#------------------------------------------------------------------------------
#$Date: 2019-07-01 12:23:26 +0300 (Mon, 01 Jul 2019) $
#$Revision: 216655 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/19/1551926.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_1551926
loop_
_publ_author_name
'Tianfei Liu'
'Meiyuan Guo'
'Andreas Orthaber'
'Reiner Lomoth'
'Marcus Lundberg'
'Sascha Ott'
'Leif Hammarstrom'
_publ_section_title
;
 Accelerating proton-coupled electron transfer of metal hydrides in
 catalyst model reactions
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              881
_journal_page_last               887
_journal_paper_doi               10.1038/s41557-018-0076-x
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C15 H13 N O4 W'
_chemical_formula_sum            'C15 H13 N O4 W'
_chemical_formula_weight         455.11
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                103.6060(10)
_cell_angle_beta                 98.720(2)
_cell_angle_gamma                108.7760(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2435(3)
_cell_length_b                   8.3778(2)
_cell_length_c                   11.8392(4)
_cell_measurement_reflns_used    3616
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.8
_cell_volume                     729.09(4)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2012)'
_computing_data_collection       'APEX2  (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2012)'
_computing_molecular_graphics    ' ORTEP for Windows (Farugia, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  ' Bruker D8 with APEX-II CCD'
_diffrn_radiation_monochromator  graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15149
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.826
_exptl_absorpt_coefficient_mu    7.936
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.608
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0220
_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)+(0.0218P)²+0.8013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0520
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3616
_reflns_number_total             3867
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            41557_2018_76_MOESM48_ESM.cif
_cod_data_source_block           shelx-3
_cod_database_code               1551926
_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.
;
_exptl_absorpt_special_details
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was 
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W001 W 0.21870(2) 0.38556(2) 0.63933(2) 0.02285(5) Uani 1 1 d . . . . .
O4 O 1.2288(3) 0.7824(3) 1.0412(2) 0.0273(5) Uani 1 1 d . . . . .
N003 N 0.7169(3) 0.7651(3) 1.0173(2) 0.0212(5) Uani 1 1 d . . . . .
O2 O 0.0704(4) 0.2289(4) 0.3616(2) 0.0433(7) Uani 1 1 d . . . . .
C1 C 0.4872(4) 0.5599(4) 0.7792(3) 0.0194(6) Uani 1 1 d . . . . .
O1 O 0.2967(5) 0.0410(4) 0.6079(4) 0.0672(11) Uani 1 1 d . . . . .
C14 C 0.1254(4) 0.2879(5) 0.4635(3) 0.0274(7) Uani 1 1 d . . . . .
C6 C 0.6021(4) 0.4936(4) 0.8505(3) 0.0231(6) Uani 1 1 d . . . . .
H6A H 0.6474 0.4196 0.7955 0.028 Uiso 1 1 calc R U . . .
H6B H 0.5306 0.4183 0.8920 0.028 Uiso 1 1 calc R U . . .
C10 C 1.0276(4) 0.9117(4) 1.1170(3) 0.0199(6) Uani 1 1 d . . . . .
H10 H 1.1180 1.0064 1.1789 0.024 Uiso 1 1 calc R U . . .
C7 C 0.7569(4) 0.6437(4) 0.9425(3) 0.0193(6) Uani 1 1 d . . . . .
C11 C 0.8523(4) 0.8943(4) 1.1011(3) 0.0214(6) Uani 1 1 d . . . . .
H11 H 0.8261 0.9816 1.1542 0.026 Uiso 1 1 calc R U . . .
C9 C 1.0659(4) 0.7855(4) 1.0390(3) 0.0192(6) Uani 1 1 d . . . . .
C8 C 0.9278(4) 0.6495(4) 0.9499(3) 0.0203(6) Uani 1 1 d . . . . .
H8 H 0.9508 0.5618 0.8948 0.024 Uiso 1 1 calc R U . . .
C5 C 0.3563(5) 0.6191(5) 0.8167(3) 0.0324(8) Uani 1 1 d . . . . .
H5 H 0.3183 0.6132 0.8879 0.039 Uiso 1 1 calc R U . . .
C12 C 1.3765(4) 0.9261(4) 1.1266(3) 0.0303(7) Uani 1 1 d . . . . .
H12A H 1.3784 1.0382 1.1141 0.045 Uiso 1 1 calc R U . . .
H12C H 1.4866 0.9104 1.1159 0.045 Uiso 1 1 calc R U . . .
H12B H 1.3653 0.9278 1.2081 0.045 Uiso 1 1 calc R U . . .
C13 C 0.2643(5) 0.1648(5) 0.6165(4) 0.0412(10) Uani 1 1 d . . . . .
C2 C 0.5014(5) 0.5934(5) 0.6678(3) 0.0356(9) Uani 1 1 d . . . . .
H2 H 0.5792 0.5673 0.6213 0.043 Uiso 1 1 calc R U . . .
C3 C 0.3799(7) 0.6720(5) 0.6389(4) 0.0557(15) Uani 1 1 d . . . . .
H3 H 0.3610 0.7077 0.5692 0.067 Uiso 1 1 calc R U . . .
O3 O -0.1808(4) 0.2906(5) 0.6348(3) 0.0565(9) Uani 1 1 d . . . . .
C4 C 0.2920(7) 0.6883(5) 0.7301(5) 0.0593(16) Uani 1 1 d . . . . .
H4 H 0.2035 0.7379 0.7333 0.071 Uiso 1 1 calc R U . . .
