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_7714844
_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         'C64 H104 N6 P4 Ru2'
_chemical_formula_sum            'C64 H104 N6 P4 Ru2'
_chemical_formula_weight         1283.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-11-20 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.7299(4)
_cell_length_b                   38.8794(11)
_cell_length_c                   49.0089(12)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      68.382
_cell_measurement_theta_min      2.902
_cell_volume                     31877.8(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            33185
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.64
_diffrn_source_power             0.0285952
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           44.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0747 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.8808.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             10848
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     864
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0835
_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^)+(0.0427P)^2^+1145.6963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5666
_reflns_number_total             7033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04014c2.cif
_cod_data_source_block           ld198
_cod_depositor_comments
'Adding full bibliography for 7714837--7714844.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7714844
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.563
_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. Restrained distances
 P1-C16A \\sim P1-C16B \\sim P1-C19A \\sim P1-C19B \\sim P2-C28A \\sim P2-C28B
\\sim P2-C31A \\sim P2-C31B
 with sigma of 0.02
 C16A-C15A \\sim C17A-C16A \\sim C16B-C15B \\sim C17B-C16B \\sim C19A-C18A
\\sim C20A-C19A \\sim C19B-
 C18B \\sim C20B-C19B \\sim C28A-C27A \\sim C29A-C28A \\sim C28B-C27B \\sim
C29B-C28B \\sim C31A-C30A ~
 C32A-C31A \\sim C31B-C30B \\sim C32B-C31B
 with sigma of 0.02
 C15A-C17A \\sim C15B-C17B \\sim C18A-C20A \\sim C18B-C20B \\sim C27A-C29A
\\sim C27B-C29B \\sim C30A-
 C32A \\sim C30B-C32B
 with sigma of 0.04
 C15A-P1 \\sim C17A-P1 \\sim C18A-P1 \\sim C20A-P1 \\sim C27A-P2 \\sim C29A-P2
\\sim C30A-P2 \\sim C32A-P2
 \\sim C15B-P1 \\sim C17B-P1 \\sim C18B-P1 \\sim C20B-P1 \\sim C27B-P2 \\sim
C29B-P2 \\sim C30B-P2 \\sim C32B-P2
 with sigma of 0.04
 C16A-C3 \\sim C19A-C3 \\sim C28A-C13 \\sim C31A-C13 \\sim C16B-C3 \\sim
C19B-C3 \\sim C28B-C13 \\sim C31B-
 C13
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
P2 \\sim C27A \\sim C27B \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim C30A
\\sim C30B \\sim C31A \\sim C31B \\sim C32A \\sim C32B: within 3A with sigma of
0.015 and sigma for terminal atoms of 0.015 within 3A
P1 \\sim C15A \\sim C15B \\sim C16A \\sim C16B \\sim C17A \\sim C17B \\sim C18A
\\sim C18B \\sim C19A \\sim C19B \\sim C20A \\sim C20B: within 3A with sigma of
0.015 and sigma for terminal atoms of 0.015 within 3A
4. Others
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16B)=Sof(C17B)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(C17A)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
 Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=Sof(H28B)=Sof(C29B)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(2)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(2)
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=Sof(H31B)=Sof(C32B)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=Sof(H31A)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19B)=Sof(C20B)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(4)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C16A(H16A), C16B(H16B), C19A(H19A), C19B(H19B), C28A(H28A),
 C28B(H28B), C31A(H31A), C31B(H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C12(H12)
5.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C20A(H20A,H20B,H20C),
 C20B(H20D,H20E,H20F), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F), C29A(H29A,H29B,H29C), C29B(H29D,
 H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F), C32A(H32A,H32B,H32C),
 C32B(H32D,H32E,H32F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80441
_shelx_fab_checksum              6394
_olex2_submission_special_instructions 'No special instructions were received'