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_7714842
_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         'C33 H52 N2 O2 P2 Ru'
_chemical_formula_sum            'C33 H52 N2 O2 P2 Ru'
_chemical_formula_weight         671.77
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-18
_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                 93.4600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.5021(2)
_cell_length_b                   30.8326(7)
_cell_length_c                   33.7646(6)
_cell_measurement_reflns_used    6004
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.819
_cell_measurement_theta_min      2.622
_cell_volume                     11952.4(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (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
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0909
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20046
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        65.083
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         1.942
_diffrn_source                   'copper microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  0.584212
_exptl_absorpt_correction_T_min  0.362922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 67139 reflections, Rint = 0.0909
 (16800 with I > 3sig(I), Rint = 0.0640)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       block
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.131
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         20046
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0994
_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^)+(0.1007P)^2^+97.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2346
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14662
_reflns_number_total             20046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04014c2.cif
_cod_data_source_block           ld111_sq
_cod_depositor_comments
'Adding full bibliography for 7714837--7714844.cif.'
_cod_database_code               7714842
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All Ru(H) groups
2. Restrained distances
 C93-C94 \\sim C93A-C94 \\sim C95-C94 \\sim C94-C95A
 with sigma of 0.02
 C95A-C93A \\sim C93-C95
 with sigma of 0.04
 P6-C93A \\sim P6-C93 \\sim P6-C95 \\sim P6-C95A
 with sigma of 0.04
 N2-C26 \\sim N2A-C26A \\sim N2-C25 \\sim N2A-C25A
 with sigma of 0.02
 N5-C87 \\sim N5-C88 \\sim N5-C87A \\sim N5-C88A
 with sigma of 0.02
 N2-C9 \\sim N2A-C9
 with sigma of 0.02
 C69-N5 \\sim C69-N5A
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A
 with sigma of 0.04
 C87-C88 \\sim C87A-C88A
 with sigma of 0.04
 C9-C25 \\sim C9-C26 \\sim C9-C25A \\sim C9-C26A
 with sigma of 0.04
 C69-C87 \\sim C69-C88 \\sim C69-C87A \\sim C69-C88A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C93 \\sim C93A \\sim C95 \\sim C95A: within 3A with sigma of 0.02 and sigma for
terminal atoms of 0.04
N2 \\sim C25 \\sim N2A \\sim C25A \\sim C26A \\sim C26: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04
C88A \\sim C88 \\sim N5 \\sim N5A \\sim C87A \\sim C87: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04
O2 \\sim C33 \\sim O1: within 3A with sigma of 0.005 and sigma for terminal
atoms of 0.001
O5 \\sim O6 \\sim C99: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04
O4 \\sim O3 \\sim C66: within 3A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C88A) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C87A) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C99) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C93A)=Sof(H93D)=Sof(H93E)=Sof(H93F)=Sof(H94A)=Sof(C95A)=Sof(H95D)=
 Sof(H95E)=Sof(H95F)=1-FVAR(1)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(H94)=Sof(C95)=Sof(H95A)=Sof(H95B)=
 Sof(H95C)=FVAR(1)
 Sof(N2A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(N2)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=FVAR(2)
 Sof(N5A)=Sof(C88A)=Sof(H88D)=Sof(H88E)=Sof(H88F)=Sof(C87A)=Sof(H87D)=
 Sof(H87E)=Sof(H87F)=1-FVAR(3)
 Sof(N5)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(H88C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31), C49(H49), C52(H52), C61(H61),
 C64(H64), C82(H82), C85(H85), C94(H94), C94(H94A), C97(H97)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C10(H10), C33(H33), C35(H35), C37(H37), C41(H41),
 C43(H43), C66(H66), C68(H68), C70(H70), C74(H74), C76(H76), C99(H99)
5.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), C48(H48A,H48B,
 H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C81(H81A,H81B,H81C), C83(H83A,
 H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C),
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C93A(H93D,H93E,H93F),
 C95(H95A,H95B,H95C), C95A(H95D,H95E,H95F), C96(H96A,H96B,H96C), C98(H98A,H98B,
 H98C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C88A(H88D,H88E,H88F),
 C87A(H87D,H87E,H87F)
;
_shelx_res_checksum              1876
_shelx_fab_checksum              92865
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'