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_7040590
_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         'C21 H35 Cl2 N2 O3 P Ru'
_chemical_formula_sum            'C21 H35 Cl2 N2 O3 P Ru'
_chemical_formula_weight         566.45
_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     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                75.471(3)
_cell_angle_beta                 89.027(4)
_cell_angle_gamma                69.116(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2138(7)
_cell_length_b                   9.8265(11)
_cell_length_c                   19.515(2)
_cell_measurement_reflns_used    2606
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.373
_cell_measurement_theta_min      2.269
_cell_volume                     1247.1(2)
_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      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  0.0676
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19433
_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         28.340
_diffrn_reflns_theta_min         1.081
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       Block
_exptl_crystal_F_000             584
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0000(2)
_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   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          1.369
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+2.2510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4526
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           15lm_darkwa_gershon_ga032_cen
_cod_database_code               7040590
_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:
 C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C14(H14), C15(H15), C3(H3)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C11(H11A,H11B,H11C), C9(H9A,H9B,
 H9C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              2742
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'