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_7040591
_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         'C31 H39 Cl2 N2 O3 P Ru'
_chemical_formula_sum            'C31 H39 Cl2 N2 O3 P Ru'
_chemical_formula_weight         690.58
_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     direct
_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                 95.697(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1458(18)
_cell_length_b                   8.9406(7)
_cell_length_c                   18.8209(17)
_cell_measurement_reflns_used    2228
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.339
_cell_measurement_theta_min      2.525
_cell_volume                     3038.3(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0960
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26475
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.376
_diffrn_reflns_theta_min         1.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6578
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8821.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5035
_reflns_number_total             7571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           15lm_gershon_ga036
_cod_database_code               7040591
_shelxl_version_number           2014/6
_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:
 C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C20(H20A,H20B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C25(H25), C24(H24), C4(H4), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C22(H22A,H22B,H22C), C21(H21A,H21B,
 H21C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              92039
_olex2_submission_special_instructions 'No special instructions were received'