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#$Date: 2021-09-06 14:01:32 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268730 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707586.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_7707586
loop_
_publ_author_name
'Cesari, Cristiana'
'Bortoluzzi, Marco'
'Femoni, Cristina'
'Iapalucci, Maria Carmela'
'Zacchini, Stefano'
_publ_section_title
;
 One-pot atmospheric pressure synthesis of
 [H₃Ru₄(CO)₁₂]<sup/>.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9610
_journal_page_last               9622
_journal_paper_doi               10.1039/d1dt01517f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C14 H6 Cu N O12 Ru4'
_chemical_formula_weight         848.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-05-06 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.3950(10)
_cell_angle_beta                 71.6300(10)
_cell_angle_gamma                85.3670(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5369(3)
_cell_length_b                   10.0317(4)
_cell_length_c                   13.1229(5)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0815
_cell_measurement_theta_min      2.519
_cell_volume                     1062.25(7)
_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 0.999
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  0.4343
_exptl_absorpt_correction_T_min  0.3097
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1194 (selected reflections only, before parameter refinement)
 R(int) = 0.0472 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.651
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0170
_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)+(0.0067P)²+0.7710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4272
_reflns_number_total             4626
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01517f3.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7707576--7707590.cif.'
_cod_database_code               7707586
_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   0.501
_shelx_estimated_absorpt_t_max   0.617
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_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 0.47625(2) 0.26666(2) 0.84977(2) 0.01207(5) Uani 1 1 d . . . . .
Ru2 Ru 0.66129(2) 0.43574(2) 0.68650(2) 0.01115(5) Uani 1 1 d . . . . .
H1 H 0.836(3) 0.315(3) 0.641(2) 0.013 Uiso 1 1 d . U . . .
Ru3 Ru 0.76517(2) 0.15110(2) 0.70975(2) 0.01146(5) Uani 1 1 d . . . . .
H2 H 0.673(3) 0.140(3) 0.613(2) 0.014 Uiso 1 1 d . U . . .
Ru4 Ru 0.46665(2) 0.22853(2) 0.64353(2) 0.01143(5) Uani 1 1 d . . . . .
H3 H 0.595(3) 0.373(3) 0.583(2) 0.014 Uiso 1 1 d . U . . .
Cu1 Cu 0.77752(4) 0.27232(3) 0.51522(2) 0.01872(7) Uani 1 1 d . . . . .
C1 C 0.5476(3) 0.3125(3) 0.9650(2) 0.0182(5) Uani 1 1 d . . . . .
C2 C 0.2761(3) 0.3751(3) 0.8959(2) 0.0176(5) Uani 1 1 d . . . . .
C3 C 0.3822(3) 0.1108(3) 0.9249(2) 0.0184(5) Uani 1 1 d . . . . .
C4 C 0.7428(3) 0.4868(3) 0.7954(2) 0.0168(5) Uani 1 1 d . . . . .
C5 C 0.4770(3) 0.5610(3) 0.7293(2) 0.0156(5) Uani 1 1 d . . . . .
C6 C 0.7940(3) 0.5528(3) 0.5759(2) 0.0162(5) Uani 1 1 d . . . . .
C7 C 0.8512(3) 0.1792(3) 0.8231(2) 0.0185(5) Uani 1 1 d . . . . .
C8 C 0.6902(3) -0.0187(3) 0.7673(2) 0.0187(5) Uani 1 1 d . . . . .
C9 C 0.9768(3) 0.0904(3) 0.6118(2) 0.0156(5) Uani 1 1 d . . . . .
C10 C 0.3506(3) 0.0791(3) 0.7146(2) 0.0181(5) Uani 1 1 d . . . . .
C11 C 0.2688(3) 0.3394(3) 0.6781(2) 0.0172(5) Uani 1 1 d . . . . .
C12 C 0.4664(3) 0.1883(3) 0.5010(2) 0.0156(5) Uani 1 1 d . . . . .
O1 O 0.5839(3) 0.3402(2) 1.03754(15) 0.0281(5) Uani 1 1 d . . . . .
O2 O 0.1541(2) 0.4378(2) 0.92560(15) 0.0266(5) Uani 1 1 d . . . . .
O3 O 0.3211(3) 0.0204(2) 0.97439(16) 0.0282(5) Uani 1 1 d . . . . .
O4 O 0.7967(3) 0.5231(2) 0.85726(16) 0.0257(5) Uani 1 1 d . . . . .
