Bidentate Ru(ii)-NC complexes as catalysts for the dehydrogenative reaction from primary alcohols to carboxylic acids.
Gong, Dawei; Hu, Bowen; Chen, Dafa; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8826–8834; doi:10.1039/c9dt01414d

data_7700029
_publ_section_title
;
 Bidentate Ru(ii)-NC complexes as catalysts for the dehydrogenative
 reaction from primary alcohols to carboxylic acids.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8826
_journal_page_last               8834
_journal_paper_doi               10.1039/c9dt01414d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C55 H43 N O3 P2 Ru), C7 H8'
_chemical_formula_sum            'C117 H94 N2 O6 P4 Ru2'
_chemical_formula_weight         1949.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-14 deposited with the CCDC.    2019-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.064(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7587(2)
_cell_length_b                   43.2244(8)
_cell_length_c                   19.8552(3)
_cell_measurement_reflns_used    12440
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.0640
_cell_measurement_theta_min      3.1710
_cell_volume                     9231.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      5.00  87.20   0.30   25.00    --   18.47  77.00 120.00  274
  2  \w      5.00  57.20   0.30   25.00    --   18.47 -99.00  60.00  174
  3  \w      0.00  29.10   0.30   25.00    --   18.47  57.00   0.00   97
  4  \w     14.00  38.90   0.30   25.00    --   18.47 -57.00 -90.00   83
  5  \w    -50.00  11.20   0.30   25.00    --   18.47 -57.00  60.00  204
  6  \w     25.00  87.10   0.30   25.00    --   18.47  57.00-150.00  207
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0115365000
_diffrn_orient_matrix_UB_12      0.0156770000
_diffrn_orient_matrix_UB_13      0.0083781000
_diffrn_orient_matrix_UB_21      -0.0012580000
_diffrn_orient_matrix_UB_22      0.0038977000
_diffrn_orient_matrix_UB_23      -0.0347005000
_diffrn_orient_matrix_UB_31      -0.0649201000
_diffrn_orient_matrix_UB_32      -0.0028743000
_diffrn_orient_matrix_UB_33      -0.0015000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58791
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.052
_diffrn_reflns_theta_min         2.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.55(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2350
_refine_ls_number_reflns         29481
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                24077
_reflns_number_total             29481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01414d2.cif
_cod_data_source_block           p181126d2
_cod_depositor_comments
'Adding full bibliography for 7700028--7700029.cif.'
_cod_database_code               7700029
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P Ru'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.906
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.45(2)
 0.55(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C228) \\sim Ueq, Uanis(C229) \\sim Ueq, Uanis(C234) \\sim Ueq,
Uanis(C230) \\sim Ueq, Uanis(C231) \\sim Ueq, Uanis(C232) \\sim Ueq,
Uanis(C233) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C223) \\sim Ueq, Uanis(C224) \\sim Ueq, Uanis(C225) \\sim Ueq,
Uanis(C226) \\sim Ueq, Uanis(C227) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C120(H120), C118(H118), C142(H142), C131(H131), C114(H114), C155(H155),
 C115(H115), C126(H126), C130(H130), C125(H125), C119(H119), C156(H156),
 C148(H148), C157(H157), C150(H150), C140(H140), C116(H116), C113(H113),
 C124(H124), C127(H127), C144(H144), C121(H121), C162(H162), C128(H128),
 C143(H143), C136(H136), C149(H149), C154(H154), C151(H151), C132(H132),
 C145(H145), C139(H139), C163(H163), C146(H146), C122(H122), C134(H134),
 C161(H161), C137(H137), C138(H138), C165(H165), C112(H112), C133(H133),
 C164(H164), C12(H12), C34(H34), C17(H17), C32(H32), C21(H21), C26(H26),
 C35(H35), C37(H37), C15(H15), C16(H16), C30(H30), C18(H18), C10(H10), C11(H11),
  C6(H6), C20(H20), C14(H14), C8(H8), C4(H4), C2(H2), C43(H43), C9(H9), C5(H5),
 C36(H36), C24(H24), C38(H38), C46(H46), C44(H44), C27(H27), C29(H29), C23(H23),
  C51(H51), C55(H55), C45(H45), C22(H22), C33(H33), C39(H39), C52(H52), C3(H3),
 C53(H53), C28(H28), C40(H40), C54(H54), C173(H173), C194(H194), C204(H204),
 C197(H197), C174(H174), C200(H200), C192(H192), C216(H216), C199(H199),
 C168(H168), C195(H195), C188(H188), C206(H206), C220(H220), C201(H201),
 C175(H175), C198(H198), C209(H209), C179(H179), C183(H183), C211(H211),
 C182(H182), C191(H191), C203(H203), C217(H217), C171(H171), C189(H189),
 C205(H205), C185(H185), C176(H176), C219(H219), C177(H177), C167(H167),
 C180(H180), C187(H187), C193(H193), C212(H212), C170(H170), C186(H186),
 C181(H181), C169(H169), C218(H218), C210(H210), C60(H60), C79(H79), C83(H83),
 C91(H91), C94(H94), C75(H75), C95(H95), C87(H87), C78(H78), C99(H99), C76(H76),
  C82(H82), C98(H98), C81(H81), C65(H65), C77(H77), C110(H110), C93(H93),
 C101(H101), C92(H92), C59(H59), C73(H73), C57(H57), C106(H106), C67(H67),
 C61(H61), C88(H88), C72(H72), C63(H63), C58(H58), C66(H66), C85(H85), C69(H69),
  C71(H71), C90(H90), C84(H84), C89(H89), C64(H64), C108(H108), C70(H70),
 C107(H107), C100(H100), C109(H109), C223(H223), C225(H225), C224(H224),
 C226(H226), C227(H227), C234(H234), C233(H233), C232(H232), C231(H231),
 C230(H230)
4.b Fitted hexagon refined as free rotating group:
 C229(C234,C233,C232,C231,C230)
4.c Idealised Me refined as rotating group:
 C221(H22A,H22B,H22C), C228(H22D,H22E,H22F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.766