#------------------------------------------------------------------------------
#$Date: 2019-11-26 02:37:46 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242418 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132431.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4132431
loop_
_publ_author_name
'Zeng, Rong'
'Feller, Moran'
'Diskin-Posner, Yael'
'Shimon, Linda J. W.'
'Ben-David, Yehoshoa'
'Milstein, David'
_publ_section_title
;
 CO Oxidation by N₂O Homogeneously Catalyzed by Ruthenium
 Hydride Pincer Complexes Indicating a New Mechanism.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7061
_journal_page_last               7064
_journal_paper_doi               10.1021/jacs.8b03927
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C21 H27 N2 O2 P Ru'
_chemical_formula_sum            'C21 H27 N2 O2 P Ru'
_chemical_formula_weight         471.48
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.433(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8526(5)
_cell_length_b                   8.5443(4)
_cell_length_c                   27.4092(13)
_cell_measurement_reflns_used    7692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9820
_cell_measurement_theta_min      3.8760
_cell_volume                     2060.16(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            28197
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.396
_diffrn_reflns_theta_min         3.537
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.049
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0333
_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/[σ²(Fo²)+(0.0236P)²+1.4954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5893
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b03927_si_002.cif
_cod_data_source_block           complex16
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132431
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.988
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ru1 Ru 0.36649(2) 0.66053(2) 0.41153(2) 0.01055(4) Uani 1 1 d . .
H H 0.251(3) 0.795(3) 0.4234(9) 0.027(7) Uiso 1 1 d . .
P1 P 0.16621(5) 0.56549(5) 0.35682(2) 0.01003(8) Uani 1 1 d . .
O1 O 0.25559(19) 0.51890(19) 0.50185(5) 0.0270(3) Uani 1 1 d . .
O2 O 0.60953(17) 0.41271(17) 0.39206(6) 0.0232(3) Uani 1 1 d . .
N1 N 0.53949(18) 0.82150(18) 0.43995(6) 0.0143(3) Uani 1 1 d . .
N2 N 0.41282(17) 0.78454(18) 0.34968(5) 0.0125(3) Uani 1 1 d . .
C1 C 0.6016(2) 0.8324(2) 0.48726(7) 0.0184(4) Uani 1 1 d . .
H1 H 0.5703 0.7601 0.5105 0.022 Uiso 1 1 calc R U
C2 C 0.7085(2) 0.9445(2) 0.50324(8) 0.0218(4) Uani 1 1 d . .
H2 H 0.7504 0.9483 0.5367 0.026 Uiso 1 1 calc R U
C3 C 0.7533(2) 1.0507(2) 0.46972(9) 0.0237(4) Uani 1 1 d . .
H3 H 0.8259 1.1293 0.4799 0.028 Uiso 1 1 calc R U
C4 C 0.6911(2) 1.0412(2) 0.42124(8) 0.0198(4) Uani 1 1 d . .
H4 H 0.7203 1.1142 0.3979 0.024 Uiso 1 1 calc R U
C5 C 0.5850(2) 0.9238(2) 0.40656(7) 0.0150(3) Uani 1 1 d . .
C6 C 0.5184(2) 0.9003(2) 0.35521(7) 0.0144(3) Uani 1 1 d . .
C7 C 0.5612(2) 0.9840(2) 0.31597(7) 0.0194(4) Uani 1 1 d . .
H7 H 0.6354 1.0646 0.3205 0.023 Uiso 1 1 calc R U
C8 C 0.4905(2) 0.9454(2) 0.26865(8) 0.0213(4) Uani 1 1 d . .
H8 H 0.5181 0.9999 0.2408 0.026 Uiso 1 1 calc R U
C9 C 0.3830(2) 0.8303(2) 0.26271(7) 0.0178(4) Uani 1 1 d . .
H9 H 0.3366 0.8061 0.2307 0.021 Uiso 1 1 calc R U
C10 C 0.3386(2) 0.7449(2) 0.30402(6) 0.0127(3) Uani 1 1 d . .
C11 C 0.2293(2) 0.6274(2) 0.30107(6) 0.0133(3) Uani 1 1 d . .
H11 H 0.1905 0.5825 0.2705 0.016 Uiso 1 1 calc R U
C12 C -0.0208(2) 0.6722(2) 0.36126(6) 0.0129(3) Uani 1 1 d . .
C13 C -0.1522(2) 0.6104(2) 0.32472(7) 0.0166(3) Uani 1 1 d . .
H13A H -0.1207 0.6096 0.2916 0.025 Uiso 1 1 calc R U
H13B H -0.2410 0.6785 0.3254 0.025 Uiso 1 1 calc R U
H13C H -0.1784 0.5039 0.3340 0.025 Uiso 1 1 calc R U
C14 C 0.0037(2) 0.8445(2) 0.34773(7) 0.0165(3) Uani 1 1 d . .
