database_code               4346002
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z'
'x-y, -y, z'
'-x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.34198(3) 0.34198(3) 0.5000 0.0194(2) Uani 1 d S .
N1 N 0.3657(4) 0.4627(3) 0.5000 0.033(2) Uani 1 d S .
H1 H 0.3230 0.4153 0.5000 0.040 Uiso 1 calc S .
N2 N 0.3661(2) 0.3661(2) 0.7343(6) 0.0266(14) Uani 1 d S .
H2 H 0.3239 0.3239 0.6996 0.032 Uiso 1 calc S .
C1 C 0.4035(3) 0.5046(3) 0.3629(5) 0.0332(13) Uani 1 d . .
H1A H 0.4616(3) 0.5258(3) 0.3675(5) 0.040 Uiso 1 calc R .
H1B H 0.3940(3) 0.5497(3) 0.3483(5) 0.040 Uiso 1 calc R .
C2 C 0.4444(3) 0.3669(4) 0.7668(6) 0.0374(14) Uani 1 d . .
H2A H 0.4328(3) 0.3118(4) 0.7848(6) 0.045 Uiso 1 calc R .
H2B H 0.4688(3) 0.3983(4) 0.8564(6) 0.045 Uiso 1 calc R .
N3 N 0.3022(3) 0.2168(3) 0.5000 0.0186(13) Uani 1 d S .
C3 C 0.2825(5) 0.1741(3) 0.3773(7) 0.069(3) Uani 1 d . .
H3 H 0.2930(5) 0.2017(3) 0.2871(7) 0.082 Uiso 1 calc R .
C4 C 0.2469(5) 0.0904(3) 0.3734(7) 0.065(2) Uani 1 d . .
H4 H 0.2364(5) 0.0641(3) 0.2819(7) 0.077 Uiso 1 calc R .
C5 C 0.2272(4) 0.0462(4) 0.5000 0.023(2) Uani 1 d S .
Cl1 Cl 0.25006(14) 0.25006(14) 0.0000 0.0353(7) Uani 1 d S .
Cl2 Cl 0.1533(5) 0.3429(4) 0.0000 0.101(2) Uani 0.50 d SP .
O3 O 0.3333 0.6667 0.5000 0.135(10) Uani 0.98 d SP .
O1 O 0.4972(4) 0.2253(4) 0.5000 0.058(2) Uani 1 d S .
O2 O 0.2082(7) 0.0000 0.0000 0.088(4) Uani 1 d S .
O4 O 0.4483(4) 0.1562(4) 0.2235(7) 0.112(2) Uani 1 d . .
O5 O 0.3810(5) 0.0000 0.3417(28) 0.343(19) Uani 1 d S .
O21 O 0.4895(12) 0.0843(12) 0.0000 0.099(7) Uiso 0.425(15) d SP .
O22 O 0.5755(15) 0.1942(16) 0.0000 0.099(7) Uiso 0.36(2) d SP .
O24 O 0.0760(29) 0.0000 0.1338(59) 0.108(17) Uiso 0.17 d SP .
C51 C 0.0275(13) 0.0275(13) 0.3562(27) 0.070(10) Uiso 0.33 d SP .
C50 C 0.0701(20) 0.0701(20) 0.2149(35) 0.081(10) Uiso 0.33 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'
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
N3 Ru1 N3 83.7(3) 7_556 .
N3 Ru1 N1 172.6(2) 7_556 7_556
N3 Ru1 N1 88.8(2) . 7_556
N3 Ru1 N1 88.8(2) 7_556 .
N3 Ru1 N1 172.6(2) . .
N1 Ru1 N1 98.6(4) 7_556 .
N3 Ru1 N2 99.13(10) 7_556 .
N3 Ru1 N2 99.13(10) . .
N1 Ru1 N2 82.02(9) 7_556 .
N1 Ru1 N2 82.02(9) . .
N3 Ru1 N2 99.12(10) 7_556 4_556
N3 Ru1 N2 99.13(10) . 4_556
N1 Ru1 N2 82.02(9) 7_556 4_556
N1 Ru1 N2 82.02(9) . 4_556
N2 Ru1 N2 155.4(3) . 4_556
C1 N1 C1 116.6(6) . 4_556
C1 N1 Ru1 112.1(3) . .
C1 N1 Ru1 112.1(3) 4_556 .
C2 N2 C2 115.4(5) . 10
C2 N2 Ru1 107.2(3) . .
C2 N2 Ru1 107.2(3) 10 .
N1 C1 C2 108.6(4) . 7_556
N2 C2 C1 111.5(4) . 7_556
C3 N3 C3 114.8(6) 4_556 .
C3 N3 Ru1 122.1(3) 4_556 .
C3 N3 Ru1 122.1(3) . .
N3 C3 C4 124.0(6) . .
C5 C4 C3 121.2(6) . .
C4 C5 C4 114.6(7) 4_556 .
C4 C5 C5 122.6(3) 4_556 8_556
C4 C5 C5 122.6(3) . 8_556
C50 O24 C50 94.6(42) 3 .
C51 C51 C51 59.998(8) 2 3
C51 C51 C50 117.8(14) 2 .
C51 C51 C50 117.8(14) 3 .
C51 C50 O24 100.4(24) . 2
C51 C50 O24 100.4(24) . .
O24 C50 O24 105.6(45) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N3 2.106(5) 7_556
Ru1 N3 2.106(5) .
Ru1 N1 2.106(6) 7_556
Ru1 N1 2.106(6) .
Ru1 N2 2.152(5) .
Ru1 N2 2.152(5) 4_556
N1 C1 1.447(5) .
N1 C1 1.447(6) 4_556
N2 C2 1.511(6) .
N2 C2 1.511(6) 10
C1 C2 1.534(7) 7_556
C2 C1 1.534(7) 7_556
N3 C3 1.307(6) 4_556
N3 C3 1.307(6) .
C3 C4 1.385(7) .
C4 C5 1.351(7) .
C5 C4 1.351(7) 4_556
C5 C5 1.521(13) 8_556
O24 C50 1.57(4) 3
O24 C50 1.57(4) .
C51 C51 0.91(4) 2
C51 C51 0.91(4) 3
C51 C50 1.50(4) .
C50 O24 1.57(4) 2
