#------------------------------------------------------------------------------
#$Date: 2020-03-05 02:15:54 +0200 (Thu, 05 Mar 2020) $
#$Revision: 248975 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/34/7703451.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_7703451
loop_
_publ_author_name
'Yoshida, Jun'
'Tateyama, Kazunori'
'Yuge, Hidetaka'
_publ_section_title
;
 Tris(tropolonato) ruthenium as a hub for connecting π-conjugated
 systems.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2102
_journal_page_last               2111
_journal_paper_doi               10.1039/c9dt04860j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C37 H23 O6 Ru, 2(C H Cl3)'
_chemical_formula_sum            'C39 H25 Cl6 O6 Ru'
_chemical_formula_weight         903.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-20 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5500(4)
_cell_length_b                   10.6232(2)
_cell_length_c                   14.7279(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    173
_cell_measurement_theta_max      77.2390
_cell_measurement_theta_min      3.6710
_cell_volume                     3816.94(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00   2.00   0.50    0.82    --  -47.94 109.00  46.00  176
  2  ω    -71.00 -13.00   0.50    3.26    --  -86.25  37.00  30.00  116
  3  ω    -85.00 -13.00   0.50    3.26    --  -86.25 109.00  46.00  144
  4  ω    -71.00 -13.00   0.50    3.26    --  -86.25  37.00-120.00  116
  5  ω    -60.00  25.00   0.50    0.82    --  -47.94  37.00-180.00  170
  6  ω     19.00  87.00   0.50    0.82    --   47.94-109.00 -49.00  136
  7  ω     35.00 111.00   0.50    3.26    --  107.75-109.00 -49.00  152
  8  ω     35.00  71.00   0.50    3.26    --  107.75 -37.00 -30.00   72
  9  ω     35.00  60.00   0.50    3.26    --  107.75 -37.00  30.00   50
 10  ω     36.00  74.00   0.50    3.26    --  107.75 -57.00  90.00   76
 11  ω     35.00 131.00   0.50    3.26    --  107.75 -77.00 150.00  192
 12  ω     83.00 116.00   0.50    3.26    --  107.75-125.00 120.00   66
 13  ω     35.00  68.00   0.50    3.26    --  107.75 -37.00 150.00   66
 14  ω     36.00  70.00   0.50    3.26    --  107.75 -37.00  90.00   68
 15  ω     38.00  67.00   0.50    3.26    --  107.75 -37.00  60.00   58
 16  ω     35.00 107.00   0.50    3.26    --  107.75 -99.00   0.00  144
 17  ω     36.00  77.00   0.50    3.26    --  107.75-125.00 120.00   82
 18  ω    141.00 166.00   0.50    3.26    --  107.75  19.00 -30.00   50
 19  ω    101.00 178.00   0.50    3.26    --  107.75 109.00  46.00  154
 20  ω    106.00 132.00   0.50    3.26    --  107.75  19.00 -30.00   52
 21  ω     36.00  71.00   0.50    3.26    --  107.75 -37.00-180.00   70
 22  ω   -120.00 -70.00   0.50    0.82    --  -47.94-125.00-180.00  100
 23  ω   -159.00 -79.00   0.50    3.26    --  -86.25-109.00 -49.00  160
 24  ω   -120.00 -70.00   0.50    0.82    --  -47.94-125.00   0.00  100
 25  ω   -120.00 -70.00   0.50    0.82    --  -47.94-125.00  90.00  100
 26  ω   -120.00 -70.00   0.50    0.82    --  -47.94-125.00 120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005024000
_diffrn_orient_matrix_UB_12      0.1413271000
_diffrn_orient_matrix_UB_13      0.0232810000
_diffrn_orient_matrix_UB_21      -0.0628119000
_diffrn_orient_matrix_UB_22      -0.0045495000
_diffrn_orient_matrix_UB_23      -0.0012860000
_diffrn_orient_matrix_UB_31      0.0065553000
_diffrn_orient_matrix_UB_32      -0.0321513000
_diffrn_orient_matrix_UB_33      0.1026546000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.285
_diffrn_reflns_theta_min         3.624
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              PhotonJet-S
_exptl_absorpt_coefficient_mu    7.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       needle
_exptl_crystal_F_000             1812
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.477
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1503P)²+11.5459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3618
_reflns_number_total             3930
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04860j2.cif
_cod_data_source_block           exp_40_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7703451.cif.'
_cod_database_code               7703451
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C37H23O6Cl3Ru
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C00L(H00L)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00E(H00E), C00F(H00F), C00H(H00H), C00I(H00I),
 C00J(H00J), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.721
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9961° 
 around [-0.17 -0.00 0.99] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
loop_
_space_group_symop_operation_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ru01 Ru 0.500000 0.56443(5) 0.250000 0.0478(2) Uani 1 2 d S T P
Cl02 Cl 0.35298(12) 0.8796(3) 0.06385(18) 0.1259(10) Uani 1 1 d . . .
