#------------------------------------------------------------------------------
#$Date: 2019-07-01 12:22:59 +0300 (Mon, 01 Jul 2019) $
#$Revision: 216653 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/19/1551924.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_1551924
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 H10 F3 N O3 W'
_chemical_formula_sum            'C15 H10 F3 N O3 W'
_chemical_formula_weight         493.09
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_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
_cell_angle_alpha                90
_cell_angle_beta                 90.639(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0122(15)
_cell_length_b                   9.8352(7)
_cell_length_c                   7.4416(6)
_cell_measurement_reflns_used    3304
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.0
_cell_volume                     1464.59(19)
_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 1.000
_diffrn_measured_fraction_theta_max 0.978
_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  0.0664
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21956
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         2.035
_exptl_absorpt_coefficient_mu    7.934
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.793
_refine_diff_density_min         -4.540
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0720
_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/[σ²(Fo²)+(0.0803P)²+46.7655P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1859
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3304
_reflns_number_total             3879
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            41557_2018_76_MOESM46_ESM.cif
_cod_data_source_block           shelx-1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1551924
_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+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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.9098(8) 0.4996(18) 0.387(3) 0.029(4) Uani 1 1 d . . . . .
C12 C 0.9498(9) 0.4975(18) 0.220(3) 0.038(5) Uani 1 1 d . . . . .
F2 F 0.9767(7) 0.6175(13) 0.183(2) 0.059(4) Uani 1 1 d . . . . .
F3 F 0.9135(5) 0.4564(14) 0.0817(19) 0.052(3) Uani 1 1 d . . . . .
H H 0.676(15) 0.30(4) 0.62(5) 0.12(13) Uiso 1 1 d . . . . .
C1 C 0.7158(8) 0.5647(16) 0.802(2) 0.025(3) Uani 1 1 d . . . . .
C13 C 0.7095(9) 0.4359(19) 0.383(2) 0.029(4) Uani 1 1 d . . . . .
C2 C 0.6898(10) 0.6694(17) 0.691(2) 0.032(4) Uani 1 1 d . . . . .
H2 H 0.7156 0.7264 0.6156 0.038 Uiso 1 1 calc R U . . .
C14 C 0.5890(8) 0.5099(15) 0.369(2) 0.023(3) Uani 1 1 d . . . . .
C3 C 0.6204(11) 0.6762(18) 0.710(3) 0.040(5) Uani 1 1 d . . . . .
H3 H 0.5916 0.7399 0.6526 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5832(8) 0.3130(15) 0.572(3) 0.029(3) Uani 1 1 d . . . . .
C4 C 0.6000(9) 0.571(2) 0.831(3) 0.044(6) Uani 1 1 d . . . . .
H4 H 0.5555 0.5521 0.8668 0.053 Uiso 1 1 calc R U . . .
C5 C 0.6588(8) 0.4993(16) 0.889(2) 0.025(3) Uiso 1 1 d . . . . .
H5 H 0.6606 0.4239 0.9688 0.030 Uiso 1 1 calc R U . . .
C6 C 0.7859(10) 0.5289(19) 0.839(3) 0.038(4) Uani 1 1 d . . . . .
H6A H 0.7865 0.4412 0.9039 0.046 Uiso 1 1 calc R U . . .
H6B H 0.8048 0.5984 0.9208 0.046 Uiso 1 1 calc R U . . .
C7 C 0.8321(8) 0.5162(17) 0.680(3) 0.028(4) Uani 1 1 d . . . . .
C8 C 0.8580(9) 0.3906(17) 0.635(3) 0.035(4) Uani 1 1 d . . . . .
H8 H 0.8487 0.3123 0.7051 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8978(9) 0.3830(17) 0.485(3) 0.032(4) Uani 1 1 d . . . . .
H9 H 0.9167 0.2987 0.4492 0.039 Uiso 1 1 calc R U . . .
C11 C 0.8815(9) 0.6214(16) 0.447(3) 0.034(4) Uani 1 1 d . . . . .
H11 H 0.8914 0.7023 0.3834 0.040 Uiso 1 1 calc R U . . .
N1 N 0.8421(7) 0.6306(14) 0.587(3) 0.036(3) Uani 1 1 d . . . . .
O1 O 0.7489(7) 0.418(2) 0.273(2) 0.053(4) Uani 1 1 d . . . . .
