On the Reaction of Potassium Phosphide KP(iPr)Ter with Chalcogenes, Heteroallenes and Acyl Chloride
Schulz, Axel; Szych, Lilian; Pilopp, Yannic; Bresien, Jonas; Villinger, Alexander; Lüdtke, Karsten Paul; Dalton Transactions  (2021) –; doi:10.1039/D1DT03400F

data_7708646
_publ_section_title
;
 On the Reaction of Potassium Phosphide KP(iPr)Ter with Chalcogenes,
 Heteroallenes and Acyl Chloride
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03400F
_journal_year                    2021
_chemical_formula_moiety
'C60 H77 K2 O2 P2 Se4, C4 H8 O, 0.5(C4 H10 O2)'
_chemical_formula_sum            'C60 H77 K2 O2 P2 Se4'
_chemical_formula_weight         1286.20
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.786(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9206(7)
_cell_length_b                   17.3366(14)
_cell_length_c                   37.912(3)
_cell_measurement_reflns_used    9473
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.53
_cell_measurement_theta_min      2.57
_cell_volume                     5856.3(8)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            97852
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.743
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
The unit cell contains four THF and two DME molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. These were removed from the model, but included 
in the empirical formula.
;
_refine_diff_density_max         2.706
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         17065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0229P)^2^+30.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15002
_reflns_number_total             17065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03400f2.cif
_cod_data_source_block           is_kpl02
_cod_depositor_comments
;

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         643.10
_cod_original_formula_moiety
'C30 H38.50 K O P Se2, 0.5(C4 H8 O), 0.25(C4 H10 O2)'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C30 H38.50 K O P Se2'
_cod_database_code               7708646
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.547
_shelx_estimated_absorpt_t_max   0.700
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              79912