Photo-decarbonylation of aldehydes by <i>trans</i>-W(N<sub>2</sub>)<sub>2</sub>(dppe)<sub>2</sub> at room temperature.
Wang, Chuang-Xin; Li, Yuhan; Yang, Yunhui; Wang, Congyang; Organic & biomolecular chemistry 23 (2025) 8426–8430; doi:10.1039/d5ob01309g

data_7160706
_publ_section_title
;
 Photo-decarbonylation of aldehydes by
 <i>trans</i>-W(N<sub>2</sub>)<sub>2</sub>(dppe)<sub>2</sub> at room
 temperature.
;
_journal_issue                   37
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8426
_journal_page_last               8430
_journal_paper_doi               10.1039/d5ob01309g
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C54 H49 O2 P4 W, C3 H3'
_chemical_formula_sum            'C57 H52 O2 P4 W'
_chemical_formula_weight         1076.71
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-11 deposited with the CCDC.	2025-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.31870(10)
_cell_length_b                   14.27450(10)
_cell_length_c                   27.5403(2)
_cell_measurement_reflns_used    25810
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      77.4400
_cell_measurement_theta_min      3.2130
_cell_volume                     4821.53(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.96a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    117.00 178.00   0.50    0.08    --  108.85  45.00 -90.00  122
  2  \w    108.00 133.00   0.50    0.08    --  108.85  84.00 -38.00   50
  3  \w    -20.00  45.00   0.50    0.05    --   46.57 -38.00  90.00  130
  4  \w     41.00  74.00   0.50    0.08    --  108.85 -61.00 150.00   66
  5  \w     42.00  74.00   0.50    0.08    --  108.85 -61.00  90.00   64
  6  \w     39.00 100.00   0.50    0.08    --  108.85-125.00 -60.00  122
  7  \w     44.00  97.00   0.50    0.08    --  108.85 -84.00-159.00  106
  8  \w     45.00 111.00   0.50    0.08    --  108.85-125.00-180.00  132
  9  \w    -24.00  65.00   0.50    0.05    --   46.57 -84.00-159.00  178
 10  \w     76.00 106.00   0.50    0.08    --  108.85 -94.00  60.00   60
 11  \w     41.00  97.00   0.50    0.08    --  108.85-125.00 120.00  112
 12  \w    -16.00  24.00   0.50    0.05    --  -46.57  19.00  30.00   80
 13  \w    -15.00  28.00   0.50    0.05    --  -46.57  19.00 -30.00   86
 14  \w    -20.00  27.00   0.50    0.05    --  -46.57  19.00 -60.00   94
 15  \w    -65.00 -39.00   0.50    0.08    -- -104.50  61.00  90.00   52
 16  \w    -68.00 -43.00   0.50    0.08    -- -104.50  61.00 150.00   50
 17  \w    -64.00 -34.00   0.50    0.08    -- -104.50 125.00 120.00   60
 18  \w    -65.00 -34.00   0.50    0.05    --  -46.57  84.00 -38.00   62
 19  \w    -15.00  24.00   0.50    0.05    --  -46.57  84.00 -38.00   78
 20  \w   -111.00 -76.00   0.50    0.08    -- -104.50 125.00 120.00   70
 21  \w   -110.00 -35.00   0.50    0.08    -- -104.50 125.00 -30.00  150
 22  \w    -92.00 -53.00   0.50    0.08    -- -104.50  84.00 -38.00   78
 23  \w   -170.00-127.00   0.50    0.08    -- -104.50 -30.00 120.00   86
 24  \w   -174.00 -79.00   0.50    0.08    -- -104.50 -84.00-159.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1218104000
_diffrn_orient_matrix_UB_12      0.0151868000
_diffrn_orient_matrix_UB_13      0.0060217000
_diffrn_orient_matrix_UB_21      0.0273787000
_diffrn_orient_matrix_UB_22      0.0934894000
_diffrn_orient_matrix_UB_23      0.0263252000
_diffrn_orient_matrix_UB_31      -0.0136109000
_diffrn_orient_matrix_UB_32      0.0517970000
_diffrn_orient_matrix_UB_33      -0.0492612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35366
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.655
_diffrn_reflns_theta_min         3.224
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0322P)^2^+3.3062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9047
_reflns_number_total             9850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob01309g2.cif
_cod_data_source_block           tx15667_autored
_cod_depositor_comments          'Adding full bibliography for 7160706.cif.'
_cod_database_code               7160706
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         WCHONPBrSiPdK
_chemical_oxdiff_usercomment     WCHONPBrSiPdK
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C56(H56A,H56B), C55(H55A,H55B), C57(H57A,H57B), C54(H54A,H54B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C20(H20), C25(H25), C30(H30), C34(H34), C14(H14),
 C35(H35), C40(H40), C44(H44), C36(H36), C29(H29), C45(H45), C39(H39), C31(H31),
  C41(H41), C19(H19), C21(H21), C46(H46), C24(H24), C33(H33), C16(H16),
 C22(H22), C37(H37), C47(H47), C42(H42), C43(H43), C17(H17), C26(H26), C38(H38),
  C23(H23), C49(H49), C11(H11), C18(H18), C48(H48), C28(H28), C27(H27),
 C12(H12), C13(H13), C51(H51), C50(H50), C52(H52)
;
_shelx_res_checksum              60988
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.835
_oxdiff_exptl_absorpt_empirical_full_min 0.704