Deoxygenation of chalcogen oxides EO2 (E = S, Se) with phospha-Wittig reagents
Dankert, Fabian; Gupta, Priyanka; Wellnitz, Tim; Baumann, Wolfgang; Hering-Junghans, Christian; Dalton Transactions  (2022) –; doi:10.1039/D2DT03703C

data_7711831
_publ_section_title
;
 Deoxygenation of chalcogen oxides EO2 (E = S, Se) with phospha-Wittig
 reagents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03703C
_journal_year                    2022
_chemical_formula_moiety         'C48 H50 P2 S'
_chemical_formula_sum            'C48 H50 P2 S'
_chemical_formula_weight         720.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-11-22 deposited with the CCDC.	2022-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.973(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9047(5)
_cell_length_b                   20.0414(8)
_cell_length_c                   16.3540(7)
_cell_measurement_reflns_used    23543
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      62.497
_cell_measurement_theta_min      3.610
_cell_volume                     3999.8(3)
_computing_cell_refinement       'APEX2, Bruker'
_computing_data_collection       'APEX2, Bruker'
_computing_data_reduction        'APEX2, Bruker'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23543
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        62.497
_diffrn_reflns_theta_max         62.497
_diffrn_reflns_theta_min         3.610
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS was used for absorption correction within APEX2'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6312
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+0.6259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4380
_reflns_number_total             6312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03703c2.cif
_cod_data_source_block           ax2253
_cod_database_code               7711831
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.594
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-P1 \\sim S2-P3 \\sim S2-P4 \\sim S1-P2
 with sigma of 0.01
 P3-C1 \\sim P1-C1
 with sigma of 0.01
 P4-C25 \\sim P2-C25
 with sigma of 0.01
 P2-P1 \\sim P4-P3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P1 \\sim P3 \\sim P4 \\sim P2 \\sim S2 \\sim S1: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.002 within 2A
Uanis(P1) = Uanis(P3)
Uanis(P2) = Uanis(P4)
4. Others
 Fixed Sof: P1(0.5) P3(0.5) S2(0.5) S1(0.5) P4(0.5) P2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C33(H33), C35(H35), C42(H42), C44(H44), C9(H9),
 C18(H18), C20(H20), C11(H11), C3(H3), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C22(H22A,H22B,
 H22C), C47(H47A,H47B,H47C), C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C46(H46A,
 H46B,H46C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              73935
_olex2_submission_special_instructions 'No special instructions were received'