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_7040589
_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         'C35 H48 Cl2 N2 O P Ru'
_chemical_formula_sum            'C35 H48 Cl2 N2 O P Ru'
_chemical_formula_weight         715.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0661(19)
_cell_length_b                   17.902(2)
_cell_length_c                   28.165(4)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.25
_cell_measurement_theta_min      2.79
_cell_volume                     7092.3(16)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.2976
_diffrn_reflns_av_unetI/netI     0.2324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.305
_diffrn_reflns_theta_min         1.978
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       Plates
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.00081(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   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.2365
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0602P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3236
_reflns_number_total             8801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           15lm_darkwa_gershon_ga017
_cod_original_cell_volume        7092.4(17)
_cod_database_code               7040589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C29(H29), C30(H30), C19(H19), C18(H18), C17(H17),
 C16(H16), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C0AA(H0AA), N1(H1),
  C6(H6)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C),
 C3(H3A,H3B,H3C)
;
_shelx_res_checksum              16769
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'