[4 + 1]- and [4 + 2]-cycloadditions of a thiazole-2-thione-based 1,4-diphosphinine - broadening the scope.
Kalisch, Tim; Schnakenburg, Gregor; Nikonov, Georgii I.; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16018–16022; doi:10.1039/d4dt02029d

data_7717018
_publ_section_title
;
 [4 + 1]- and [4 + 2]-cycloadditions of a thiazole-2-thione-based
 1,4-diphosphinine - broadening the scope.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16018
_journal_page_last               16022
_journal_paper_doi               10.1039/d4dt02029d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H26 N2 P2 S4'
_chemical_formula_sum            'C18 H26 N2 P2 S4'
_chemical_formula_weight         460.62
_chemical_name_systematic        KT-374
_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             2022-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                102.542(3)
_cell_angle_beta                 101.566(3)
_cell_angle_gamma                106.023(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3076(3)
_cell_length_b                   10.2906(4)
_cell_length_c                   15.3615(6)
_cell_measurement_reflns_used    34334
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.03
_cell_measurement_theta_min      4.68
_cell_volume                     1183.70(9)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27308
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.614
_diffrn_reflns_theta_min         4.671
_diffrn_source                   'Axo Cu'
_exptl_absorpt_coefficient_mu    5.00
_exptl_absorpt_correction_T_max  0.4032
_exptl_absorpt_correction_T_min  0.2631
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0756P)^2^+0.5265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3926
_reflns_number_total             4455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02029d2.cif
_cod_data_source_block           4f
_cod_depositor_comments
'Adding full bibliography for 7717017--7717018.cif.'
_cod_original_cell_volume        1183.70(8)
_cod_database_code               7717018
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.434
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              73926
_shelx_hkl_checksum              34259
_shelx_fab_checksum              90432
_olex2_submission_special_instructions 'No special instructions were received'