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_7707580
_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            'C56 H84 Br5 K2 N3 O32 Ru8'
_chemical_formula_weight         2597.57
_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
;
2021-05-06 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.980(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.210(3)
_cell_length_b                   24.421(4)
_cell_length_c                   19.758(4)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3085
_cell_measurement_theta_min      2.2225
_cell_volume                     8303(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1250
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59265
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.556
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.4302
_exptl_absorpt_correction_T_min  0.1554
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1835 (selected reflections only, before parameter refinement)
 R(int) = 0.1001 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_description       plate
_exptl_crystal_F_000             5048
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         4.955
_refine_diff_density_min         -2.562
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     571
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1745
_refine_ls_R_factor_gt           0.1514
_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^)+(0.0001P)^2^+2073.4719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3548
_refine_ls_wR_factor_ref         0.3675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11319
_reflns_number_total             14377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01517f3.cif
_cod_data_source_block           2BrTEA3K2
_cod_depositor_comments
'Adding full bibliography for 7707576--7707590.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707580
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.533
_shelx_estimated_absorpt_t_max   0.667
_shelx_res_checksum              99146
_shelx_hkl_checksum              82104