O5 O 0.3696(2) 0.6401(2) 0.75219(15) 0.0237(4) Uani 1 1 d . . . . .
O6 O 0.8673(2) 0.6326(2) 0.52077(16) 0.0228(4) Uani 1 1 d . . . . .
O7 O 0.9130(3) 0.1932(2) 0.88684(16) 0.0258(5) Uani 1 1 d . . . . .
O8 O 0.6491(3) -0.1227(2) 0.79809(17) 0.0275(5) Uani 1 1 d . . . . .
O9 O 1.1077(2) 0.0541(2) 0.56448(15) 0.0230(4) Uani 1 1 d . . . . .
O10 O 0.2758(3) -0.0106(2) 0.75236(16) 0.0255(4) Uani 1 1 d . . . . .
O11 O 0.1495(2) 0.4063(2) 0.69639(16) 0.0252(4) Uani 1 1 d . . . . .
O12 O 0.4505(3) 0.1582(2) 0.42303(15) 0.0230(4) Uani 1 1 d . . . . .
N1 N 0.8886(3) 0.2599(2) 0.36605(17) 0.0175(5) Uani 1 1 d . . . . .
C101 C 0.9337(3) 0.2494(3) 0.2754(2) 0.0174(5) Uani 1 1 d . . . . .
C102 C 0.9862(4) 0.2356(3) 0.1596(2) 0.0238(6) Uani 1 1 d . . . . .
H10A H 0.9241 0.1671 0.1422 0.036 Uiso 1 1 calc R U . . .
H10B H 1.1046 0.2091 0.1341 0.036 Uiso 1 1 calc R U . . .
H10C H 0.9651 0.3213 0.1246 0.036 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'
Cu Cu 0.3201 1.2651 '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
C3 Ru1 C1 92.22(11) . . ?
C3 Ru1 C2 94.21(12) . . ?
C1 Ru1 C2 93.40(11) . . ?
C3 Ru1 Ru3 99.58(8) . . ?
C1 Ru1 Ru3 102.21(8) . . ?
C2 Ru1 Ru3 158.64(8) . . ?
C3 Ru1 Ru4 101.71(7) . . ?
C1 Ru1 Ru4 162.03(8) . . ?
C2 Ru1 Ru4 96.80(7) . . ?
Ru3 Ru1 Ru4 64.555(7) . . ?
C3 Ru1 Ru2 161.05(8) . . ?
C1 Ru1 Ru2 99.94(8) . . ?
C2 Ru1 Ru2 99.47(8) . . ?
Ru3 Ru1 Ru2 63.780(7) . . ?
Ru4 Ru1 Ru2 63.825(7) . . ?
C4 Ru2 C5 91.56(11) . . ?
C4 Ru2 C6 95.05(11) . . ?
C5 Ru2 C6 94.88(11) . . ?
C4 Ru2 Cu1 135.27(8) . . ?
C5 Ru2 Cu1 132.71(7) . . ?
C6 Ru2 Cu1 77.64(7) . . ?
C4 Ru2 Ru1 83.37(8) . . ?
C5 Ru2 Ru1 85.87(8) . . ?
C6 Ru2 Ru1 178.28(7) . . ?
Cu1 Ru2 Ru1 102.987(11) . . ?
C4 Ru2 Ru3 93.23(8) . . ?
C5 Ru2 Ru3 142.57(8) . . ?
C6 Ru2 Ru3 121.57(8) . . ?
Cu1 Ru2 Ru3 57.279(9) . . ?
Ru1 Ru2 Ru3 57.954(7) . . ?
C4 Ru2 Ru4 140.38(8) . . ?
C5 Ru2 Ru4 93.61(8) . . ?
C6 Ru2 Ru4 123.51(7) . . ?
Cu1 Ru2 Ru4 56.758(9) . . ?
Ru1 Ru2 Ru4 57.933(7) . . ?
Ru3 Ru2 Ru4 60.585(7) . . ?
C4 Ru2 H1 90.5(8) . . ?
C5 Ru2 H1 177.9(8) . . ?
C6 Ru2 H1 84.6(9) . . ?
Cu1 Ru2 H1 45.2(8) . . ?
Ru1 Ru2 H1 94.7(9) . . ?
Ru3 Ru2 H1 37.5(9) . . ?
Ru4 Ru2 H1 85.0(9) . . ?
C4 Ru2 H3 174.6(9) . . ?
C5 Ru2 H3 93.4(9) . . ?
