One-pot atmospheric pressure synthesis of [H<sub>3</sub>Ru<sub>4</sub>(CO)<sub>12</sub>]<sup/>.
Cesari, Cristiana; Bortoluzzi, Marco; Femoni, Cristina; Iapalucci, Maria Carmela; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9610–9622; doi:10.1039/d1dt01517f

data_7707581
_publ_section_title
;
 One-pot atmospheric pressure synthesis of
 [H<sub>3</sub>Ru<sub>4</sub>(CO)<sub>12</sub>]<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            'C39 H36 Br4 K0.5 N1.5 O33 Ru10'
_chemical_formula_weight         2403.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 99.623(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.7547(15)
_cell_length_b                   13.3024(6)
_cell_length_c                   32.2056(15)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.180
_cell_measurement_theta_min      2.479
_cell_volume                     13412.7(11)
_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  0.0602
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            86381
_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         25.998
_diffrn_reflns_theta_min         1.663
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.682
_exptl_absorpt_correction_T_max  0.5628
_exptl_absorpt_correction_T_min  0.4078
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1342 (selected reflections only, before parameter refinement)
 R(int) = 0.0631 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.381
_exptl_crystal_description       prism
_exptl_crystal_F_000             9072
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13176
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0529
_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/[\s^2^(Fo^2^)+(0.0268P)^2^+426.8114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11687
_reflns_number_total             13176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01517f3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7707576--7707590.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C39 H36 Br4 K0.50 N1.50 O33 Ru10'
_cod_database_code               7707581
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.540
_shelx_estimated_absorpt_t_max   0.766
_shelx_res_checksum              7095
_shelx_hkl_checksum              72708