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_7711832
_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 Se'
_chemical_formula_sum            'C48 H50 P2 Se'
_chemical_formula_weight         767.78
_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             2021-09-15
_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                 108.913(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8943(14)
_cell_length_b                   20.007(3)
_cell_length_c                   16.3852(19)
_cell_measurement_reflns_used    9434
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      1.27
_cell_volume                     3998.8(9)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_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
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 234 frames, detector distance = 120 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1357
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35099
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.662
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.500
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.793
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.793
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1136
_reflns_d_resolution_high        0.788
_reflns_d_resolution_low         15.501
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                3523
_reflns_number_total             7449
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d2dt03703c2.cif
_cod_data_source_block           ks1544
_cod_original_cell_volume        3998.9(8)
_cod_database_code               7711832
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.817
_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 Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C29(H29), C34(H34), C37(H37), C10(H10), C19(H19),
 C46(H46), C43(H43), C5(H5), C13(H13), C22(H22), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C36(H36A,H36B,H36C), C42(H42A,H42B,
 H42C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C24(H24A,
 H24B,H24C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C),
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              63717
_olex2_submission_special_instructions 'No special instructions were received'