#------------------------------------------------------------------------------
#$Date: 2022-01-05 02:04:14 +0200 (Wed, 05 Jan 2022) $
#$Revision: 271804 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/92/7709212.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_7709212
loop_
_publ_author_name
'Cesari, Cristiana'
'Bortoluzzi, Marco'
'Femoni, Cristina'
'Iapalucci, Maria Carmela'
'Zacchini, Stefano'
_publ_section_title
;
 Synthesis, molecular structure and fluxional behavior of the elusive
 [HRu4(CO)12]3-- carbonyl anion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03622J
_journal_year                    2022
_chemical_formula_sum            'C19 H21 N O11 Ru3'
_chemical_formula_weight         742.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.810(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3458(10)
_cell_length_b                   11.7217(9)
_cell_length_c                   17.4163(15)
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.5195
_cell_measurement_theta_min      2.3605
_cell_volume                     2497.0(4)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'PHOTON2 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30401
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_min         1.665
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.4574
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1587 (selected reflections only, before parameter refinement)
 R(int) = 0.0844 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.156
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0184P)²+6.6082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4254
_reflns_number_total             5447
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03622j3.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7709212
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.782
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.84684(3) 0.36505(3) 0.21776(2) 0.01155(10) Uani 1 1 d . . . . .
H1 H 0.854(4) 0.208(4) 0.225(3) 0.014 Uiso 1 1 d . U . . .
Ru2 Ru 0.77090(3) 0.18571(3) 0.30326(2) 0.01060(10) Uani 1 1 d . . . . .
Ru3 Ru 0.61778(3) 0.32664(3) 0.21008(2) 0.01184(10) Uani 1 1 d . . . . .
C1 C 0.8375(4) 0.3442(4) 0.3353(3) 0.0142(11) Uani 1 1 d . . . . .
C2 C 1.0007(5) 0.3659(4) 0.2286(3) 0.0163(11) Uani 1 1 d . . . . .
C3 C 0.8323(4) 0.5257(4) 0.2266(3) 0.0195(12) Uani 1 1 d . . . . .
C4 C 0.8304(4) 0.3572(5) 0.1037(3) 0.0176(11) Uani 1 1 d . . . . .
C5 C 0.8905(4) 0.1109(4) 0.3632(3) 0.0156(11) Uani 1 1 d . . . . .
C6 C 0.6814(4) 0.1927(4) 0.3833(3) 0.0143(11) Uani 1 1 d . . . . .
C7 C 0.7068(4) 0.0482(5) 0.2501(3) 0.0188(12) Uani 1 1 d . . . . .
C8 C 0.6212(4) 0.4228(4) 0.3009(3) 0.0175(12) Uani 1 1 d . . . . .
C9 C 0.4829(5) 0.2561(4) 0.2278(3) 0.0191(12) Uani 1 1 d . . . . .
C10 C 0.6402(4) 0.2164(4) 0.1308(3) 0.0171(11) Uani 1 1 d . . . . .
C11 C 0.5812(5) 0.4499(5) 0.1377(3) 0.0209(12) Uani 1 1 d . . . . .
O1 O 0.8640(3) 0.3950(3) 0.3942(2) 0.0182(8) Uani 1 1 d . . . . .
O2 O 1.0950(3) 0.3681(3) 0.2331(2) 0.0216(9) Uani 1 1 d . . . . .
O3 O 0.8265(3) 0.6222(3) 0.2322(3) 0.0327(11) Uani 1 1 d . . . . .
O4 O 0.8254(3) 0.3663(4) 0.0385(2) 0.0340(11) Uani 1 1 d . . . . .
O5 O 0.9621(3) 0.0686(3) 0.4000(2) 0.0236(9) Uani 1 1 d . . . . .
O6 O 0.6280(3) 0.1980(3) 0.4325(2) 0.0244(9) Uani 1 1 d . . . . .
O7 O 0.6661(3) -0.0340(3) 0.2270(2) 0.0287(10) Uani 1 1 d . . . . .
O8 O 0.6172(3) 0.4791(3) 0.3534(2) 0.0282(10) Uani 1 1 d . . . . .
O9 O 0.4030(3) 0.2145(3) 0.2383(3) 0.0343(11) Uani 1 1 d . . . . .
O10 O 0.6463(3) 0.1516(3) 0.0827(2) 0.0252(9) Uani 1 1 d . . . . .
O11 O 0.5613(4) 0.5220(3) 0.0954(2) 0.0330(11) Uani 1 1 d . . . . .
N1 N 0.7809(3) 0.7008(3) 0.5062(2) 0.0129(9) Uani 1 1 d . . . . .