C6 Ru2 H3 86.5(9) . . ?
Cu1 Ru2 H3 40.1(9) . . ?
Ru1 Ru2 H3 95.0(9) . . ?
Ru3 Ru2 H3 81.6(9) . . ?
Ru4 Ru2 H3 37.2(9) . . ?
H1 Ru2 H3 84.5(12) . . ?
C8 Ru3 C7 93.39(11) . . ?
C8 Ru3 C9 97.97(11) . . ?
C7 Ru3 C9 94.39(11) . . ?
C8 Ru3 Cu1 129.22(8) . . ?
C7 Ru3 Cu1 136.68(8) . . ?
C9 Ru3 Cu1 74.58(7) . . ?
C8 Ru3 Ru1 88.13(8) . . ?
C7 Ru3 Ru1 82.71(8) . . ?
C9 Ru3 Ru1 173.41(8) . . ?
Cu1 Ru3 Ru1 103.482(10) . . ?
C8 Ru3 Ru2 144.27(8) . . ?
C7 Ru3 Ru2 93.85(8) . . ?
C9 Ru3 Ru2 116.26(8) . . ?
Cu1 Ru3 Ru2 57.589(9) . . ?
Ru1 Ru3 Ru2 58.266(7) . . ?
C8 Ru3 Ru4 93.46(8) . . ?
C7 Ru3 Ru4 139.53(8) . . ?
C9 Ru3 Ru4 123.95(7) . . ?
Cu1 Ru3 Ru4 56.538(9) . . ?
Ru1 Ru3 Ru4 57.724(7) . . ?
Ru2 Ru3 Ru4 59.739(7) . . ?
C8 Ru3 H1 174.7(8) . . ?
C7 Ru3 H1 91.8(8) . . ?
C9 Ru3 H1 80.4(9) . . ?
Cu1 Ru3 H1 45.5(8) . . ?
Ru1 Ru3 H1 93.7(8) . . ?
Ru2 Ru3 H1 36.2(8) . . ?
Ru4 Ru3 H1 83.3(8) . . ?
C8 Ru3 H2 89.2(10) . . ?
C7 Ru3 H2 173.8(9) . . ?
C9 Ru3 H2 90.9(9) . . ?
Cu1 Ru3 H2 42.1(10) . . ?
Ru1 Ru3 H2 91.7(9) . . ?
Ru2 Ru3 H2 80.8(9) . . ?
Ru4 Ru3 H2 34.5(9) . . ?
H1 Ru3 H2 85.8(13) . . ?
C11 Ru4 C10 91.12(12) . . ?
C11 Ru4 C12 96.05(10) . . ?
C10 Ru4 C12 95.77(11) . . ?
C11 Ru4 Cu1 131.71(8) . . ?
C10 Ru4 Cu1 136.56(8) . . ?
C12 Ru4 Cu1 75.60(8) . . ?
C11 Ru4 Ru1 87.38(7) . . ?
C10 Ru4 Ru1 81.52(7) . . ?
C12 Ru4 Ru1 175.70(8) . . ?
Cu1 Ru4 Ru1 104.049(10) . . ?
C11 Ru4 Ru2 93.48(8) . . ?
C10 Ru4 Ru2 139.17(7) . . ?
C12 Ru4 Ru2 123.93(8) . . ?
Cu1 Ru4 Ru2 57.774(9) . . ?
Ru1 Ru4 Ru2 58.242(7) . . ?
C11 Ru4 Ru3 143.17(7) . . ?
C10 Ru4 Ru3 94.55(8) . . ?
C12 Ru4 Ru3 119.43(8) . . ?
Cu1 Ru4 Ru3 57.236(9) . . ?
Ru1 Ru4 Ru3 57.721(7) . . ?
Ru2 Ru4 Ru3 59.676(7) . . ?
C11 Ru4 H2 172.2(9) . . ?
C10 Ru4 H2 94.9(9) . . ?
C12 Ru4 H2 88.2(8) . . ?
Cu1 Ru4 H2 43.2(9) . . ?
Ru1 Ru4 H2 88.7(8) . . ?
Ru2 Ru4 H2 78.7(9) . . ?
Ru3 Ru4 H2 31.4(8) . . ?
C11 Ru4 H3 92.3(8) . . ?
C10 Ru4 H3 173.9(8) . . ?
C12 Ru4 H3 88.9(8) . . ?
Cu1 Ru4 H3 41.2(8) . . ?
