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_7714843
_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         'C65 H102 N4 O3 P4 Ru2'
_chemical_formula_sum            'C65 H102 N4 O3 P4 Ru2'
_chemical_formula_weight         1313.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-11-20 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.262(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9521(16)
_cell_length_b                   16.3988(9)
_cell_length_c                   25.3602(10)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.895
_cell_measurement_theta_min      3.254
_cell_volume                     9115.3(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31623
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.046
_diffrn_reflns_theta_max         67.046
_diffrn_reflns_theta_min         3.255
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0733 before and 0.0476 after correction. The Ratio of minimum to maximum transmission is 0.8120. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.696
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1244P)^2^+28.6225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6697
_reflns_number_total             8059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04014c2.cif
_cod_data_source_block           ld137_sq
_cod_depositor_comments
'Adding full bibliography for 7714837--7714844.cif.'
_cod_database_code               7714843
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.377
_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, All O(H) groups
2. Restrained distances
 N2A-C9 \\sim N2-C9
 with sigma of 0.02
 N2-C26 \\sim N2A-C26A \\sim N2A-C25A \\sim N2-C25
 with sigma of 0.02
 C9-C25 \\sim C9-C25A \\sim C9-C26 \\sim C9-C26A
 with sigma of 0.04
 C8-N2 \\sim C8-N2A \\sim C10-N2 \\sim C10-N2A
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim C33: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02
N2 \\sim C25 \\sim C26 \\sim N2A \\sim C25A \\sim C26A: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N2, C25, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N2A, C25A, C26A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(N2A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(N2)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=FVAR(1)
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) C33(0.5)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C10(H10)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C25A(H25D,H25E,
 H25F), C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              19060
_shelx_fab_checksum              30995
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'