Development of a novel secondary phosphine oxide-ruthenium(ii) catalyst and its application for carbonyl reduction.
Tan, Xuefeng; Zeng, Weijun; Zhang, Xiaoyong; Chung, Lung Wa; Zhang, Xumu; Chemical communications (Cambridge, England) 54 (2018) 535–538; doi:10.1039/c7cc07647a

data_7121001
_publ_section_title
;
 Development of a novel secondary phosphine oxide-ruthenium(ii) catalyst
 and its application for carbonyl reduction.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              535
_journal_page_last               538
_journal_paper_doi               10.1039/c7cc07647a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'C55 H44 O2 P4 Ru, 0.44(C H2 Cl2), 0.78(C4 H10 O), H2 O'
_chemical_formula_sum            'C58.56 H54.68 Cl0.88 O3.78 P4 Ru'
_chemical_formula_weight         1074.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5318)
;
_audit_update_record
;
2017-03-01 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.103(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4387(11)
_cell_length_b                   16.8670(15)
_cell_length_c                   24.294(2)
_cell_measurement_reflns_used    9342
_cell_measurement_temperature    140
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.34
_cell_volume                     5097.0(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            193627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_min         2.199
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1430 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8796.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             2221
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         11791
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+3.6003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10337
_reflns_number_total             11791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07647a2.cif
_cod_data_source_block           cxy0006
_cod_depositor_comments          'Adding full bibliography for 7121001.cif.'
_cod_database_code               7121001
_shelx_shelxl_version_number     2014/7
_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, All O(H,H) groups
2. Restrained distances
 Cl3-C59 = Cl4-C59 = Cl1-C60 = Cl2-C60
 1.79 with sigma of 0.02
 C58-C57 = C56-C55
 1.54 with sigma of 0.02
 Cl2-Cl1 = Cl4-Cl3
 2.92 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl3 \\sim Cl4 \\sim Cl4 \\sim C59 \\sim C59 \\sim C59: within 2.3A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl1 \\sim Cl1 \\sim Cl2 \\sim Cl2 \\sim C60 \\sim C60 \\sim C60: within 2.3A
with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim O3 \\sim O3 \\sim C55 \\sim C55 \\sim C56 \\sim C56 \\sim C56 \\sim
C57 \\sim C57 \\sim C57 \\sim C58 \\sim C58: within 2.3A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(Cl3)=Sof(Cl4)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(Cl1)=Sof(Cl2)=Sof(C60)=
 Sof(H60A)=Sof(H60B)=1-FVAR(1)
 Sof(O3)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(1)
5.a Free rotating group:
 O4(H4A,H4B)
5.b Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C60(H60A,H60B), C56(H56A,H56B), C57(H57A,H57B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54)
5.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C)
;
_olex2_submission_special_instructions 'No special instructions were received'