Ru1 Ru4 H3 93.6(8) . . ?
Ru2 Ru4 H3 35.5(8) . . ?
Ru3 Ru4 H3 79.8(8) . . ?
H2 Ru4 H3 81.3(12) . . ?
N1 Cu1 Ru4 134.25(7) . . ?
N1 Cu1 Ru3 142.02(7) . . ?
Ru4 Cu1 Ru3 66.226(10) . . ?
N1 Cu1 Ru2 146.78(7) . . ?
Ru4 Cu1 Ru2 65.468(9) . . ?
Ru3 Cu1 Ru2 65.132(9) . . ?
N1 Cu1 H1 136.2(8) . . ?
Ru4 Cu1 H1 89.5(8) . . ?
Ru3 Cu1 H1 43.2(8) . . ?
Ru2 Cu1 H1 41.3(8) . . ?
N1 Cu1 H2 128.7(8) . . ?
Ru4 Cu1 H2 42.8(8) . . ?
Ru3 Cu1 H2 37.7(8) . . ?
Ru2 Cu1 H2 84.3(8) . . ?
H1 Cu1 H2 79.3(12) . . ?
N1 Cu1 H3 129.3(9) . . ?
Ru4 Cu1 H3 43.3(9) . . ?
Ru3 Cu1 H3 88.1(9) . . ?
Ru2 Cu1 H3 40.2(9) . . ?
H1 Cu1 H3 80.7(12) . . ?
H2 Cu1 H3 82.8(12) . . ?
O1 C1 Ru1 177.0(2) . . ?
O2 C2 Ru1 178.2(3) . . ?
O3 C3 Ru1 176.7(2) . . ?
O4 C4 Ru2 176.1(3) . . ?
O5 C5 Ru2 177.2(2) . . ?
O6 C6 Ru2 171.5(2) . . ?
O7 C7 Ru3 175.4(3) . . ?
O8 C8 Ru3 177.2(3) . . ?
O9 C9 Ru3 171.9(2) . . ?
O10 C10 Ru4 175.5(2) . . ?
O11 C11 Ru4 178.3(2) . . ?
O12 C12 Ru4 172.5(2) . . ?
C101 N1 Cu1 170.2(2) . . ?
N1 C101 C102 178.3(3) . . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 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 C3 1.889(3) . ?
Ru1 C1 1.892(3) . ?
Ru1 C2 1.897(3) . ?
Ru1 Ru3 2.7844(3) . ?
Ru1 Ru4 2.7845(3) . ?
Ru1 Ru2 2.7938(3) . ?
Ru2 C4 1.888(3) . ?
Ru2 C5 1.893(3) . ?
Ru2 C6 1.932(3) . ?
Ru2 Cu1 2.7421(4) . ?
Ru2 Ru3 2.9469(3) . ?
Ru2 Ru4 2.9489(3) . ?
Ru2 H1 1.81(3) . ?
Ru2 H3 1.79(3) . ?
Ru3 C8 1.895(3) . ?
Ru3 C7 1.899(3) . ?
Ru3 C9 1.935(3) . ?
Ru3 Cu1 2.7327(4) . ?
Ru3 Ru4 2.9739(3) . ?
Ru3 H1 1.87(3) . ?
Ru3 H2 1.70(3) . ?
Ru4 C11 1.890(3) . ?
Ru4 C10 1.892(3) . ?
Ru4 C12 1.939(2) . ?
Ru4 Cu1 2.7110(4) . ?
Ru4 H2 1.84(3) . ?
Ru4 H3 1.87(3) . ?
Cu1 N1 1.894(2) . ?
Cu1 H1 1.95(3) . ?
Cu1 H2 1.86(3) . ?
Cu1 H3 1.79(3) . ?
C1 O1 1.146(3) . ?
C2 O2 1.141(3) . ?
C3 O3 1.143(3) . ?
C4 O4 1.142(3) . ?
C5 O5 1.140(3) . ?
C6 O6 1.131(3) . ?
C7 O7 1.141(3) . ?
C8 O8 1.136(3) . ?
C9 O9 1.137(3) . ?
C10 O10 1.140(3) . ?
C11 O11 1.141(3) . ?
C12 O12 1.135(3) . ?
N1 C101 1.138(3) . ?
C101 C102 1.454(3) . ?
C102 H10A 0.9800 . ?
C102 H10B 0.9800 . ?
C102 H10C 0.9800 . ?
