Inorganic ligand-supported Mo oxide as a hydrogen atom transfer photocatalyst for direct C(sp2)–H phosphorylation
Jiang, Zeqi; Jiang, Shuangfei; Gao, Jin; Xia, Junmei; Yu, Hongwei; Ma, Lixin; Chen, Xi; Chen, Bo; Zhang, Xinghua; Zhu, Wenchao; Green Chemistry 26 (2024) 5538–5545; doi:10.1039/D4GC00589A

data_7248360
_publ_section_title
;
 Inorganic ligand-supported Mo oxide as a hydrogen atom transfer
 photocatalyst for direct C(sp2)--H phosphorylation
;
_journal_issue                   9
_journal_name_full               'Green Chemistry'
_journal_page_first              5538
_journal_page_last               5545
_journal_paper_doi               10.1039/D4GC00589A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C19 H18 N O3 P S'
_chemical_formula_sum            'C19 H18 N O3 P S'
_chemical_formula_weight         371.37
_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
_audit_creation_date             2023-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2024-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.256(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3863(7)
_cell_length_b                   8.7024(3)
_cell_length_c                   12.2510(5)
_cell_measurement_reflns_used    7082
_cell_measurement_temperature    150
_cell_measurement_theta_max      69.78
_cell_measurement_theta_min      5.21
_cell_volume                     1811.36(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19403
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.122
_diffrn_reflns_theta_min         5.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6160
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1356 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.8177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0529P)^2^+0.5038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2988
_reflns_number_total             3426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4gc00589a2.cif
_cod_data_source_block           ff1
_cod_depositor_comments          'Adding full bibliography for 7248360.cif.'
_cod_database_code               7248360
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00G(H00G), C00I(H00I), C00J(H00J), C00L(H00N),
 C00M(H00O), C00N(H00P), C00O(H00Q), C00P(H00R)
2.c Idealised Me refined as rotating group:
 C00H(H00C,H00F,H00H), C00K(H00K,H00L,H00M)
;
_shelx_res_checksum              79251
_shelx_hkl_checksum              9800
_olex2_submission_special_instructions 'No special instructions were received'