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_7715199
_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 Se2'
_chemical_formula_sum            'C28 H48 N4 P2 Se2'
_chemical_formula_weight         660.56
_chemical_name_systematic        TT-500
_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
_audit_creation_date             2022-03-25
_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                108.515(2)
_cell_angle_beta                 95.741(3)
_cell_angle_gamma                97.957(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1836(4)
_cell_length_b                   11.7770(5)
_cell_length_c                   14.4181(6)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      71.86
_cell_measurement_theta_min      3.27
_cell_volume                     1604.70(12)
_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
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0612
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19425
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.731
_diffrn_reflns_theta_min         3.271
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.988
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.4152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1190 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.5510.
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    1.367
_exptl_crystal_description       plank
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5640
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0636P)^2^+16.1980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4712
_reflns_number_total             5640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00378k2.cif
_cod_data_source_block           A
_cod_depositor_comments
'Adding full bibliography for 7715199--7715200.cif.'
_cod_database_code               7715199
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.447
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. 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
3.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6B,H6A), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C25(H25A,H25B), C27(H27A,H27B)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              95018
_olex2_submission_special_instructions 'No special instructions were received'