Visible light induced formation of a tungsten hydride complex.
Isaacs, Diane P.; Gruninger, Cole T.; Huang, Tao; Jordan, Aldo M.; Nicholas, Genique; Chen, Chun-Hsing; Ter Horst, Marc A.; Dempsey, Jillian L.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03675d

data_7712316
_publ_section_title
;
 Visible light induced formation of a tungsten hydride complex.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03675d
_journal_year                    2023
_chemical_formula_moiety         'C10.00 H8.00 F6 N1.00 O3 P1 W1.00'
_chemical_formula_sum            'C10 H8 F6 N O3 P W'
_chemical_formula_weight         518.99
_chemical_melting_point          ?
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2023-01-29
_audit_creation_method           'CRYSTALS_ver_*****_build_0e3dcff '
_audit_update_record
;
2023-02-02 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2330(6)
_cell_length_b                   7.7115(4)
_cell_length_c                   16.5205(6)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150
_cell_measurement_theta_max      74.66
_cell_measurement_theta_min      4.69
_cell_volume                     1430.36(12)
_computing_cell_refinement       'Apex4 (Bruker AXS, 2021)'
_computing_data_collection       'Apex4 (Bruker AXS, 2021)'
_computing_data_reduction        'Apex4 (Bruker AXS, 2021)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17784
_diffrn_reflns_theta_full        25.878
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         2.161
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.265
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968.000
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.93
_refine_diff_density_min         -2.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         2901
_refine_ls_number_restraints     410
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0354410
_refine_ls_shift/su_mean         0.0022379
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +35.20P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1021
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1021
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                2657
_reflns_number_total             2912
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2631(3)
_oxford_structure_analysis_title 'I in C:\Frames\guest\23001a\work At 23:12 on'
_cod_data_source_file            d2dt03675d2.cif
_cod_data_source_block           23001
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C10.00 H8.00 F6 N1.00 O3 P1 W1.00'
_cod_database_code               7712316
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0454
_reflns_number_all               2901