H14A H 0.0887 0.8878 0.3696 0.025 Uiso 1 1 calc R U
H14B H -0.0888 0.9044 0.3513 0.025 Uiso 1 1 calc R U
H14C H 0.0269 0.8509 0.3137 0.025 Uiso 1 1 calc R U
C15 C -0.0664(2) 0.6669(2) 0.41381(7) 0.0170(3) Uani 1 1 d . .
H15A H -0.0781 0.5577 0.4237 0.025 Uiso 1 1 calc R U
H15B H -0.1629 0.7224 0.4148 0.025 Uiso 1 1 calc R U
H15C H 0.0128 0.7172 0.4364 0.025 Uiso 1 1 calc R U
C16 C 0.1274(2) 0.3480(2) 0.35196(7) 0.0144(3) Uani 1 1 d . .
C17 C 0.0532(2) 0.3016(2) 0.30035(7) 0.0205(4) Uani 1 1 d . .
H17A H -0.0438 0.3568 0.2932 0.031 Uiso 1 1 calc R U
H17B H 0.0352 0.1884 0.2992 0.031 Uiso 1 1 calc R U
H17C H 0.1210 0.3301 0.2759 0.031 Uiso 1 1 calc R U
C18 C 0.0293(2) 0.2921(2) 0.39154(7) 0.0178(4) Uani 1 1 d . .
H18A H 0.0753 0.3270 0.4239 0.027 Uiso 1 1 calc R U
H18B H 0.0234 0.1776 0.3910 0.027 Uiso 1 1 calc R U
H18C H -0.0731 0.3361 0.3849 0.027 Uiso 1 1 calc R U
C19 C 0.2794(2) 0.2595(2) 0.35979(7) 0.0182(4) Uani 1 1 d . .
H19A H 0.3474 0.2987 0.3367 0.027 Uiso 1 1 calc R U
H19B H 0.2613 0.1475 0.3542 0.027 Uiso 1 1 calc R U
H19C H 0.3264 0.2760 0.3935 0.027 Uiso 1 1 calc R U
C20 C 0.3026(2) 0.5698(2) 0.46772(7) 0.0160(3) Uani 1 1 d . .
C21 C 0.5175(2) 0.5010(2) 0.39849(7) 0.0146(3) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C20 Ru1 C21 97.86(8)
C20 Ru1 N2 171.81(7)
C21 Ru1 N2 90.27(7)
C20 Ru1 N1 103.73(7)
C21 Ru1 N1 92.19(7)
N2 Ru1 N1 76.74(6)
C20 Ru1 P1 96.13(6)
C21 Ru1 P1 97.16(5)
N2 Ru1 P1 81.87(4)
N1 Ru1 P1 156.67(4)
C20 Ru1 H 82.6(9)
C21 Ru1 H 177.0(10)
N2 Ru1 H 89.4(9)
N1 Ru1 H 84.9(10)
P1 Ru1 H 85.7(9)
C11 P1 C16 107.81(8)
C11 P1 C12 105.86(8)
C16 P1 C12 108.78(8)
C11 P1 Ru1 99.23(6)
C16 P1 Ru1 120.37(6)
C12 P1 Ru1 113.27(6)
C1 N1 C5 118.79(16)
C1 N1 Ru1 126.18(13)
C5 N1 Ru1 115.00(12)
C6 N2 C10 121.92(15)
C6 N2 Ru1 118.45(12)
C10 N2 Ru1 119.61(12)
N1 C1 C2 122.76(19)
N1 C1 H1 118.6
C2 C1 H1 118.6
C3 C2 C1 118.81(19)
C3 C2 H2 120.6
C1 C2 H2 120.6
C2 C3 C4 119.23(19)
C2 C3 H3 120.4
C4 C3 H3 120.4
C3 C4 C5 119.93(19)
C3 C4 H4 120.0
C5 C4 H4 120.0
N1 C5 C4 120.45(18)
N1 C5 C6 115.94(16)
C4 C5 C6 123.59(18)
N2 C6 C7 122.43(18)
N2 C6 C5 113.68(16)
C7 C6 C5 123.87(17)
C6 C7 C8 117.51(18)
C6 C7 H7 121.2
C8 C7 H7 121.2
C9 C8 C7 120.56(18)
C9 C8 H8 119.7
C7 C8 H8 119.7
C8 C9 C10 121.30(18)
C8 C9 H9 119.4
C10 C9 H9 119.3
N2 C10 C11 118.98(15)
N2 C10 C9 116.26(16)
C11 C10 C9 124.76(17)
C10 C11 P1 116.84(13)
C10 C11 H11 121.6
P1 C11 H11 121.6
C15 C12 C14 108.20(15)
C15 C12 C13 109.90(15)
C14 C12 C13 106.72(15)
C15 C12 P1 111.49(12)
C14 C12 P1 107.15(12)
C13 C12 P1 113.11(12)
C12 C13 H13A 109.5
C12 C13 H13B 109.5
H13A C13 H13B 109.5
C12 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C12 C14 H14A 109.5
C12 C14 H14B 109.5
H14A C14 H14B 109.5
