Development of a ruthenium–aquo complex for utilization in synthesis and catalysis for selective hydration of nitriles and alkynes
Saha, Rumpa; Mukherjee, Aparajita; Bhattacharya, Samaresh; New Journal of Chemistry 46 (2022) 9098–9110; doi:10.1039/D1NJ04736A

data_7061431
_publ_section_title
;
 Development of a ruthenium--aquo complex for utilization in synthesis and
 catalysis for selective hydration of nitriles and alkynes
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9098
_journal_page_last               9110
_journal_paper_doi               10.1039/D1NJ04736A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C37 H34 N6 O2 Ru, 2(Cl O4), 3[H2O]'
_chemical_formula_sum            'C37 H40 Cl2 N6 O13 Ru'
_chemical_formula_weight         948.72
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-14
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.03.10 svn.r54f81f84 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-04-05 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.054(3)
_cell_length_b                   11.0969(10)
_cell_length_c                   25.405(2)
_cell_measurement_reflns_used    300
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.136
_cell_measurement_theta_min      1.956
_cell_volume                     8472.7(13)
_computing_data_collection       'APEX3 (Bruker)'
_computing_data_reduction        'APEX3 (Bruker)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1191
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            175782
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.956
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       Block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         15798
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0633P)^2^+11.9093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12122
_reflns_number_total             15798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04736a2.cif
_cod_data_source_block           sb-rs-60-o-s4
_cod_depositor_comments
'Adding full bibliography for 7061431--7061433.cif.'
_cod_original_cell_volume        8472.6(13)
_cod_database_code               7061431
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.81(6)
 0.19(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl4A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O303) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O6, Cl4A, O5, O7, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O404, Cl4, O401, O403, O402
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl3, O301, O302, O304, O303
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl4A)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=1-FVAR(1)
 Sof(Cl4)=Sof(O401)=Sof(O403)=Sof(O404)=Sof(O402)=FVAR(1)
 Fixed X: Ru1(0.76233)
 Fixed Y: Ru1(0.48866)
 Fixed Z: Ru1(0.53804)
6.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C68(H68), C65(H65), C1(H1), C70(H70), C55(H55), C54(H54), C69(H69),
 C23(H23), C19(H19), C51(H51), C31(H31), C36(H36), C2(H2), C11(H11), C15(H15),
 C72(H72), C60(H60), C18(H18), C38(H38), C12(H12), C32(H32), C66(H66), C49(H49),
  C30(H30), C14(H14), C67(H67), C57(H57), C17(H17), C25(H25), C20(H20),
 C73(H73), C24(H24), C39(H39), C29(H29), C52(H52), C56(H56), C61(H61), C33(H33),
  C62(H62), C48(H48), C35(H35), C4(H4), C7(H7), C5(H5), C8(H8), C45(H45),
 C41(H41), C42(H42), C44(H44)
6.b Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C37(H37A,H37B,H37C), C53(H53A,H53B,H53C), C9(H9A,H9B,
 H9C), C16(H16A,H16B,H16C), C46(H46A,H46B,H46C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 256 electrons were 
found in a volume of 1502\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 3[H2O] per Formula Unit 
which account for 240 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87064
_shelx_fab_checksum              73700
_olex2_submission_special_instructions 'No special instructions were received'