Synthesis, molecular structure and fluxional behavior of the elusive [HRu4(CO)12]3– carbonyl anion
Cesari, Cristiana; Bortoluzzi, Marco; Femoni, Cristina; Iapalucci, Maria Carmela; Zacchini, Stefano; Dalton Transactions  (2022) –; doi:10.1039/D1DT03622J

data_7709216
_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            'C36 H61 N3 O12 Ru4'
_chemical_formula_weight         1132.15
_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   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                 97.884(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9763(8)
_cell_length_b                   19.4012(12)
_cell_length_c                   18.0370(11)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.860
_cell_measurement_theta_min      2.510
_cell_volume                     4498.0(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0815
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56877
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.036
_diffrn_reflns_theta_min         1.549
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.3348
_exptl_absorpt_correction_T_min  0.2641
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1244 (selected reflections only, before parameter refinement)
 R(int) = 0.0823 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.194
_refine_diff_density_min         -1.663
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         8833
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0879
_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/[\s^2^(Fo^2^)+(0.0658P)^2^+49.9903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7610
_reflns_number_total             8833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03622j3.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709216
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.863
_shelx_res_checksum              4572
_shelx_hkl_checksum              30568