C12 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
C12 C15 H15A 109.5
C12 C15 H15B 109.5
H15A C15 H15B 109.5
C12 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
C19 C16 C18 107.62(15)
C19 C16 C17 106.12(15)
C18 C16 C17 110.51(16)
C19 C16 P1 108.91(12)
C18 C16 P1 111.57(13)
C17 C16 P1 111.86(13)
C16 C17 H17A 109.5
C16 C17 H17B 109.5
H17A C17 H17B 109.5
C16 C17 H17C 109.5
H17A C17 H17C 109.5
H17B C17 H17C 109.5
C16 C18 H18A 109.5
C16 C18 H18B 109.5
H18A C18 H18B 109.5
C16 C18 H18C 109.5
H18A C18 H18C 109.5
H18B C18 H18C 109.5
C16 C19 H19A 109.5
C16 C19 H19B 109.5
H19A C19 H19B 109.5
C16 C19 H19C 109.5
H19A C19 H19C 109.5
H19B C19 H19C 109.5
O1 C20 Ru1 176.02(18)
O2 C21 Ru1 177.01(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru1 C20 1.8677(19)
Ru1 C21 1.9697(19)
Ru1 N2 2.0787(15)
Ru1 N1 2.1392(16)
Ru1 P1 2.3358(5)
Ru1 H 1.59(3)
P1 C11 1.7661(18)
P1 C16 1.8915(19)
P1 C12 1.9061(18)
O1 C20 1.151(2)
O2 C21 1.139(2)
N1 C1 1.354(2)
N1 C5 1.359(2)
N2 C6 1.358(2)
N2 C10 1.389(2)
C1 C2 1.383(3)
C1 H1 0.9500
C2 C3 1.380(3)
C2 H2 0.9500
C3 C4 1.383(3)
C3 H3 0.9500
C4 C5 1.402(3)
C4 H4 0.9500
C5 C6 1.477(3)
C6 C7 1.380(3)
C7 C8 1.414(3)
C7 H7 0.9500
C8 C9 1.366(3)
C8 H8 0.9500
C9 C10 1.438(2)
C9 H9 0.9500
C10 C11 1.390(3)
C11 H11 0.9500
C12 C15 1.539(2)
C12 C14 1.539(3)
C12 C13 1.540(3)
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C14 H14A 0.9800
C14 H14B 0.9800
C14 H14C 0.9800
C15 H15A 0.9800
C15 H15B 0.9800
C15 H15C 0.9800
C16 C19 1.537(3)
C16 C18 1.540(3)
C16 C17 1.543(3)
C17 H17A 0.9800
C17 H17B 0.9800
C17 H17C 0.9800
C18 H18A 0.9800
C18 H18B 0.9800
C18 H18C 0.9800
C19 H19A 0.9800
C19 H19B 0.9800
C19 H19C 0.9800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N1 C1 C2 0.7(3)
Ru1 N1 C1 C2 -177.06(15)
N1 C1 C2 C3 0.5(3)
C1 C2 C3 C4 -0.5(3)
C2 C3 C4 C5 -0.6(3)
C1 N1 C5 C4 -1.8(3)
Ru1 N1 C5 C4 176.15(14)
C1 N1 C5 C6 177.08(16)
Ru1 N1 C5 C6 -4.9(2)
C3 C4 C5 N1 1.8(3)
C3 C4 C5 C6 -176.99(18)
C10 N2 C6 C7 -1.3(3)
Ru1 N2 C6 C7 177.11(14)
C10 N2 C6 C5 -179.58(15)
Ru1 N2 C6 C5 -1.2(2)
N1 C5 C6 N2 4.1(2)
C4 C5 C6 N2 -177.06(17)
N1 C5 C6 C7 -174.20(18)
C4 C5 C6 C7 4.7(3)
N2 C6 C7 C8 0.0(3)
C5 C6 C7 C8 178.15(18)
C6 C7 C8 C9 0.7(3)
C7 C8 C9 C10 -0.2(3)
C6 N2 C10 C11 -178.65(17)
Ru1 N2 C10 C11 3.0(2)
C6 N2 C10 C9 1.7(2)
Ru1 N2 C10 C9 -176.65(12)
C8 C9 C10 N2 -1.0(3)
C8 C9 C10 C11 179.39(19)
N2 C10 C11 P1 12.6(2)
C9 C10 C11 P1 -167.87(15)
C16 P1 C11 C10 -144.91(14)
C12 P1 C11 C10 98.80(15)
Ru1 P1 C11 C10 -18.74(15)
C11 P1 C16 C19 77.96(14)
C12 P1 C16 C19 -167.67(12)
Ru1 P1 C16 C19 -34.59(14)
C11 P1 C16 C18 -163.39(13)
C12 P1 C16 C18 -49.02(15)
Ru1 P1 C16 C18 84.06(13)
C11 P1 C16 C17 -39.01(16)
C12 P1 C16 C17 75.35(15)
Ru1 P1 C16 C17 -151.56(11)