C15 C -0.0355(5) 0.3210(5) 0.6326(3) 0.0353(8) Uani 1 1 d . . . . .
H H 0.133(7) 0.274(7) 0.720(5) 0.058(15) Uiso 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'
W W -0.8490 6.8722 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C13 W001 C14 81.75(16) . .
C13 W001 C15 106.43(18) . .
C14 W001 C15 81.36(14) . .
C13 W001 C1 94.59(13) . .
C14 W001 C1 138.93(13) . .
C15 W001 C1 137.62(13) . .
C13 W001 C2 101.61(17) . .
C14 W001 C2 104.85(13) . .
C15 W001 C2 151.90(17) . .
C1 W001 C2 35.56(11) . .
C13 W001 C5 120.88(15) . .
C14 W001 C5 152.75(15) . .
C15 W001 C5 103.86(14) . .
C1 W001 C5 35.22(12) . .
C2 W001 C5 58.57(14) . .
C13 W001 C3 134.5(2) . .
C14 W001 C3 95.44(16) . .
C15 W001 C3 118.07(19) . .
C1 W001 C3 58.69(12) . .
C2 W001 C3 35.05(17) . .
C5 W001 C3 58.24(16) . .
C13 W001 C4 152.99(15) . .
C14 W001 C4 118.73(18) . .
C15 W001 C4 94.65(18) . .
C1 W001 C4 58.44(13) . .
C2 W001 C4 58.07(18) . .
C5 W001 C4 35.05(15) . .
C3 W001 C4 34.6(2) . .
C13 W001 H 68.0(19) . .
C14 W001 H 118.4(19) . .
C15 W001 H 59.8(19) . .
C1 W001 H 97.2(19) . .
C2 W001 H 132.3(19) . .
C5 W001 H 86.2(19) . .
C3 W001 H 143.7(19) . .
C4 W001 H 110.8(19) . .
C9 O4 C12 118.0(3) . .
C11 N003 C7 116.4(3) . .
C5 C1 C2 107.2(3) . .
C5 C1 C6 125.8(3) . .
C2 C1 C6 126.8(3) . .
C5 C1 W001 72.36(17) . .
C2 C1 W001 72.28(19) . .
C6 C1 W001 125.8(2) . .
O2 C14 W001 179.1(4) . .
C1 C6 C7 111.9(2) . .
C1 C6 H6A 109.2 . .
C7 C6 H6A 109.2 . .
C1 C6 H6B 109.2 . .
C7 C6 H6B 109.2 . .
H6A C6 H6B 107.9 . .
C9 C10 C11 117.3(3) . .
C9 C10 H10 121.4 . .
C11 C10 H10 121.4 . .
N003 C7 C8 122.9(3) . .
N003 C7 C6 116.2(3) . .
C8 C7 C6 120.9(3) . .
N003 C11 C10 125.4(3) . .
N003 C11 H11 117.3 . .
C10 C11 H11 117.3 . .
O4 C9 C10 125.2(3) . .
O4 C9 C8 116.0(3) . .
C10 C9 C8 118.8(3) . .
C7 C8 C9 119.2(3) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C4 C5 C1 108.1(4) . .
C4 C5 W001 72.9(2) . .
C1 C5 W001 72.42(18) . .
C4 C5 H5 125.9 . .
C1 C5 H5 125.9 . .
W001 C5 H5 120.5 . .
O4 C12 H12A 109.5 . .
O4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
O4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
H12C C12 H12B 109.5 . .
O1 C13 W001 176.8(4) . .
C3 C2 C1 107.9(4) . .
C3 C2 W001 72.7(2) . .
C1 C2 W001 72.15(19) . .
C3 C2 H2 126.1 . .
C1 C2 H2 126.1 . .
W001 C2 H2 120.9 . .
C4 C3 C2 108.3(4) . .
C4 C3 W001 72.8(2) . .
C2 C3 W001 72.2(2) . .
C4 C3 H3 125.9 . .
C2 C3 H3 125.9 . .
W001 C3 H3 120.9 . .
C3 C4 C5 108.6(4) . .
C3 C4 W001 72.6(2) . .
C5 C4 W001 72.1(2) . .
C3 C4 H4 125.7 . .
C5 C4 H4 125.7 . .
W001 C4 H4 121.3 . .
O3 C15 W001 176.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W001 C13 1.969(4) .
W001 C14 1.975(3) .
W001 C15 1.972(4) .
W001 C1 2.333(3) .
W001 C2 2.335(4) .
W001 C5 2.332(3) .
W001 C3 2.341(4) .
W001 C4 2.343(4) .
W001 H 1.57(5) .
O4 C9 1.348(4) .
O4 C12 1.437(4) .
N003 C11 1.335(4) .
N003 C7 1.345(4) .
O2 C14 1.147(4) .
C1 C5 1.411(5) .
C1 C2 1.426(5) .
C1 C6 1.496(4) .
O1 C13 1.138(5) .
C6 C7 1.515(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C10 C9 1.383(4) .
C10 C11 1.384(4) .
C10 H10 0.9500 .
C7 C8 1.383(4) .
C11 H11 0.9500 .
C9 C8 1.394(4) .
C8 H8 0.9500 .
C5 C4 1.408(6) .
C5 H5 0.9500 .
C12 H12A 0.9800 .
C12 H12C 0.9800 .
C12 H12B 0.9800 .
C2 C3 1.408(7) .
C2 H2 0.9500 .
C3 C4 1.393(8) .
C3 H3 0.9500 .
O3 C15 1.147(5) .
C4 H4 0.9500 .
