Selectivity of Tungsten Mediated Dinitrogen Splitting vs. Proton Reduction
Schluschaß, Bastian; Abbenseth, Josh; Demeshko, Serhiy; Finger, Markus; Franke, Alicja; Herwig, Christian; Würtele, Christian; Ivanović-Burmazović, Ivana; Limberg, Christian; Telser, Joshua; Schneider, Sven; Chemical Science  (2019) –; doi:10.1039/C9SC03779A

data_1552347
_publ_section_title
;
 Selectivity of Tungsten Mediated Dinitrogen Splitting vs. Proton
 Reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03779A
_journal_year                    2019
_chemical_formula_sum            'C47 H94 Cl2 F3 N4 O3 P4 S W2'
_chemical_formula_weight         1414.80
_chemical_name_common            BS-C-116
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-07-29 deposited with the CCDC.    2019-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7515(9)
_cell_length_b                   13.2485(6)
_cell_length_c                   22.2689(10)
_cell_measurement_reflns_used    9341
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.4560
_cell_measurement_theta_min      2.2559
_cell_volume                     5827.3(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.4'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1450
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            175705
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'microfucus sealed tube'
_diffrn_source_type              'INCOATEC microfocus sealed tube'
_exptl_absorpt_coefficient_mu    4.232
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   'Numerical Mu From Formula'
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear intense brown'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.033
_refine_diff_density_max         2.428
_refine_diff_density_min         -1.729
_refine_ls_abs_structure_details
;

Flack x determined using 5071 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         14544
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0387P)^2^+33.6704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                12528
_reflns_number_total             14544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03779a2.cif
_cod_data_source_block           CW_BS_170118_2
_cod_database_code               1552347
_shelx_res_checksum              57767