Access to and reactions of P-functional 1,4-dihydro-1,4-diphosphinines fused to two TTF units.
Kermanshahian, Shahriar; Kalisch, Tim; Kelemen, Zsolt; Schnakenburg, Gregor; Nyulászi, László; Boeré, René T; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00985h

data_7713304
_publ_section_title
;
 Access to and reactions of P-functional 1,4-dihydro-1,4-diphosphinines
 fused to two TTF units.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00985h
_journal_year                    2023
_chemical_formula_moiety         'C H2 Cl2, 2(C24 H32 N2 P2 S8)'
_chemical_formula_sum            'C49 H66 Cl2 N4 P4 S16'
_chemical_formula_weight         1418.79
_chemical_name_systematic        SHK-150
_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             2019-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.950(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.909(2)
_cell_length_b                   11.9462(15)
_cell_length_c                   17.630(2)
_cell_measurement_reflns_used    8474
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.28
_cell_volume                     3187.5(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33038
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.277
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5748
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1718 before and 0.0724 after correction. The Ratio of minimum to maximum transmission is 0.7704. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7663
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.004
_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^+4.7952P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4841
_reflns_number_total             7663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00985h2.cif
_cod_data_source_block           cis-5d
_cod_original_cell_volume        3187.4(7)
_cod_database_code               7713304
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.875
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C25(0.5) H25A(0.5) H25B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              22566
_shelx_hkl_checksum              41531
_olex2_submission_special_instructions 'No special instructions were received'