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_7061432
_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         'C31 H29 N5 O3 Ru, 2(Cl O4), H2 O, C2 H6 O'
_chemical_formula_sum            'C33 H37 Cl2 N5 O13 Ru'
_chemical_formula_weight         883.64
_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
_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                83.522(3)
_cell_angle_beta                 69.862(2)
_cell_angle_gamma                82.487(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3948(10)
_cell_length_b                   12.4038(10)
_cell_length_c                   14.2466(12)
_cell_measurement_reflns_used    234
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.165
_cell_measurement_theta_min      2.408
_cell_volume                     1869.3(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            65108
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.165
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       Block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8246
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7615
_reflns_number_total             8246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04736a2.cif
_cod_data_source_block           sb-am-36_a
_cod_depositor_comments
'Adding full bibliography for 7061431--7061433.cif.'
_cod_database_code               7061432
_shelx_shelxl_version_number     2018/3
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O32-C33 \\sim O32A-C33A
 with sigma of 0.02
 O32-C34 \\sim O32A-C34A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O32) \\sim Ueq, Uanis(O32A) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34A)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O32, C34, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O32(0.45) H32(0.45) C33(0.45) H33A(0.45) H33B(0.45) H33C(0.45)
 C34(0.45) H34A(0.45) H34B(0.45) O32A(0.55) H32A(0.55) C33A(0.55) H33D(0.55)
 H33E(0.55) H33F(0.55) C34A(0.55) H34C(0.55) H34D(0.55)
6.a Free rotating group:
 O101(H10A,H10B)
6.b Rotating group:
 O3(H3A,H3B)
6.c Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C34A(H34C,H34D)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C31(H31), C2(H2), C15(H15), C14(H14), C12(H12), C11(H11), C8(H8),
 C7(H7), C5(H5), C4(H4), C20(H20), C19(H19), C18(H18), C17(H17), C23(H23),
 C24(H24), C25(H25), C28(H28), C29(H29), C30(H30)
6.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F)
6.f Idealised tetrahedral OH refined as rotating group:
 O32(H32), O32A(H32A)
;
_shelx_res_checksum              69390
_olex2_submission_special_instructions 'No special instructions were received'