RhIII and IrIII complexes bearing NNO-heteroscorpionates and their application in catalytic transfer hydrogenation
Cerón-Castelán, Jesus E.; Salazar-Pereda, Veronica; González-Montiel, Simplicio; Mendoza-Espinosa, Daniel; Castro-Osma, José A.; López-Santos, Laura; Gómez-Bonilla, Manuel A.; Sandoval-Chavez, Cesar I.; New Journal of Chemistry 46 (2022) 19841–19847; doi:10.1039/D2NJ02704F

data_7061925
_publ_section_title
;
 RhIII and IrIII complexes bearing NNO-heteroscorpionates and their
 application in catalytic transfer hydrogenation
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19841
_journal_page_last               19847
_journal_paper_doi               10.1039/D2NJ02704F
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C19 H24 Cl3 Ir N4 O, C H4 O'
_chemical_formula_sum            'C20 H28 Cl3 Ir N4 O2'
_chemical_formula_weight         655.045
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-09-08
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.07.25 svn.r36e0af09 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-09-21 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                87.523(3)
_cell_angle_beta                 84.864(3)
_cell_angle_gamma                74.434(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0513(3)
_cell_length_b                   9.9959(3)
_cell_length_c                   14.4880(5)
_cell_measurement_reflns_used    71161
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.8320
_cell_measurement_theta_min      25.8320
_cell_volume                     1257.41(7)
_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  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9379
_diffrn_measurement_device_type  Atlas
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.9976
_diffrn_reflns_Laue_measured_fraction_max 0.9379
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71161
_diffrn_reflns_point_group_measured_fraction_full 0.9976
_diffrn_reflns_point_group_measured_fraction_max 0.9379
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.86
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    5.650
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             639.364
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.1485
_refine_diff_density_min         -3.3579
_refine_diff_density_rms         0.2912
_refine_ls_d_res_high            0.7137
_refine_ls_d_res_low             6.9170
_refine_ls_goodness_of_fit_ref   1.1002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    49
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6785
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.0972
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+10.9871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5314
_reflns_number_total             6785
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj02704f2.cif
_cod_data_source_block           dm-59
_cod_depositor_comments
'Adding full bibliography for 7061925--7061926.cif.'
_cod_database_code               7061925
_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
 O1-H1
 0.85 with sigma of 0.01
 C12-H1
 1.886286 with sigma of 0.02
 Ir1-H1
 2.745493 with sigma of 0.02
 O0AA-C1AA \\sim O0Ab-C1Ab
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O0Ab) \\sim Ueq, Uanis(C1Ab) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O0Ab, C1Ab
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O0AA(0.5) H0AA(0.5) C1AA(0.5) H1Aa(0.5) H1Ab(0.5) H1Ac(0.5)
 O0Ab(0.5) H0Ab(0.5) C1Ab(0.5) H1Ad(0.5) H1Ae(0.5) H1Af(0.5)
6.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12)
6.b Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C11(H11a,H11b,H11c), C10(H10a,H10b,H10c), C19(H19a,H19b,
 H19c), C5(H5a,H5b,H5c)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C14(H14), C18(H18), C17(H17), C15(H15)
6.d Idealised Me refined as rotating group:
 C1AA(H1Aa,H1Ab,H1Ac), C1Ab(H1Ad,H1Ae,H1Af)
6.e Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA), O0Ab(H0Ab)
;
_olex2_submission_special_instructions 'No special instructions were received'