Ruthenium polyhydrides supported by rigid PCP pincer ligands: dynamic behaviour and reactions with CO<sub>2</sub>.
Donnelly, Laurie J.; Lin, Jian-Bin; Gelfand, Benjamin S.; Chang, Chia Yun; Piers, Warren E.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1862–1869; doi:10.1039/d3dt04014c

data_7714839
_publ_section_title
;
 Ruthenium polyhydrides supported by rigid PCP pincer ligands: dynamic
 behaviour and reactions with CO<sub>2</sub>.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1862
_journal_page_last               1869
_journal_paper_doi               10.1039/d3dt04014c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C56 H86 P4 Ru2'
_chemical_formula_sum            'C56 H86 P4 Ru2'
_chemical_formula_weight         1085.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-11-20 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                106.789(4)
_cell_angle_beta                 90.328(4)
_cell_angle_gamma                91.710(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9417(7)
_cell_length_b                   14.5639(11)
_cell_length_c                   17.1311(10)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.665
_cell_measurement_theta_min      3.518
_cell_volume                     2612.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_av_unetI/netI     0.1401
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31954
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.762
_diffrn_reflns_theta_max         66.762
_diffrn_reflns_theta_min         2.694
_diffrn_source_current           0.64
_diffrn_source_power             0.028576
_diffrn_source_voltage           44.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.096
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5391
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1464 before and 0.1092 after correction.
The Ratio of minimum to maximum transmission is 0.7161.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8889
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6822
_reflns_number_total             8889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04014c2.cif
_cod_data_source_block           ld281
_cod_depositor_comments
'Adding full bibliography for 7714837--7714844.cif.'
_cod_database_code               7714839
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Ru1 \\sim H \\sim HA \\sim HB \\sim Ru2 \\sim HC: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
3.a Ternary CH refined with riding coordinates:
 C13(H13), C17(H17), C20(H20), C23(H23), C26(H26), C41(H41), C45(H45),
 C48(H48), C51(H51), C54(H54)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C31(H31), C32(H32),
 C33(H33), C37(H37), C38(H38), C39(H39)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              20657
_olex2_submission_special_instructions 'No special instructions were received'