[4 + 2]-Cycloadditions of a thiazol-based tricyclic 1,4-diphosphinine and a new easy 1,4-diphosphinine protection deprotection strategy.
Begum, Imtiaz; Kalisch, Tim; Schnakenburg, Gregor; Kelemen, Zsolt; Nyulászi, László; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12776–12779; doi:10.1039/d0dt02529a

data_7705333
_publ_section_title
;
 [4 + 2]-Cycloadditions of a thiazol-based tricyclic 1,4-diphosphinine and
 a new easy 1,4-diphosphinine protection deprotection strategy.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12776
_journal_page_last               12779
_journal_paper_doi               10.1039/d0dt02529a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H20 N2 O4 P2 S4'
_chemical_formula_sum            'C18 H20 N2 O4 P2 S4'
_chemical_formula_weight         518.54
_chemical_name_systematic        IB-282
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                77.826(3)
_cell_angle_beta                 75.301(3)
_cell_angle_gamma                89.011(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1125(6)
_cell_length_b                   10.1260(6)
_cell_length_c                   11.9070(7)
_cell_measurement_reflns_used    7410
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.38
_cell_volume                     1151.99(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29215
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.084
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1266 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.8712. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0225P)^2^+2.7851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4440
_reflns_number_total             5556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02529a2.cif
_cod_data_source_block           5246f
_cod_depositor_comments
'Adding full bibliography for 7705332--7705333.cif.'
_cod_database_code               7705333
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.873
_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)
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              25321
_olex2_submission_special_instructions 'No special instructions were received'