Structural, Kinetic, and DFT Studies of the Transfer Hydro-genation of Ketones Mediated by (Pyrazole)pyridine Iron(II) and Nickel(II) Complexes
Magubane, Makhosozane N.; Nyamato, George Simba; Ojwach, Stephen O.; Munro, Orde Q.; RSC Adv.  (2016) –; doi:10.1039/C6RA12788F

data_7225764
_publ_section_title
;
 Structural, Kinetic, and DFT Studies of the Transfer Hydro-genation of
 Ketones Mediated by (Pyrazole)pyridine Iron(II) and Nickel(II) Complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA12788F
_journal_year                    2016
_chemical_formula_moiety         '2(Br), C34 H42 N10 Ni, H2 O'
_chemical_formula_sum            'C34 H44 Br2 N10 Ni O'
_chemical_formula_weight         827.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-08
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_audit_update_record
;
2016-05-16 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.113(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.2365(8)
_cell_length_b                   12.1008(6)
_cell_length_c                   38.373(2)
_cell_measurement_temperature    100.15
_cell_volume                     7075.0(6)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            61206
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.79
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.5358
_exptl_absorpt_correction_T_min  0.3951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         16119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+9.6494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                13567
_reflns_number_total             16119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra12788f2.cif
_cod_data_source_block           mo_so_george_gnc2_cry2_0ma
_cod_original_cell_volume        7074.9(6)
_cod_database_code               7225764
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H31 of C31, H8 of C8, H9 of C9, H10 of C10, {H12A,H12B} of C12, {H6A,H6B}
  of C6, H15 of C15, H3 of C3, {H29A,H29B} of C29, H27 of C27, H26 of C26, H25
  of C25, {H23A,H23B} of C23, H20 of C20
 At 1.5 times of:
  {H33A,H33B,H33C} of C33, {H34A,H34B,H34C} of C34, {H14A,H14B,H14C} of C14,
  {H5A,H5B,H5C} of C5, {H1A,H1B,H1C} of C1, {H22A,H22B,H22C} of C22, {H18A,H18B,
  H18C} of C18, {H17A,H17B,H17C} of C17
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C23(H23A,H23B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C15(H15), C20(H20), C25(H25), C26(H26),
 C27(H27), C31(H31)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;