Optimum bifunctionality in a 2-(2-pyridyl-2-ol)-1,10-phenanthroline based ruthenium complex for transfer hydrogenation of ketones and nitriles: impact of the number of 2-hydroxypyridine fragments.
Paul, Bhaskar; Chakrabarti, Kaushik; Kundu, Sabuj; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11162–11171; doi:10.1039/c6dt01961g

data_7039532
_publ_section_title
;
 Optimum bifunctionality in a 2-(2-pyridyl-2-ol)-1,10-phenanthroline based
 ruthenium complex for transfer hydrogenation of ketones and nitriles:
 impact of the number of 2-hydroxypyridine fragments.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11162
_journal_page_last               11171
_journal_paper_doi               10.1039/c6dt01961g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C54 H43 Cl N3 O P2 Ru, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C56 H47 Cl5 F6 N3 O P3 Ru'
_chemical_formula_weight         1263.19
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-02-16 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                101.331(5)
_cell_angle_beta                 91.090(5)
_cell_angle_gamma                100.225(5)
_cell_formula_units_Z            2
_cell_length_a                   11.925(5)
_cell_length_b                   14.713(5)
_cell_length_c                   15.876(5)
_cell_measurement_reflns_used    3706
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.45
_cell_volume                     2683.6(17)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13852
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         4.079
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6670
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0627 before and 0.0381 after correction.
The Ratio of minimum to maximum transmission is 0.8951.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.153
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         9255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1509P)^2^+5.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6969
_reflns_number_total             9255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01961g2.cif
_cod_data_source_block           Complex
_cod_depositor_comments
'Adding full bibliography for 7039532--7039533.cif.'
_cod_database_code               7039532
_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
2.a Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C85(H85A,H85B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C54(H54), C23(H23), C29(H29), C15(H15), C45(H45), C49(H49),
 C33(H33), C6(H6), C53(H53), C5(H5), C32(H32), C39(H39), C44(H44), C35(H35),
 C28(H28), C34(H34), C22(H22), C3(H3), C11(H11), C40(H40), C14(H14), C2(H2),
 C31(H31), C16(H16), C25(H25), C52(H52), C27(H27), C12(H12), C9(H9), C18(H18),
 C8(H8), C26(H26), C4(H4), C17(H17), C21(H21), C24(H24), C48(H48), C41(H41),
 C10(H10)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              59663
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'