#------------------------------------------------------------------------------
#$Date: 2019-11-24 08:28:58 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237303 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/81/4088131.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_4088131
loop_
_publ_author_name
'Saha, Sayantani'
'Daw, Prosenjit'
'Bera, Jitendra K.'
_publ_section_title
;
 Oxidative Route to Abnormal NHC Compounds from Singly Bonded [M--M] (M =
 Ru, Rh, Pd) Precursors
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5509
_journal_paper_doi               10.1021/acs.organomet.5b00872
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C108 H96 N30 O12 Ru6, B2 F8, 4(B F4)'
_chemical_formula_sum            'C108 H96 B6 F24 N30 O12 Ru6'
_chemical_formula_weight         3133.43
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.236(4)
_cell_length_b                   19.236(4)
_cell_length_c                   33.377(7)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.52
_cell_volume                     10696(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'omega scans'
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            40468
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         3.396
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5968
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1705P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2517
_reflns_number_gt                3998
_reflns_number_total             5968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00872_si_002.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Trigonal' was changed to
'trigonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4088131
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ru1 Ru 0.89393(3) 0.24899(3) 0.018597(13) 0.0458(2) Uani 1 1 d .
N3 N 1.0250(3) 0.2236(2) 0.04489(12) 0.0422(9) Uani 1 1 d .
N1 N 0.7755(3) 0.1501(3) 0.09542(14) 0.0521(11) Uani 1 1 d .
N2 N 0.9012(3) 0.1851(3) 0.07144(13) 0.0447(10) Uani 1 1 d .
C7 C 0.8401(3) 0.1419(3) 0.09917(15) 0.0464(12) Uani 1 1 d .
C11 C 1.0050(3) 0.2647(3) 0.01553(16) 0.0469(12) Uani 1 1 d .
C4 C 0.7810(4) 0.0483(3) 0.15495(16) 0.0540(14) Uani 1 1 d .
C10 C 0.9670(3) 0.1782(3) 0.07397(15) 0.0455(12) Uani 1 1 d .
C8 C 0.9183(4) 0.0890(3) 0.12892(16) 0.0535(13) Uani 1 1 d .
H8 H 0.9249 0.0576 0.1481 0.064 Uiso 1 1 calc R
C6 C 0.8477(4) 0.0927(3) 0.12841(15) 0.0486(12) Uani 1 1 d .
C3 C 0.7158(4) 0.0581(4) 0.14988(18) 0.0627(16) Uani 1 1 d .
H3 H 0.6718 0.0309 0.1667 0.075 Uiso 1 1 calc R
C9 C 0.9765(4) 0.1297(3) 0.10228(17) 0.0532(13) Uani 1 1 d .
H9 H 1.0228 0.1259 0.1025 0.064 Uiso 1 1 calc R
C15 C 0.9403(5) 0.3495(4) 0.0446(2) 0.0671(18) Uani 1 1 d .
C2 C 0.7139(4) 0.1081(3) 0.11988(17) 0.0545(14) Uani 1 1 d .
O2 O 0.9687(5) 0.4105(4) 0.0583(2) 0.112(2) Uani 1 1 d .
C5 C 0.7831(5) -0.0071(4) 0.18515(19) 0.0699(17) Uani 1 1 d .
H5A H 0.8166 0.0233 0.2072 0.105 Uiso 1 1 calc R
H5B H 0.8044 -0.0379 0.1731 0.105 Uiso 1 1 calc R
H5C H 0.7297 -0.0427 0.1947 0.105 Uiso 1 1 calc R
C1 C 0.6424(4) 0.1183(5) 0.1153(2) 0.077(2) Uani 1 1 d .
H1A H 0.6556 0.1710 0.1242 0.116 Uiso 1 1 calc R
H1B H 0.5990 0.0787 0.1312 0.116 Uiso 1 1 calc R
H1C H 0.6267 0.1119 0.0877 0.116 Uiso 1 1 calc R
C12 C 1.0740(3) 0.3070(3) -0.00566(17) 0.0445(12) Uani 1 1 d .
H12 H 1.0802 0.3400 -0.0273 0.053 Uiso 1 1 calc R
N5 N 0.7745(3) 0.2296(3) 0.02187(17) 0.0652(14) Uani 1 1 d .
C13 C 1.1034(3) 0.2435(3) 0.03987(16) 0.0460(12) Uani 1 1 d .
C14 C 1.1478(4) 0.2149(4) 0.06541(17) 0.0574(14) Uani 1 1 d .
H14A H 1.1359 0.1625 0.0567 0.086 Uiso 1 1 calc R
H14B H 1.1315 0.2122 0.0928 0.086 Uiso 1 1 calc R
H14C H 1.2044 0.2515 0.0632 0.086 Uiso 1 1 calc R
O1 O 0.9224(4) 0.3366(4) -0.06044(18) 0.0955(17) Uani 1 1 d .
C16 C 0.9064(4) 0.3026(4) -0.0306(2) 0.0650(16) Uani 1 1 d .
C17 C 0.7100(5) 0.2162(5) 0.0195(2) 0.079(2) Uani 1 1 d .