C12 C 0.8357(5) 0.6722(4) 0.4360(3) 0.0193(12) Uani 1 1 d . . . . .
H12A H 0.8385 0.5882 0.4308 0.023 Uiso 1 1 calc R U . . .
H12B H 0.7901 0.7023 0.3892 0.023 Uiso 1 1 calc R U . . .
C13 C 0.9501(5) 0.7191(5) 0.4387(4) 0.0290(14) Uani 1 1 d . . . . .
H13A H 0.9482 0.8025 0.4428 0.043 Uiso 1 1 calc R U . . .
H13B H 0.9796 0.6977 0.3912 0.043 Uiso 1 1 calc R U . . .
H13C H 0.9967 0.6877 0.4837 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7705(5) 0.8282(4) 0.5149(3) 0.0196(12) Uani 1 1 d . . . . .
H14A H 0.8448 0.8616 0.5237 0.024 Uiso 1 1 calc R U . . .
H14B H 0.7354 0.8436 0.5617 0.024 Uiso 1 1 calc R U . . .
C15 C 0.7057(5) 0.8882(4) 0.4468(3) 0.0274(14) Uani 1 1 d . . . . .
H15A H 0.7447 0.8824 0.4016 0.041 Uiso 1 1 calc R U . . .
H15B H 0.6968 0.9687 0.4597 0.041 Uiso 1 1 calc R U . . .
H15C H 0.6337 0.8524 0.4350 0.041 Uiso 1 1 calc R U . . .
C16 C 0.8484(4) 0.6568(4) 0.5801(3) 0.0178(12) Uani 1 1 d . . . . .
H16A H 0.9186 0.6987 0.5880 0.021 Uiso 1 1 calc R U . . .
H16B H 0.8090 0.6747 0.6245 0.021 Uiso 1 1 calc R U . . .
C17 C 0.8726(5) 0.5308(4) 0.5812(3) 0.0200(12) Uani 1 1 d . . . . .
H17A H 0.8039 0.4880 0.5759 0.030 Uiso 1 1 calc R U . . .
H17B H 0.9171 0.5107 0.6303 0.030 Uiso 1 1 calc R U . . .
H17C H 0.9127 0.5119 0.5380 0.030 Uiso 1 1 calc R U . . .
C18 C 0.6692(4) 0.6432(5) 0.4935(3) 0.0186(12) Uani 1 1 d . . . . .
H18A H 0.6309 0.6672 0.4424 0.022 Uiso 1 1 calc R U . . .
H18B H 0.6803 0.5597 0.4915 0.022 Uiso 1 1 calc R U . . .
C19 C 0.5963(5) 0.6684(5) 0.5542(4) 0.0321(15) Uani 1 1 d . . . . .
H19A H 0.6332 0.6454 0.6052 0.048 Uiso 1 1 calc R U . . .
H19B H 0.5277 0.6258 0.5423 0.048 Uiso 1 1 calc R U . . .
H19C H 0.5805 0.7503 0.5545 0.048 Uiso 1 1 calc R U . . .
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'
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
C2 Ru1 C3 95.2(2) . . ?
C2 Ru1 C4 93.8(2) . . ?
C3 Ru1 C4 97.4(2) . . ?
C2 Ru1 C1 95.3(2) . . ?
C3 Ru1 C1 91.1(2) . . ?
C4 Ru1 C1 167.0(2) . . ?
C2 Ru1 Ru2 110.82(15) . . ?
C3 Ru1 Ru2 131.06(16) . . ?
C4 Ru1 Ru2 120.22(16) . . ?
C1 Ru1 Ru2 47.42(13) . . ?
C2 Ru1 Ru3 170.72(15) . . ?
C3 Ru1 Ru3 93.24(17) . . ?
C4 Ru1 Ru3 88.85(15) . . ?
C1 Ru1 Ru3 80.80(14) . . ?
Ru2 Ru1 Ru3 60.399(14) . . ?
C2 Ru1 H1 87.8(15) . . ?
C3 Ru1 H1 170.7(15) . . ?
C4 Ru1 H1 91.1(15) . . ?
C1 Ru1 H1 79.9(15) . . ?
Ru2 Ru1 H1 40.0(15) . . ?
Ru3 Ru1 H1 83.2(15) . . ?
C6 Ru2 C5 95.9(2) . . ?
C6 Ru2 C7 98.3(2) . . ?
C5 Ru2 C7 96.5(2) . . ?
C6 Ru2 C1 90.7(2) . . ?
C5 Ru2 C1 90.9(2) . . ?
C7 Ru2 C1 167.7(2) . . ?
C6 Ru2 Ru1 128.86(15) . . ?
C5 Ru2 Ru1 110.22(16) . . ?
