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_7713306
_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         'C32 H48 N2 P2 S8 Se2'
_chemical_formula_sum            'C32 H48 N2 P2 S8 Se2'
_chemical_formula_weight         937.06
_chemical_name_systematic        SHK-474
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0643(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.4912(5)
_cell_length_b                   7.70630(10)
_cell_length_c                   21.8491(5)
_cell_measurement_reflns_used    58628
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.29
_cell_measurement_theta_min      3.67
_cell_volume                     4080.54(14)
_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                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.737
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'Axo Cu'
_exptl_absorpt_coefficient_mu    7.03
_exptl_absorpt_correction_T_max  0.3100
_exptl_absorpt_correction_T_min  0.1542
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7388
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+18.8734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6702
_reflns_number_total             7388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00985h2.cif
_cod_data_source_block           cis-8f
_cod_database_code               7713306
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.540
_shelx_estimated_absorpt_t_min   0.418
_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. Restrained distances
 C27S-C28S = C32-C31 = C31S-C32S
 1.5 with sigma of 0.01
 N1S-C27S = N1S-C25S = N2S-C29S = N2-C29 = N2-C31
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N1S \\sim C25 \\sim C25S \\sim C26 \\sim C26S \\sim C27 \\sim C27S
\\sim C28 \\sim C28S: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
N2 \\sim N2S \\sim C29 \\sim C29S \\sim C30 \\sim C30S \\sim C31 \\sim C31S
\\sim C32 \\sim C32S: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C25S) \\sim Ueq, Uanis(C26S) \\sim Ueq, Uanis(C28S) \\sim Ueq,
Uanis(C27S) \\sim Ueq, Uanis(N1S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(Se2S)=Sof(P2S)=Sof(N2S)=Sof(C29S)=Sof(H29C)=Sof(H29D)=Sof(C30S)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=Sof(C31S)=Sof(H31C)=Sof(H31D)=Sof(C32S)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(Se2)=Sof(P2)=Sof(N2)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=FVAR(1)
 Sof(Se1S)=Sof(P1S)=Sof(N1S)=Sof(C25S)=Sof(H25C)=Sof(H25D)=Sof(C26S)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C27S)=Sof(H27C)=Sof(H27D)=Sof(C28S)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(Se1)=Sof(P1)=Sof(N1)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C25S(H25C,
 H25D), C27(H27A,H27B), C27S(H27C,H27D), C29(H29A,H29B), C29S(H29C,H29D),
 C31S(H31C,H31D)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C26S(H26D,H26E,H26F), C28(H28A,H28B,H28C),
 C28S(H28D,H28E,H28F), C30(H30A,H30B,H30C), C30S(H30D,H30E,H30F), C32(H32A,H32B,
 H32C), C32S(H32D,H32E,H32F)
;
_shelx_res_checksum              60097
_shelx_hkl_checksum              83965
_olex2_submission_special_instructions 'No special instructions were received'