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_7040109
_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         'C19 H17 Fe N3 Pd0.5, C32 H12 B F25.44'
_chemical_formula_sum            'C51 H29 B F24 Fe N3 Pd0.5'
_chemical_formula_weight         1259.63
_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'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc146xlv
_audit_creation_date             2013-05-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.401(4)
_cell_angle_beta                 83.876(5)
_cell_angle_gamma                70.096(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3530(11)
_cell_length_b                   13.7363(12)
_cell_length_c                   14.4942(12)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.33
_cell_measurement_theta_min      3.07
_cell_volume                     2484.5(4)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.591
_diffrn_measured_fraction_theta_max 0.616
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.591
_diffrn_reflns_Laue_measured_fraction_max 0.616
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20258
_diffrn_reflns_point_group_measured_fraction_full 0.591
_diffrn_reflns_point_group_measured_fraction_max 0.616
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.853
_diffrn_reflns_theta_min         3.068
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.049
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_F_000             1252
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         5313
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          14.922
_refine_ls_shift/su_mean         0.217
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4638
_reflns_number_total             5313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02164f2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7040108--7040111.cif.'
_cod_original_formula_sum        'C51 H29 B F24 Fe N3 Pd0.50'
_cod_database_code               7040109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(F1) = Uiso(F1A)
Uiso(F3) = Uiso(F3A)
Uiso(F2) = Uiso(F2A)
Uiso(F2A) = Uiso(F2B)
Uiso(F3A) = Uiso(F3B)
Uiso(F3) = Uiso(F1A)
3. Others
 1*[Sof(F3)+Sof(F3A)+Sof(F2A)+Sof(F2B)+Sof(F3B)+Sof(F0AA)]+1*[Sof(F3)+Sof(F3A)+
 Sof(F2A)+Sof(F2B)+Sof(F3B)+Sof(F0AA)]+1*[Sof(F3)+Sof(F3A)+Sof(F2A)+Sof(F2B)+
 Sof(F3B)+Sof(F0AA)]=1 with esd of 0.01
 1*[Sof(F1)+Sof(F2)+Sof(F1A)]+1*[Sof(F3)+Sof(F3A)+Sof(F2A)+Sof(F2B)+Sof(F3B)+
 Sof(F0AA)]+1*[Sof(F3)+Sof(F3A)+Sof(F2A)+Sof(F2B)+Sof(F3B)+Sof(F0AA)]=1 with
 esd of 0.01
 1*[Sof(F1)+Sof(F2)+Sof(F1A)]+1*[Sof(F3)+Sof(F3A)+Sof(F2A)+Sof(F2B)+Sof(F3B)+
 Sof(F0AA)]=1 with esd of 0.01
 Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=FVAR(1)
 Sof(F2B)=Sof(F3B)=Sof(F0AA)=1-FVAR(2)
 Sof(F3)=Sof(F3A)=Sof(F2A)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C24(H24),
  C27(H27), C29(H29), C32(H32), C35(H35), C38(H38), C41(H41), C44(H44),
 C46(H46), C49(H49), C52(H52)
;
_shelxl_version_number           2013-3