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_7713307
_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, C24 H32 N2 O2 P2 S8'
_chemical_formula_sum            'C25 H32 Cl2 N2 O2 P2 S8'
_chemical_formula_weight         781.84
_chemical_name_systematic        SHK-499
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_beta                 102.0920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9063(4)
_cell_length_b                   7.61506(10)
_cell_length_c                   19.2661(3)
_cell_measurement_reflns_used    77321
_cell_measurement_temperature    100
_cell_measurement_theta_max      3.78
_cell_measurement_theta_min      70.99
_cell_volume                     3429.53(9)
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            87125
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.734
_diffrn_reflns_theta_min         3.782
_diffrn_source                   'Axo Cu'
_exptl_absorpt_coefficient_mu    7.374
_exptl_absorpt_correction_T_max  0.6081
_exptl_absorpt_correction_T_min  0.4930
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0532P)^2^+8.2969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2767
_reflns_number_total             3093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00985h2.cif
_cod_data_source_block           trans-6d
_cod_database_code               7713307
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.608
_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
 Cl2S-C13S = Cl1S-C13S = Cl2-C13 = Cl1-C13
 1.7 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C13 \\sim Cl1S \\sim Cl2S \\sim Cl2 \\sim C13S \\sim Cl1: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(Cl1S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Cl2S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1S)=Sof(Cl2S)=Sof(C13S)=Sof(H13C)=Sof(H13D)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(Cl2)=Sof(C13)=Sof(H13A)=Sof(H13B)=0.5*FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13S(H13C,H13D), C9(H9A,H9B), C11(H11A,H11B)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              87751
_shelx_hkl_checksum              55527
_olex2_submission_special_instructions 'No special instructions were received'