Application of phosphorus-bridged rigid, bent bis(NHCs) as dipodal ligands in main group and transition metal chemistry.
Terschüren, Tatjana; Schnakenburg, Gregor; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5043–5050; doi:10.1039/d4dt00378k

data_7715200
_publ_section_title
;
 Application of phosphorus-bridged rigid, bent bis(NHCs) as dipodal
 ligands in main group and transition metal chemistry.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5043
_journal_page_last               5050
_journal_paper_doi               10.1039/d4dt00378k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H48 N4 P2'
_chemical_formula_sum            'C28 H48 N4 P2'
_chemical_formula_weight         502.64
_chemical_name_systematic        TT-592
_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   geom
_audit_creation_date             2022-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-10-18 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.089(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3905(7)
_cell_length_b                   14.4115(4)
_cell_length_c                   24.3244(11)
_cell_measurement_reflns_used    25445
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.52
_cell_measurement_theta_min      3.59
_cell_volume                     5937.9(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      '2590 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stadivari
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1397
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73734
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.746
_diffrn_reflns_theta_min         3.590
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.6694
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         10503
_refine_ls_number_restraints     541
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+15.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6258
_reflns_number_total             10503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00378k2.cif
_cod_data_source_block           B
_cod_depositor_comments
'Adding full bibliography for 7715199--7715200.cif.'
_cod_database_code               7715200
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.756
_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
 C17'-C18' \\sim C17'-C18"
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Sof(H17C)=Sof(H17D)=Sof(C18")=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(H17A)=Sof(H17B)=Sof(C18')=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C23'(H23'), C24'(H24')
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11C,H11D), C12(H12C,H12D),
 C13(H13C,H13D), C15(H15C,H15D), C16(H16C,H16D), C17(H17E,H17F), C19(H19C,H19D),
  C20(H20C,H20D), C21(H21C,H21D), C25(H25C,H25D), C27(H27C,H27D), C7'(H7'A,
 H7'B), C8'(H8'A,H8'B), C9'(H9'A,H9'B), C11'(H11A,H11B), C12'(H12A,H12B),
 C13'(H13A,H13B), C15'(H15A,H15B), C16'(H16A,H16B), C17'(H17A,H17B), C17'(H17C,
 H17D), C19'(H19A,H19B), C20'(H20A,H20B), C21'(H21A,H21B), C25'(H25A,H25B),
 C27'(H27A,H27B)
5.c Idealised Me refined as rotating group:
 C10(H10D,H10E,H10F), C14(H14D,H14E,H14F), C18(H18G,H18H,H18I), C22(H22D,H22E,
 H22F), C26(H26D,H26E,H26F), C28(H28D,H28E,H28F), C10'(H10A,H10B,H10C),
 C14'(H14A,H14B,H14C), C18'(H18A,H18B,H18C), C22'(H22A,H22B,H22C), C26'(H26A,
 H26B,H26C), C28'(H28A,H28B,H28C), C18"(H18D,H18E,H18F)
;
_shelx_res_checksum              99872
_olex2_submission_special_instructions 'No special instructions were received'