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_7040110
_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         'C20 Fe N3 Pd0.5, C36 B F21'
_chemical_formula_sum            'C53 B0.5 Cl2 F0.5 Fe0.5 N14 Pd2.5'
_chemical_formula_weight         1212.40
_chemical_name_systematic
;
 ?
;
_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'
_audit_block_doi                 10.5517/cc146xmw
_audit_creation_date             2014-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                68.205(4)
_cell_angle_beta                 82.925(4)
_cell_angle_gamma                74.290(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0582(16)
_cell_length_b                   14.0879(17)
_cell_length_c                   15.0938(19)
_cell_measurement_reflns_used    2027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.82
_cell_measurement_theta_min      2.54
_cell_volume                     2481.1(5)
_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)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.966
_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  0.0846
_diffrn_reflns_av_unetI/netI     0.2582
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17183
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.387
_diffrn_reflns_theta_min         1.605
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0516 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.8886.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         12008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.2521
_refine_ls_R_factor_gt           0.1111
_refine_ls_shift/su_max          1.668
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2776
_refine_ls_wR_factor_ref         0.3722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4730
_reflns_number_total             12008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           mo_13hp_co12_0m
_cod_depositor_comments
'Adding full bibliography for 7040108--7040111.cif.'
_cod_original_formula_sum        'C53 B0.50 Cl2 F0.50 Fe0.50 N14 Pd2.50'
_cod_database_code               7040110
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.786
_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 Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C14(H14), C9(H9), C19(H19), C1g(H1g), C1c(H1c), C1b(H1b),
 C1a(H1a), C24(H24), C26(H26), C23(H23), C41(H41), C39(H39), C35(H35), C31(H31),
  C30(H30), C4(H4), C1I(H1I), C12(H12), C53(H53), C20(H20), C1f(H1f), C18(H18),
 C17(H17), C2(H2), C47(H47)
2.c Idealised Me refined as rotating group:
 C1d(H1da,H1db,H1dc)
;
_shelx_res_checksum              85769