Cl03 Cl 0.38810(16) 0.6743(2) -0.04291(19) 0.1409(12) Uani 1 1 d . . .
Cl04 Cl 0.46009(14) 0.8755(3) 0.0077(3) 0.1393(11) Uani 1 1 d . . .
O005 O 0.49180(16) 0.5761(3) 0.3836(2) 0.0528(8) Uani 1 1 d . . .
O006 O 0.44019(15) 0.7003(4) 0.2490(2) 0.0555(8) Uani 1 1 d . . .
O007 O 0.44691(16) 0.4180(4) 0.2391(3) 0.0566(9) Uani 1 1 d . . .
C008 C 0.4483(2) 0.6385(5) 0.4022(3) 0.0500(10) Uani 1 1 d . . .
C009 C 0.4198(2) 0.7100(5) 0.3263(3) 0.0523(11) Uani 1 1 d . . .
C00A C 0.3916(2) 0.6859(6) 0.5299(4) 0.0588(12) Uani 1 1 d . . .
H00A H 0.389370 0.662844 0.591715 0.071 Uiso 1 1 calc R . .
C00B C 0.4335(2) 0.6300(5) 0.4906(4) 0.0565(12) Uani 1 1 d . . .
H00B H 0.456315 0.576654 0.530302 0.068 Uiso 1 1 calc R . .
C00C C 0.3155(2) 0.8163(6) 0.5565(5) 0.0660(14) Uani 1 1 d . . .
C00D C 0.2896(2) 0.8541(6) 0.6162(5) 0.0677(14) Uani 1 1 d . . .
C00E C 0.3754(2) 0.7897(5) 0.3320(4) 0.0608(13) Uani 1 1 d . . .
H00E H 0.362896 0.831594 0.276498 0.073 Uiso 1 1 calc R . .
C00F C 0.3459(2) 0.8190(6) 0.4048(4) 0.0655(14) Uani 1 1 d . . .
H00F H 0.317926 0.880295 0.392159 0.079 Uiso 1 1 calc R . .
C00G C 0.3515(2) 0.7712(5) 0.4937(4) 0.0594(12) Uani 1 1 d . . .
C00H C 0.500000 0.0182(11) 0.250000 0.094(3) Uani 1 2 d S T P
H00H H 0.499999 -0.071194 0.250002 0.113 Uiso 1 2 calc RS T P
C00I C 0.4492(4) 0.0758(6) 0.2424(6) 0.083(2) Uani 1 1 d . . .
H00I H 0.418621 0.020455 0.238233 0.099 Uiso 1 1 calc R . .
C00J C 0.2141(3) 0.9755(8) 0.6681(6) 0.0831(19) Uani 1 1 d . . .
H00J H 0.205144 1.006389 0.607734 0.100 Uiso 1 1 calc R . .
C00K C 0.4703(2) 0.3098(6) 0.2450(4) 0.0574(12) Uani 1 1 d . . .
C00L C 0.4080(4) 0.7838(7) 0.0411(5) 0.082(2) Uani 1 1 d . . .
H00L H 0.421998 0.738053 0.098365 0.098 Uiso 1 1 calc R . .
C00M C 0.4367(3) 0.2028(6) 0.2402(5) 0.0702(15) Uani 1 1 d . . .
H00M H 0.398586 0.220720 0.234223 0.084 Uiso 1 1 calc R . .
C00N C 0.2583(2) 0.8952(6) 0.6872(5) 0.0685(15) Uani 1 1 d . . .
C00O C 0.1829(3) 1.0110(8) 0.7362(7) 0.090(2) Uani 1 1 d . . .
H00O H 0.152111 1.064471 0.722147 0.108 Uiso 1 1 calc R . .
C00P C 0.1963(4) 0.9695(10) 0.8242(8) 0.107(3) Uani 1 1 d . . .
H00P H 0.175304 0.996384 0.871017 0.129 Uiso 1 1 calc R . .
C00Q C 0.2707(3) 0.8511(9) 0.7771(6) 0.092(2) Uani 1 1 d . . .
H00Q H 0.300565 0.794799 0.790913 0.110 Uiso 1 1 calc R . .
C00R C 0.2404(4) 0.8884(11) 0.8453(7) 0.106(3) Uani 1 1 d . . .
H00R H 0.249361 0.859066 0.906036 0.127 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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
O005 Ru01 O005 172.9(2) . 2_655
O005 Ru01 O006 95.73(15) 2_655 .
O005 Ru01 O006 79.26(14) 2_655 2_655
O005 Ru01 O006 79.26(14) . .
O005 Ru01 O006 95.73(15) . 2_655
O005 Ru01 O007 89.47(16) . .
O005 Ru01 O007 89.47(16) 2_655 2_655
O005 Ru01 O007 95.97(15) . 2_655
O005 Ru01 O007 95.97(15) 2_655 .
O006 Ru01 O006 90.9(2) 2_655 .
O007 Ru01 O006 94.91(16) 2_655 2_655
O007 Ru01 O006 94.91(16) . .