C7 Ru2 Ru1 120.29(16) . . ?
C1 Ru2 Ru1 47.52(14) . . ?
C6 Ru2 Ru3 89.18(14) . . ?
C5 Ru2 Ru3 170.41(15) . . ?
C7 Ru2 Ru3 90.76(16) . . ?
C1 Ru2 Ru3 80.91(14) . . ?
Ru1 Ru2 Ru3 60.478(15) . . ?
C6 Ru2 H1 169.2(15) . . ?
C5 Ru2 H1 90.3(15) . . ?
C7 Ru2 H1 89.8(15) . . ?
C1 Ru2 H1 80.3(15) . . ?
Ru1 Ru2 H1 40.3(15) . . ?
Ru3 Ru2 H1 83.5(15) . . ?
C9 Ru3 C11 107.2(2) . . ?
C9 Ru3 C8 92.4(2) . . ?
C11 Ru3 C8 94.3(2) . . ?
C9 Ru3 C10 92.2(2) . . ?
C11 Ru3 C10 94.4(2) . . ?
C8 Ru3 C10 168.5(2) . . ?
C9 Ru3 Ru2 100.46(16) . . ?
C11 Ru3 Ru2 152.25(17) . . ?
C8 Ru3 Ru2 86.16(15) . . ?
C10 Ru3 Ru2 82.62(15) . . ?
C9 Ru3 Ru1 159.55(16) . . ?
C11 Ru3 Ru1 93.14(17) . . ?
C8 Ru3 Ru1 87.60(16) . . ?
C10 Ru3 Ru1 84.38(16) . . ?
Ru2 Ru3 Ru1 59.123(14) . . ?
O1 C1 Ru2 136.9(4) . . ?
O1 C1 Ru1 137.9(4) . . ?
Ru2 C1 Ru1 85.06(19) . . ?
O2 C2 Ru1 177.8(5) . . ?
O3 C3 Ru1 178.2(5) . . ?
O4 C4 Ru1 171.5(5) . . ?
O5 C5 Ru2 178.4(5) . . ?
O6 C6 Ru2 179.0(5) . . ?
O7 C7 Ru2 172.4(5) . . ?
O8 C8 Ru3 176.2(5) . . ?
O9 C9 Ru3 179.9(6) . . ?
O10 C10 Ru3 175.6(5) . . ?
O11 C11 Ru3 179.1(5) . . ?
C14 N1 C12 110.8(4) . . ?
C14 N1 C18 111.4(4) . . ?
C12 N1 C18 106.3(4) . . ?
C14 N1 C16 107.1(4) . . ?
C12 N1 C16 110.7(4) . . ?
C18 N1 C16 110.6(4) . . ?
C13 C12 N1 114.4(4) . . ?
C13 C12 H12A 108.7 . . ?
N1 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
N1 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 C15 115.2(4) . . ?
N1 C14 H14A 108.5 . . ?
C15 C14 H14A 108.5 . . ?
N1 C14 H14B 108.5 . . ?
C15 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N1 115.3(4) . . ?
C17 C16 H16A 108.5 . . ?
N1 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
N1 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 115.3(4) . . ?
C19 C18 H18A 108.5 . . ?
N1 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
N1 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
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 C2 1.883(6) . ?
Ru1 C3 1.900(5) . ?
Ru1 C4 1.972(5) . ?
Ru1 C1 2.080(5) . ?
Ru1 Ru2 2.8098(6) . ?
Ru1 Ru3 2.8487(6) . ?
Ru1 H1 1.84(5) . ?
Ru2 C6 1.895(5) . ?
Ru2 C5 1.903(5) . ?
Ru2 C7 1.971(5) . ?
Ru2 C1 2.077(5) . ?
Ru2 Ru3 2.8465(6) . ?
Ru2 H1 1.83(5) . ?
Ru3 C9 1.921(6) . ?
Ru3 C11 1.931(6) . ?
Ru3 C8 1.937(6) . ?
Ru3 C10 1.938(6) . ?
C1 O1 1.193(6) . ?
C2 O2 1.156(6) . ?
C3 O3 1.138(6) . ?
C4 O4 1.133(6) . ?
C5 O5 1.133(6) . ?
C6 O6 1.151(6) . ?
C7 O7 1.134(6) . ?
C8 O8 1.135(6) . ?
C9 O9 1.138(6) . ?
C10 O10 1.140(6) . ?
C11 O11 1.126(6) . ?
N1 C14 1.507(6) . ?
N1 C12 1.513(6) . ?
N1 C18 1.525(6) . ?
N1 C16 1.526(6) . ?
C12 C13 1.511(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.511(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.506(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.507(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
