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_7039533
_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         'C53 H41 Cl N3 O P2 Ru, F6 P, 3(C3 H3)'
_chemical_formula_sum            'C62 H50 Cl F6 N3 O P3 Ru'
_chemical_formula_weight         1196.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 98.455(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.058(5)
_cell_length_b                   23.924(5)
_cell_length_c                   22.914(5)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.50
_cell_volume                     5454(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         4.096
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1481 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.8250.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.483
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0381P)^2^+27.7519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7342
_reflns_number_total             9570
_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               7039533
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C74) = Uanis(C80) = Uanis(C76) = Uanis(C51) = Uanis(C2) = Uanis(C50)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C16(H16), C18(H18), C21(H21), C25(H25), C27(H27), C28(H28),
 C30(H30), C32(H32), C35(H35), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C72(H72), C73(H73), C75(H75), C80(H80), C76(H76), C51(H51),
  C2(H2), C50(H50), C74(H74)
3.b Fitted hexagon refined as free rotating group:
 C80(C76,C51,C2,C50,C74)
3.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              93572
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'