Tapping into the coordinative potential of a <i>C</i>-functional 1,4-diphosphabarrelene using two sets of complementary ligand centres.
Terschüren, Tatjana; Schnakenburg, Gregor; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13335–13339; doi:10.1039/d4dt01817f

data_7716811
_publ_section_title
;
 Tapping into the coordinative potential of a <i>C</i>-functional
 1,4-diphosphabarrelene using two sets of complementary ligand centres.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13335
_journal_page_last               13339
_journal_paper_doi               10.1039/d4dt01817f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H46 B2 N4 P2 Se2, C H2 Cl2'
_chemical_formula_sum            'C25 H48 B2 Cl2 N4 P2 Se2'
_chemical_formula_weight         717.05
_chemical_name_systematic        TT-893
_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   mixed
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-17 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.475(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5526(7)
_cell_length_b                   15.9233(12)
_cell_length_c                   23.092(2)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.419
_cell_measurement_theta_min      3.906
_cell_volume                     3442.3(5)
_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      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1538
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51353
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.744
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    5.147
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1729 before and 0.0868 after correction. The Ratio of minimum to maximum transmission is 0.6584. 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    1.384
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0544P)^2^+6.1864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4443
_reflns_number_total             6234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01817f2.cif
_cod_data_source_block           B
_cod_depositor_comments
'Adding full bibliography for 7716810--7716811.cif.'
_cod_database_code               7716811
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.577
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C7S-C6S = C5S-C6S = C5S-C4 = C6-C5 = C7-C6
 1.5 with sigma of 0.01
 C21-C20 = C21S-C20
 1.5 with sigma of 0.01
 B2-H2B = B2-H2A = B2-H2C = B1-H1B = B1-H1C = B1-H1A
 1.17 with sigma of 0.01
 C20-C21 \\sim C20-C21S
 with sigma of 0.02
 C22-C21 \\sim C22S-C21S
 with sigma of 0.02
 C20-C22 \\sim C20-C22S
 with sigma of 0.04
3. Rigid bond restraints
 Se2, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C10, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C5S \\sim C6 \\sim C6S \\sim C7 \\sim C7S: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C13) \\sim Ueq, Uanis(Se2) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22S)
\\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Rigid body (RIGU) restrains
 C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(C6S)=Sof(H6SA)=Sof(H6SB)=
 Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(H20D)=Sof(H20C)=Sof(C21S)=Sof(H21C)=Sof(H21D)=Sof(C22S)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5S(H5SA,H5SB), C6(H6A,H6B),
 C6S(H6SA,H6SB), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C20(H20D,H20C),
  C21(H21A,H21B), C21S(H21C,H21D), C23(H23A,H23B), C24(H24A,H24B), C27(H27A,
 H27B)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C7S(H7SA,H7SB,H7SC), C11(H11A,H11B,H11C), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C22S(H22D,H22E,H22F)
;
_shelx_res_checksum              80625
_shelx_hkl_checksum              9821
_olex2_submission_special_instructions 'No special instructions were received'