Novel pyrazolylphosphite- and pyrazolylphosphinite-ruthenium(ii) complexes as catalysts for hydrogenation of acetophenone.
Amenuvor, Gershon; Obuah, Collins; Nordlander, Ebbe; Darkwa, James; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13514–13524; doi:10.1039/c6dt02164f

data_7040592
_publ_section_title
;
 Novel pyrazolylphosphite- and pyrazolylphosphinite-ruthenium(ii)
 complexes as catalysts for hydrogenation of acetophenone.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13514
_journal_page_last               13524
_journal_paper_doi               10.1039/c6dt02164f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C39 H39 Cl2 N2 O P Ru'
_chemical_formula_sum            'C39 H39 Cl2 N2 O P Ru'
_chemical_formula_weight         754.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.11.03 svn.r3071 for OlexSys, GUI svn.r4932)
;
_audit_update_record
;
2015-07-15 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.990(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.682(2)
_cell_length_b                   10.3987(13)
_cell_length_c                   21.897(3)
_cell_measurement_reflns_used    2159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.122
_cell_measurement_theta_min      2.296
_cell_volume                     3870.4(8)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1746
_diffrn_reflns_av_unetI/netI     0.1559
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42619
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         1.735
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.397
_exptl_crystal_size_min          0.212
_refine_diff_density_max         2.357
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       0.0142(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.0840
_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^)+(0.1321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5292
_reflns_number_total             9697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           15lm_darkwa_gershonga039
_cod_database_code               7040592
_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 Ternary CH refined with riding coordinates:
 C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C0AA(H0AA,H0AB)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C23(H23), C36(H36), C20(H20), C19(H19), C29(H29), C17(H17), C35(H35),
 C33(H33), C25(H25), C13(H13), C32(H32), C27(H27), C22(H22), C21(H21), C26(H26),
  C16(H16), C15(H15), C8(H8), C11(H11), C14(H14), C28(H28), C9(H9), C7(H7),
 C10(H10)
2.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              36115
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'