[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_7717017
_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 H24 N2 P2 S4'
_chemical_formula_sum            'C18 H24 N2 P2 S4'
_chemical_formula_weight         458.57
_chemical_name_systematic        TK-326
_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             2022-03-25
_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                94.948(3)
_cell_angle_beta                 94.001(3)
_cell_angle_gamma                96.798(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2842(5)
_cell_length_b                   9.9259(6)
_cell_length_c                   15.0111(9)
_cell_measurement_reflns_used    8115
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.59
_cell_volume                     1070.17(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20653
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0724 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.9040.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6196
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0295P)^2^+0.4535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5449
_reflns_number_total             6196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02029d2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7717017--7717018.cif.'
_cod_database_code               7717017
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C6 \\sim C5-C6A
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H5BC)=Sof(H5BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(1)
 Sof(H5AA)=Sof(H5AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5AA,H5AB), C5(H5BC,H5BD), C10(H10A,H10B), C11(H11A,H11B),
 C15(H15A,H15B), C17(H17A,H17B)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C6A(H6AA,H6AB,H6AC)
;
_shelx_res_checksum              65629
_shelx_hkl_checksum              86728
_olex2_submission_special_instructions 'No special instructions were received'