O007 Ru01 O006 172.83(15) 2_655 .
O007 Ru01 O006 172.83(15) . 2_655
O007 Ru01 O007 79.6(2) . 2_655
C008 O005 Ru01 114.2(3) . .
C009 O006 Ru01 113.2(3) . .
C00K O007 Ru01 113.8(3) . .
O005 C008 C009 115.7(4) . .
O005 C008 C00B 117.7(4) . .
C00B C008 C009 126.6(5) . .
O006 C009 C008 115.6(4) . .
O006 C009 C00E 118.8(5) . .
C00E C009 C008 125.5(5) . .
C00B C00A H00A 114.8 . .
C00B C00A C00G 130.5(5) . .
C00G C00A H00A 114.8 . .
C008 C00B H00B 114.6 . .
C00A C00B C008 130.7(5) . .
C00A C00B H00B 114.6 . .
C00D C00C C00G 173.4(7) . .
C00C C00D C00N 178.3(8) . .
C009 C00E H00E 114.4 . .
C009 C00E C00F 131.2(5) . .
C00F C00E H00E 114.4 . .
C00E C00F H00F 115.3 . .
C00E C00F C00G 129.5(5) . .
C00G C00F H00F 115.3 . .
C00A C00G C00C 115.5(5) . .
C00F C00G C00A 125.7(5) . .
C00F C00G C00C 118.7(5) . .
C00I C00H H00H 116.3 2_655 .
C00I C00H H00H 116.3 . .
C00I C00H C00I 127.5(10) . 2_655
C00H C00I H00I 115.5 . .
C00H C00I C00M 128.9(8) . .
C00M C00I H00I 115.5 . .
C00N C00J H00J 119.8 . .
C00O C00J H00J 119.8 . .
C00O C00J C00N 120.4(8) . .
O007 C00K C00K 116.3(3) . 2_655
O007 C00K C00M 117.9(5) . .
C00M C00K C00K 125.7(4) . 2_655
Cl02 C00L H00L 108.7 . .
Cl03 C00L Cl02 111.4(5) . .
Cl03 C00L H00L 108.7 . .
Cl04 C00L Cl02 109.8(4) . .
Cl04 C00L Cl03 109.6(5) . .
Cl04 C00L H00L 108.7 . .
C00I C00M C00K 131.6(7) . .
C00I C00M H00M 114.2 . .
C00K C00M H00M 114.2 . .
C00J C00N C00D 120.8(7) . .
C00J C00N C00Q 118.7(6) . .
C00Q C00N C00D 120.5(6) . .
C00J C00O H00O 119.9 . .
C00P C00O C00J 120.3(8) . .
C00P C00O H00O 119.9 . .
C00O C00P H00P 119.8 . .
C00O C00P C00R 120.5(7) . .
C00R C00P H00P 119.8 . .
C00N C00Q H00Q 119.5 . .
C00R C00Q C00N 120.9(8) . .
C00R C00Q H00Q 119.5 . .
C00P C00R H00R 120.4 . .
C00Q C00R C00P 119.2(9) . .
C00Q C00R H00R 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru01 O005 2.004(3) .
Ru01 O005 2.004(3) 2_655
Ru01 O006 2.058(4) .
Ru01 O006 2.058(4) 2_655
Ru01 O007 2.024(4) 2_655
Ru01 O007 2.024(4) .
Cl02 C00L 1.754(8) .
Cl03 C00L 1.728(8) .
Cl04 C00L 1.723(9) .
O005 C008 1.312(6) .
O006 C009 1.297(6) .
O007 C00K 1.283(7) .
C008 C009 1.462(7) .
C008 C00B 1.393(7) .
C009 C00E 1.392(7) .
C00A H00A 0.9500 .
C00A C00B 1.371(8) .
C00A C00G 1.399(8) .
C00B H00B 0.9500 .
C00C C00D 1.211(9) .
C00C C00G 1.430(8) .
C00D C00N 1.434(9) .
C00E H00E 0.9500 .
C00E C00F 1.395(8) .
C00F H00F 0.9500 .
C00F C00G 1.396(9) .
C00H H00H 0.9500 .
C00H C00I 1.382(11) 2_655
C00H C00I 1.382(11) .
C00I H00I 0.9500 .
C00I C00M 1.384(10) .
C00J H00J 0.9500 .
C00J C00N 1.384(10) .
C00J C00O 1.380(11) .
C00K C00K 1.451(11) 2_655
C00K C00M 1.400(8) .
C00L H00L 1.0000 .
C00M H00M 0.9500 .
C00N C00Q 1.406(11) .
C00O H00O 0.9500 .
C00O C00P 1.374(14) .
C00P H00P 0.9500 .
C00P C00R 1.391(14) .
C00Q H00Q 0.9500 .
C00Q C00R 1.374(11) .
C00R H00R 0.9500 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7754 13285 5368 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.2246 13198 5368 nmt -1.0013 -0.0000 -0.3497 -0.0000 -1.0004 -0.0008 0.0092
-0.0023 1.0027
