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_7716810
_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         'C56 H88 Cl4 N4 P2 Rh4 Se2, 2(C7 H8)'
_chemical_formula_sum            'C70 H104 Cl4 N4 P2 Rh4 Se2'
_chemical_formula_weight         1774.87
_chemical_name_systematic        TT-808
_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     dual
_audit_creation_date             2024-06-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-17 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                109.729(2)
_cell_angle_beta                 92.124(3)
_cell_angle_gamma                106.197(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2812(4)
_cell_length_b                   15.1399(5)
_cell_length_c                   20.6038(7)
_cell_measurement_reflns_used    40940
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.97
_cell_measurement_theta_min      3.51
_cell_volume                     3705.3(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.975
_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_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54383
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.547
_diffrn_reflns_theta_min         4.609
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'Microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    10.254
_exptl_absorpt_correction_T_max  0.2369
_exptl_absorpt_correction_T_min  0.0800
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         13851
_refine_ls_number_restraints     1132
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0631P)^2^+62.3057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10483
_reflns_number_total             13851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01817f2.cif
_cod_data_source_block           A
_cod_depositor_comments
'Adding full bibliography for 7716810--7716811.cif.'
_cod_database_code               7716810
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.373
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C57-C63
 1.54 with sigma of 0.001
 C56-C55 \\sim C52-C51 \\sim C56-C49 \\sim C55-C54 \\sim C51-C50 \\sim C53-C52
 with sigma of 0.02
 C70-C64 \\sim C70S-C64S
 with sigma of 0.02
 C57-C58 \\sim C57A-C58A
 with sigma of 0.02
 C57-C62 \\sim C57A-C62A
 with sigma of 0.02
 C57-C63 \\sim C57A-C63A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.02
 C59-C60 \\sim C59A-C60A
 with sigma of 0.02
 C60-C61 \\sim C60A-C61A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 C57-C59 \\sim C57A-C59A
 with sigma of 0.04
 C57-C61 \\sim C57A-C61A
 with sigma of 0.04
 C58-C60 \\sim C58A-C60A
 with sigma of 0.04
 C58-C62 \\sim C58A-C62A
 with sigma of 0.04
 C58-C63 \\sim C58A-C63A
 with sigma of 0.04
 C59-C61 \\sim C59A-C61A
 with sigma of 0.04
 C60-C62 \\sim C60A-C62A
 with sigma of 0.04
 C62-C63 \\sim C62A-C63A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C70 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.02 within 2A
C50 \\sim C49 \\sim C56 \\sim C55 \\sim C54 \\sim C52 \\sim C51 \\sim C53:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C60) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C70S) \\sim Ueq, Uanis(C64S) \\sim Ueq, Uanis(C65S) \\sim Ueq,
Uanis(C66S) \\sim Ueq, Uanis(C67S) \\sim Ueq, Uanis(C68S) \\sim Ueq,
Uanis(C69S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C27S)=Sof(H27S)=Sof(C28S)=Sof(H28C)=Sof(H28D)=Sof(H29C)=Sof(H29D)=
 Sof(H32C)=Sof(H32D)=Sof(C33S)=Sof(H33C)=Sof(H33D)=Sof(C34S)=Sof(H34S)=1-FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H29A)=Sof(H29B)=Sof(H32A)=
 Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34)=FVAR(1)
 Sof(C64S)=Sof(C65S)=Sof(H65S)=Sof(C66S)=Sof(H66S)=Sof(C67S)=Sof(H67S)=
 Sof(C68S)=Sof(H68S)=Sof(C69S)=Sof(H69S)=Sof(C70S)=Sof(H70D)=Sof(H70E)=
 Sof(H70F)=1-FVAR(2)
 Sof(C64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=Sof(C68)=
 Sof(H68)=Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(2)
 Sof(C57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=
 Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63D)=Sof(H63E)=
 Sof(H63F)=1-FVAR(3)
 Sof(C57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=
 Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9), C12(H12), C13(H13), C27(H27), C27S(H27S), C30(H30), C31(H31),
 C34(H34), C34S(H34S), C41(H41), C42(H42), C45(H45), C46(H46), C49(H49),
 C50(H50), C53(H53), C54(H54)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C11(H11A,H11B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C28S(H28C,
 H28D), C29(H29A,H29B), C29(H29C,H29D), C32(H32A,H32B), C32(H32C,H32D),
 C33(H33A,H33B), C33S(H33C,H33D), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C39(H39A,H39B), C40(H40A,H40B), C43(H43A,H43B), C44(H44A,H44B),
 C47(H47A,H47B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,H52B), C55(H55A,H55B),
  C56(H56A,H56B)
6.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C38(H38A,H38B,H38C)
6.d Aromatic/amide H refined with riding coordinates:
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C65S(H65S), C66S(H66S), C67S(H67S), C68S(H68S),
 C69S(H69S), C58A(H58A), C59A(H59A), C60A(H60A), C61A(H61A), C62A(H62A)
6.e Fitted hexagon refined as free rotating group:
 C57(C58,C59,C60,C61,C62), C64(C65,C66,C67,C68,C69), C64S(C65S,C66S,C67S,C68S,
 C69S), C57A(C58A,C59A,C60A,C61A,C62A)
6.f Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C70S(H70D,H70E,H70F), C63A(H63D,
 H63E,H63F)
;
_shelx_res_checksum              29137
_shelx_hkl_checksum              43692
_olex2_submission_special_instructions 'No special instructions were received'