O2 O 0.5546(6) 0.5370(12) 0.250(2) 0.036(3) Uani 1 1 d . . . . .
O3 O 0.5458(7) 0.2253(12) 0.566(2) 0.047(3) Uani 1 1 d . . . . .
W1 W 0.64632(3) 0.46627(4) 0.57871(10) 0.01987(17) Uani 1 1 d . . . . .
F1 F 1.0007(6) 0.4101(14) 0.2352(19) 0.050(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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C9 C10 C11 118.0(17) . .
C9 C10 C12 121.7(16) . .
C11 C10 C12 120.2(17) . .
F3 C12 F2 109(2) . .
F3 C12 F1 106.4(14) . .
F2 C12 F1 106.2(15) . .
F3 C12 C10 111.1(14) . .
F2 C12 C10 112.6(14) . .
F1 C12 C10 110.9(19) . .
C2 C1 C6 128.8(16) . .
C2 C1 C5 107.2(14) . .
C6 C1 C5 123.9(15) . .
C2 C1 W1 71.3(10) . .
C6 C1 W1 125.9(13) . .
C5 C1 W1 71.2(9) . .
O1 C13 W1 177.1(16) . .
C3 C2 C1 109.5(17) . .
C3 C2 W1 73.1(11) . .
C1 C2 W1 73.6(10) . .
O2 C14 W1 178.3(15) . .
C2 C3 C4 108.7(17) . .
C2 C3 W1 72.0(10) . .
C4 C3 W1 72.1(10) . .
O3 C15 W1 178.8(16) . .
C3 C4 C5 107.7(17) . .
C3 C4 W1 72.3(11) . .
C5 C4 W1 72.2(10) . .
C4 C5 C1 106.9(16) . .
C4 C5 W1 72.2(10) . .
C1 C5 W1 72.5(10) . .
C1 C6 C7 117.7(18) . .
N1 C7 C8 124.6(17) . .
N1 C7 C6 115.6(15) . .
C8 C7 C6 119.7(16) . .
C9 C8 C7 117.7(16) . .
C10 C9 C8 119.0(16) . .
N1 C11 C10 124.1(16) . .
C11 N1 C7 116.5(15) . .
C13 W1 C15 106.4(8) . .
C13 W1 C14 79.7(7) . .
C15 W1 C14 77.2(7) . .
C13 W1 C2 98.9(7) . .
C15 W1 C2 154.6(7) . .
C14 W1 C2 108.0(6) . .
C13 W1 C4 157.8(8) . .
C15 W1 C4 95.7(8) . .
C14 W1 C4 107.9(7) . .
C2 W1 C4 59.0(7) . .
C13 W1 C5 133.6(6) . .
C15 W1 C5 101.2(7) . .
C14 W1 C5 143.5(6) . .
C2 W1 C5 59.5(6) . .
C4 W1 C5 35.7(6) . .
C13 W1 C3 126.2(8) . .
C15 W1 C3 122.8(7) . .
C14 W1 C3 90.6(7) . .
C2 W1 C3 34.8(7) . .
C4 W1 C3 35.6(8) . .
C5 W1 C3 59.2(6) . .
C13 W1 C1 101.8(6) . .
C15 W1 C1 134.9(7) . .
C14 W1 C1 143.1(6) . .
C2 W1 C1 35.1(6) . .
C4 W1 C1 59.4(6) . .
C5 W1 C1 36.3(5) . .
C3 W1 C1 58.4(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C10 C9 1.38(2) .
C10 C11 1.40(2) .
C10 C12 1.49(3) .
C12 F3 1.32(2) .
C12 F2 1.33(2) .
C12 F1 1.34(2) .
C1 C2 1.41(2) .
C1 C6 1.47(3) .
C1 C5 1.47(2) .
C1 W1 2.361(17) .
C13 O1 1.16(2) .
C13 W1 1.961(16) .
C2 C3 1.40(3) .
C2 W1 2.332(17) .
C14 O2 1.15(2) .
C14 W1 1.974(18) .
C3 C4 1.43(3) .
C3 W1 2.346(17) .
C15 O3 1.143(19) .
C15 W1 1.967(16) .
C4 C5 1.44(2) .
C4 W1 2.344(18) .
C5 W1 2.344(17) .
C6 C7 1.51(3) .
C7 N1 1.34(2) .
C7 C8 1.38(2) .
C8 C9 1.38(3) .
C11 N1 1.31(2) .