C18 C 0.6246(5) 0.1976(8) 0.0149(4) 0.121(4) Uani 1 1 d .
H18A H 0.5906 0.1411 0.0102 0.182 Uiso 1 1 calc R
H18B H 0.6210 0.2271 -0.0075 0.182 Uiso 1 1 calc R
H18C H 0.6079 0.2126 0.0388 0.182 Uiso 1 1 calc R
N4 N 1.1345(3) 0.2941(2) 0.00940(12) 0.0428(9) Uani 1 1 d .
F4A F 0.9888(3) 0.9269(3) 0.2353(2) 0.1045(16) Uani 1 1 d .
F1 F 0.5939(8) 0.2809(8) 0.9385(4) 0.258(6) Uani 1 1 d D
F4B F 1.0000 1.0000 0.1806(3) 0.101(3) Uani 1 3 d S
B1 B 1.0000 1.0000 0.2205(6) 0.081(4) Uani 1 3 d S
F2 F 0.6667 0.3333 0.8776(7) 0.352(19) Uani 1 3 d SD
B2 B 0.6667 0.3333 0.9196(9) 0.30(5) Uani 1 3 d SD
B3 B 1.0000 0.0000 0.0100 0.102(7) Uani 1 3 d SD
F3 F 1.0000 0.0000 -0.0368(3) 0.213(8) Uani 1 3 d SD
F6 F 0.9718(9) 0.0538(8) 0.0153(3) 0.202(4) Uani 1 1 d D
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
C15 Ru1 C16 88.5(3) . .
C15 Ru1 C11 87.0(3) . .
C16 Ru1 C11 92.2(3) . .
C15 Ru1 N4 178.7(2) . 12_545
C16 Ru1 N4 92.7(2) . 12_545
C11 Ru1 N4 93.54(19) . 12_545
C15 Ru1 N5 94.1(3) . .
C16 Ru1 N5 88.4(3) . .
C11 Ru1 N5 178.8(2) . .
N4 Ru1 N5 85.4(2) 12_545 .
C15 Ru1 N2 94.3(2) . .
C16 Ru1 N2 168.0(2) . .
C11 Ru1 N2 76.37(19) . .
N4 Ru1 N2 84.62(16) 12_545 .
N5 Ru1 N2 102.99(18) . .
C13 N3 C10 132.9(4) . .
C13 N3 C11 109.0(4) . .
C10 N3 C11 117.9(4) . .
C2 N1 C7 118.1(5) . .
C10 N2 C7 117.0(4) . .
C10 N2 Ru1 115.7(3) . .
C7 N2 Ru1 126.6(4) . .
N1 C7 N2 115.0(5) . .
N1 C7 C6 123.8(5) . .
N2 C7 C6 121.1(5) . .
C12 C11 N3 103.6(4) . .
C12 C11 Ru1 140.0(4) . .
N3 C11 Ru1 116.3(4) . .
C3 C4 C6 116.7(5) . .
C3 C4 C5 122.6(6) . .
C6 C4 C5 120.6(6) . .
N2 C10 C9 123.5(5) . .
N2 C10 N3 113.0(4) . .
C9 C10 N3 123.4(5) . .
C9 C8 C6 120.9(5) . .
C8 C6 C7 118.1(5) . .
C8 C6 C4 124.4(5) . .
C7 C6 C4 117.5(5) . .
C4 C3 C2 121.5(6) . .
C8 C9 C10 119.3(6) . .
O2 C15 Ru1 176.9(6) . .
N1 C2 C3 122.3(6) . .
N1 C2 C1 117.3(6) . .
C3 C2 C1 120.4(6) . .
C11 C12 N4 111.0(5) . .
C17 N5 Ru1 172.6(6) . .
N4 C13 N3 109.2(5) . .
N4 C13 C14 125.3(5) . .
N3 C13 C14 125.5(5) . .
O1 C16 Ru1 172.6(7) . .
N5 C17 C18 178.0(10) . .
C13 N4 C12 107.2(4) . .
C13 N4 Ru1 134.8(4) . 11_665
C12 N4 Ru1 117.9(3) . 11_665
F4B B1 F4A 110.6(8) . 2_765
F4B B1 F4A 110.6(8) . 3_675
F4A B1 F4A 108.3(9) 2_765 3_675
F4B B1 F4A 110.6(8) . .
F4A B1 F4A 108.3(9) 2_765 .
F4A B1 F4A 108.3(9) 3_675 .
F1 B2 F1 101.2(15) 2_655 .
F1 B2 F1 101.2(15) 2_655 3_665
F1 B2 F1 101.2(15) . 3_665
F1 B2 F2 116.8(12) 2_655 .
F1 B2 F2 116.8(12) . .
F1 B2 F2 116.8(12) 3_665 .
B3 B3 F3 180.0 10_755 10_755
B3 B3 F6 97.3(5) 10_755 3_765
F3 B3 F6 82.7(5) 10_755 3_765
B3 B3 F6 97.3(5) 10_755 2_645
F3 B3 F6 82.7(5) 10_755 2_645
F6 B3 F6 118.4(2) 3_765 2_645
B3 B3 F6 97.3(5) 10_755 .
