Catalytic Oxidative Deamination by Water with H<sub>2</sub> Liberation.
Tang, Shan; Rauch, Michael; Montag, Michael; Diskin-Posner, Yael; Ben-David, Yehoshoa; Milstein, David; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c10826

data_4135379
_publ_section_title
;
 Catalytic Oxidative Deamination by Water with H<sub>2</sub> Liberation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c10826
_journal_year                    2020
_chemical_formula_moiety         '2(C35 H45 N O3 P2 Ru), C5 H12'
_chemical_formula_sum            'C75 H102 N2 O6 P4 Ru2'
_chemical_formula_weight         1453.60
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.3220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7295(3)
_cell_length_b                   11.20140(10)
_cell_length_c                   25.9806(3)
_cell_measurement_reflns_used    25283
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.4430
_cell_measurement_theta_min      3.5960
_cell_volume                     7066.02(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -30.00  88.00   0.40   15.00    --    0.00  57.00 -90.00  295
  2  \w    -89.00  29.00   0.40   15.00    --    0.00 -57.00   0.00  295
  3  \w    -30.00  88.00   0.40   15.00    --    0.00  57.00 150.00  295
  4  \w      1.00 127.00   0.40   80.00    --   90.00 -82.00 -60.00  315
  5  \w     54.00 179.20   0.40   80.00    --   90.00  80.00 107.39  313
  6  \w     53.00 126.20   0.40   80.00    --   90.00 -82.00   0.00  183
  7  \w    116.00 150.00   0.40   80.00    --   90.00  77.00 150.00   85
  8  \w     47.00 115.00   0.40   80.00    --   90.00 -82.00 -90.00  170
  9  \w      1.00 120.20   0.40   80.00    --   90.00 -82.00 -30.00  298
 10  \w     83.00 134.20   0.40   80.00    --   90.00  82.00  90.00  128
 11  \w     94.00 120.00   0.40   80.00    --   90.00 -82.00-120.00   65
 12  \w     53.00 179.00   0.40   80.00    --   90.00  82.00-180.00  315
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0148676000
_diffrn_orient_matrix_UB_12      0.1337548000
_diffrn_orient_matrix_UB_13      0.0038579000
_diffrn_orient_matrix_UB_21      -0.0604265000
_diffrn_orient_matrix_UB_22      0.0319874000
_diffrn_orient_matrix_UB_23      -0.0082266000
_diffrn_orient_matrix_UB_31      0.0123919000
_diffrn_orient_matrix_UB_32      -0.0040201000
_diffrn_orient_matrix_UB_33      0.0621836000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52331
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        65.087
_diffrn_reflns_theta_max         65.087
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.727
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         12024
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0420P)^2^+4.9152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10396
_reflns_number_total             12024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c10826_si_002.cif
_cod_data_source_block           mm2258a
_cod_database_code               4135379
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C35H60N1O3P2Ru1
_chemical_oxdiff_usercomment     'Miki mm260720-2'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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. Rigid body (RIGU) restrains
 C74, C71, H73D, C75, C72, C73, H73C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(H60A)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C72A)=Sof(H72A)=
 Sof(H72B)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(C75A)=Sof(H75A)=Sof(H75B)=
 Sof(H75C)=Sof(C73A)=Sof(H73A)=Sof(H73B)=Sof(C71A)=Sof(H71A)=Sof(H71B)=
 Sof(H71C)=1-FVAR(1)
 Sof(H60)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C74)=Sof(H74C)=Sof(H74D)=
 Sof(C75)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C73)=Sof(H73C)=Sof(H73D)=Sof(C71)=
 Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C72)=Sof(H72C)=Sof(H72D)=FVAR(1)
 Sof(H57A)=Sof(C59)=Sof(H59D)=Sof(H59E)=Sof(H59F)=1-FVAR(2)
 Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(H57)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C22(H22), C25(H25), C51(H51), C54(H54), C57(H57),
 C57(H57A), C60(H60), C60(H60A)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C36(H36A,H36B), C43(H43A,H43B),
 C50(H50A,H50B), C72A(H72A,H72B), C74(H74C,H74D), C74A(H74A,H74B), C73A(H73A,
 H73B), C73(H73C,H73D), C72(H72C,H72D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47),
  C48(H48), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C59A(H59A,H59B,H59C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C59(H59D,H59E,
 H59F), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C62A(H62D,H62E,H62F),
 C75(H75D,H75E,H75F), C75A(H75A,H75B,H75C), C71A(H71A,H71B,H71C), C71(H71D,H71E,
 H71F)
;
_shelx_res_checksum              67737
_shelx_hkl_checksum              48238
_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 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.797