#------------------------------------------------------------------------------
#$Date: 2022-01-05 02:04:14 +0200 (Wed, 05 Jan 2022) $
#$Revision: 271804 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/92/7709215.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_7709215
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            'C24 H40 N2 O8 Ru2'
_chemical_formula_weight         686.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 113.085(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5198(6)
_cell_length_b                   13.7870(8)
_cell_length_c                   11.8620(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.552
_cell_measurement_theta_min      2.7555
_cell_volume                     1432.21(15)
_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 0.999
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31227
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.380
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.4339
_exptl_absorpt_correction_T_min  0.2995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1491 (selected reflections only, before parameter refinement)
 R(int) = 0.0516 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0161
_refine_ls_R_factor_gt           0.0145
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0132P)²+0.5656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3298
_reflns_number_total             3453
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03622j3.cif
_cod_data_source_block           Ru2CO8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709215
_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   0.778
_shelx_estimated_absorpt_t_max   0.818
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.14027(2) 0.56149(2) 0.54134(2) 0.01037(3) Uani 1 1 d . . . . .
C1 C 0.31927(14) 0.63570(9) 0.58760(11) 0.0145(2) Uani 1 1 d . . . . .
C2 C 0.01360(14) 0.66029(9) 0.43424(11) 0.0160(2) Uani 1 1 d . . . . .
C3 C 0.13938(14) 0.55732(9) 0.70296(12) 0.0173(2) Uani 1 1 d . . . . .
C4 C 0.21329(14) 0.45383(9) 0.47858(11) 0.0158(2) Uani 1 1 d . . . . .
O1 O 0.42919(10) 0.68172(7) 0.61442(9) 0.02170(19) Uani 1 1 d . . . . .
O2 O -0.05129(11) 0.72449(7) 0.37444(9) 0.0268(2) Uani 1 1 d . . . . .
O3 O 0.14921(13) 0.55922(8) 0.80341(9) 0.0291(2) Uani 1 1 d . . . . .
O4 O 0.26664(11) 0.39065(7) 0.44363(9) 0.0253(2) Uani 1 1 d . . . . .
N1 N 0.35128(11) 0.62352(7) 0.19540(9) 0.01297(19) Uani 1 1 d . . . . .
C11 C 0.44746(14) 0.67748(9) 0.13900(12) 0.0184(2) Uani 1 1 d . . . . .
H11A H 0.4301 0.6478 0.0586 0.022 Uiso 1 1 calc R U . . .
H11B H 0.4118 0.7455 0.1240 0.022 Uiso 1 1 calc R U . . .
C12 C 0.61721(15) 0.67737(11) 0.21635(15) 0.0280(3) Uani 1 1 d . . . . .
H12A H 0.6367 0.7107 0.2941 0.042 Uiso 1 1 calc R U . . .
H12B H 0.6710 0.7110 0.1723 0.042 Uiso 1 1 calc R U . . .
H12C H 0.6538 0.6103 0.2328 0.042 Uiso 1 1 calc R U . . .
C13 C 0.40040(14) 0.51794(9) 0.22079(11) 0.0160(2) Uani 1 1 d . . . . .
H13A H 0.5042 0.5159 0.2864 0.019 Uiso 1 1 calc R U . . .
H13B H 0.3308 0.4848 0.2521 0.019 Uiso 1 1 calc R U . . .
C14 C 0.40193(18) 0.46158(10) 0.11149(13) 0.0244(3) Uani 1 1 d . . . . .
H14A H 0.3018 0.4667 0.0436 0.037 Uiso 1 1 calc R U . . .
H14B H 0.4247 0.3933 0.1341 0.037 Uiso 1 1 calc R U . . .
H14C H 0.4803 0.4884 0.0861 0.037 Uiso 1 1 calc R U . . .
C15 C 0.37121(14) 0.66608(9) 0.31915(11) 0.0168(2) Uani 1 1 d . . . . .
H15A H 0.3073 0.6285 0.3522 0.020 Uiso 1 1 calc R U . . .
H15B H 0.4790 0.6575 0.3762 0.020 Uiso 1 1 calc R U . . .
C16 C 0.33029(17) 0.77252(10) 0.31766(12) 0.0240(3) Uani 1 1 d . . . . .
H16A H 0.3976 0.8113 0.2906 0.036 Uiso 1 1 calc R U . . .
H16B H 0.3429 0.7927 0.4003 0.036 Uiso 1 1 calc R U . . .
H16C H 0.2239 0.7823 0.2611 0.036 Uiso 1 1 calc R U . . .
C17 C 0.18683(13) 0.63264(9) 0.10391(11) 0.0156(2) Uani 1 1 d . . . . .
H17A H 0.1599 0.7023 0.0920 0.019 Uiso 1 1 calc R U . . .
H17B H 0.1795 0.6063 0.0241 0.019 Uiso 1 1 calc R U . . .
C18 C 0.07083(15) 0.58111(10) 0.14093(12) 0.0215(3) Uani 1 1 d . . . . .
H18A H 0.0917 0.5113 0.1472 0.032 Uiso 1 1 calc R U . . .
H18B H -0.0321 0.5929 0.0791 0.032 Uiso 1 1 calc R U . . .
H18C H 0.0779 0.6058 0.2204 0.032 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
C1 Ru1 C4 96.33(5) . . ?
C1 Ru1 C3 94.78(5) . . ?
C4 Ru1 C3 120.69(5) . . ?
C1 Ru1 C2 93.96(5) . . ?
C4 Ru1 C2 121.41(5) . . ?
C3 Ru1 C2 115.60(5) . . ?
C1 Ru1 Ru1 177.20(4) . 3_566 ?
C4 Ru1 Ru1 81.14(4) . 3_566 ?
C3 Ru1 Ru1 87.56(4) . 3_566 ?
C2 Ru1 Ru1 86.39(4) . 3_566 ?
O1 C1 Ru1 179.04(11) . . ?
O2 C2 Ru1 174.09(11) . . ?
O3 C3 Ru1 174.59(11) . . ?
O4 C4 Ru1 175.83(11) . . ?
C17 N1 C15 111.13(9) . . ?
C17 N1 C13 111.76(9) . . ?
C15 N1 C13 105.39(9) . . ?
C17 N1 C11 105.91(9) . . ?
C15 N1 C11 111.49(10) . . ?
C13 N1 C11 111.28(9) . . ?
C12 C11 N1 114.59(10) . . ?
C12 C11 H11A 108.6 . . ?
N1 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
N1 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N1 115.21(10) . . ?
C14 C13 H13A 108.5 . . ?
N1 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N1 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 115.31(10) . . ?
C16 C15 H15A 108.4 . . ?
N1 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
N1 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N1 114.69(10) . . ?
C18 C17 H17A 108.6 . . ?
N1 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
N1 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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 C1 1.8758(12) . ?
Ru1 C4 1.9095(12) . ?
Ru1 C3 1.9214(13) . ?
Ru1 C2 1.9293(13) . ?
Ru1 Ru1 2.9857(2) 3_566 ?
C1 O1 1.1566(15) . ?
C2 O2 1.1509(16) . ?
C3 O3 1.1583(16) . ?
C4 O4 1.1635(16) . ?
N1 C17 1.5206(15) . ?
N1 C15 1.5221(15) . ?
N1 C13 1.5224(15) . ?
N1 C11 1.5231(14) . ?
C11 C12 1.5135(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.5165(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.5167(18) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.5157(17) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