F3 B3 F6 82.7(5) 10_755 .
F6 B3 F6 118.4(2) 3_765 .
F6 B3 F6 118.4(2) 2_645 .
B3 B3 F3 0.0 10_755 .
F3 B3 F3 180.0 10_755 .
F6 B3 F3 97.3(5) 3_765 .
F6 B3 F3 97.3(5) 2_645 .
F6 B3 F3 97.3(5) . .
B3 B3 F6 58.6(4) 10_755 12_545
F3 B3 F6 121.4(4) 10_755 12_545
F6 B3 F6 155.95(14) 3_765 12_545
F6 B3 F6 69.1(4) 2_645 12_545
F6 B3 F6 69.1(4) . 12_545
F3 B3 F6 58.6(4) . 12_545
B3 B3 F6 58.6(4) 10_755 10_755
F3 B3 F6 121.4(4) 10_755 10_755
F6 B3 F6 69.1(4) 3_765 10_755
F6 B3 F6 69.1(4) 2_645 10_755
F6 B3 F6 155.95(14) . 10_755
F3 B3 F6 58.6(4) . 10_755
F6 B3 F6 95.4(5) 12_545 10_755
B3 B3 F6 58.6(4) 10_755 11_665
F3 B3 F6 121.4(4) 10_755 11_665
F6 B3 F6 69.1(4) 3_765 11_665
F6 B3 F6 155.95(14) 2_645 11_665
F6 B3 F6 69.1(4) . 11_665
F3 B3 F6 58.6(4) . 11_665
F6 B3 F6 95.4(5) 12_545 11_665
F6 B3 F6 95.4(5) 10_755 11_665
B3 F3 F6 62.7(5) 10_755 10_755
B3 F3 F6 62.7(5) 10_755 11_665
F6 F3 F6 100.7(7) 10_755 11_665
B3 F3 F6 62.7(5) 10_755 12_545
F6 F3 F6 100.7(7) 10_755 12_545
F6 F3 F6 100.7(7) 11_665 12_545
B3 F3 B3 0.0 10_755 .
F6 F3 B3 62.7(5) 10_755 .
F6 F3 B3 62.7(5) 11_665 .
F6 F3 B3 62.7(5) 12_545 .
B3 F6 F3 34.6(4) . 10_755
B3 F6 B3 24.05(14) . 10_755
F3 F6 B3 58.6(5) 10_755 10_755
B3 F6 F6 61.66(14) . 12_545
F3 F6 F6 85.1(3) 10_755 12_545
B3 F6 F6 49.3(3) 10_755 12_545
B3 F6 F6 61.66(14) . 11_665
F3 F6 F6 85.1(3) 10_755 11_665
B3 F6 F6 49.3(3) 10_755 11_665
F6 F6 F6 88.3(9) 12_545 11_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C15 1.888(7) .
Ru1 C16 1.889(6) .
Ru1 C11 2.004(6) .
Ru1 N4 2.126(4) 12_545
Ru1 N5 2.138(5) .
Ru1 N2 2.194(4) .
N3 C13 1.368(7) .
N3 C10 1.406(7) .
N3 C11 1.428(6) .
N1 C2 1.328(7) .
N1 C7 1.335(7) .
N2 C10 1.340(7) .
N2 C7 1.397(7) .
C7 C6 1.416(7) .
C11 C12 1.358(8) .
C4 C3 1.367(9) .
C4 C6 1.437(8) .
C4 C5 1.483(8) .
C10 C9 1.403(8) .
C8 C9 1.334(8) .
C8 C6 1.395(9) .
C3 C2 1.402(9) .
C15 O2 1.114(8) .
C2 C1 1.491(9) .
C12 N4 1.399(6) .
N5 C17 1.137(9) .
C13 N4 1.325(7) .
C13 C14 1.493(8) .
O1 C16 1.146(8) .
C17 C18 1.503(11) .
N4 Ru1 2.126(4) 11_665
F4A B1 1.401(9) .
F1 B2 1.401(15) .
F4B B1 1.33(2) .
B1 F4A 1.401(9) 2_765
B1 F4A 1.401(9) 3_675
F2 B2 1.40(2) .
B2 F1 1.401(15) 2_655
B2 F1 1.401(15) 3_665
B3 B3 0.66756(15) 10_755
B3 F3 0.894(11) 10_755
B3 F6 1.399(8) 3_765
B3 F6 1.399(8) 2_645
B3 F6 1.399(8) .
B3 F3 1.561(11) .
B3 F6 1.625(8) 12_545
B3 F6 1.625(8) 10_755
B3 F6 1.625(8) 11_665
F3 B3 0.894(11) 10_755
F3 F6 1.561(11) 10_755
F3 F6 1.561(11) 11_665
F3 F6 1.561(11) 12_545
F6 F3 1.561(11) 10_755
F6 B3 1.625(8) 10_755
F6 F6 1.724(14) 12_545
F6 F6 1.724(14) 11_665
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.167 745 157 ' '
2 0.000 0.000 0.500 741 156 ' '
3 -0.333 0.333 0.833 745 157 ' '
