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_7711835
_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         'C60 H74 P2 Se2, 3(C6 H6)'
_chemical_formula_sum            'C78 H92 P2 Se2'
_chemical_formula_weight         1249.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-21
_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                75.973(2)
_cell_angle_beta                 71.929(2)
_cell_angle_gamma                67.041(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6443(5)
_cell_length_b                   13.4424(5)
_cell_length_c                   13.6754(6)
_cell_measurement_reflns_used    2846
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      21.87
_cell_measurement_theta_min      2.24
_cell_volume                     1696.32(13)
_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)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20466
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.667
_diffrn_reflns_theta_max         66.667
_diffrn_reflns_theta_min         3.433
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'APEX2, SADABS was used for absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0482P)^2^+0.6103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5326
_reflns_number_total             5981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03703c2.cif
_cod_data_source_block           ax2263_cu
_cod_database_code               7711835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.742
_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.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22),
 C23(H23), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              49534
_olex2_submission_special_instructions 'No special instructions were received'