Synthesis of P-bridged, planar bis(NHC) BCl<sub>3</sub> adducts.
Terschüren, Tatjana; Schnakenburg, Gregor; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16377–16383; doi:10.1039/d4dt02235a

data_7717039
_publ_section_title
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 Synthesis of P-bridged, planar bis(NHC) BCl<sub>3</sub> adducts.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16377
_journal_page_last               16383
_journal_paper_doi               10.1039/d4dt02235a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H56 B2 Cl6 N6 O2 P2'
_chemical_formula_sum            'C30 H56 B2 Cl6 N6 O2 P2'
_chemical_formula_weight         829.06
_chemical_name_systematic        TT-274
_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             2021-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                115.6440(10)
_cell_angle_beta                 92.465(2)
_cell_angle_gamma                97.618(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9165(4)
_cell_length_b                   10.3070(4)
_cell_length_c                   11.5166(5)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    123
_cell_measurement_theta_max      72.58
_cell_measurement_theta_min      4.29
_cell_volume                     1045.14(8)
_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      123
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.974
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12580
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.577
_diffrn_reflns_theta_min         4.527
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.752
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.4836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1362 before and 0.0739 after correction. The Ratio of minimum to maximum transmission is 0.6418. 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    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4054
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0600P)^2^+3.3054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3560
_reflns_number_total             4054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02235a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7717039.cif.'
_cod_original_cell_volume        1045.14(7)
_cod_database_code               7717039
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.312
_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
 C12-C13 \\sim C12S-C13S
 with sigma of 0.0001
 C13-C14 \\sim C13S-C14S
 with sigma of 0.0001
 C14-C15 \\sim C14S-C15S
 with sigma of 0.0001
 N2-C12 \\sim N2-C12S
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
C13 \\sim C13S: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.005
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13S) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
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(C13S)=Sof(H13C)=Sof(H13D)=Sof(C14S)=Sof(H14C)=Sof(H14D)=Sof(C15S)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C12S)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C13(H13A,
 H13B), C14(H14A,H14B), C13S(H13C,H13D), C14S(H14C,H14D), C12(H12A,H12B),
 C12S(H12C,H12D)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C),
 C15S(H15D,H15E,H15F)
;
_shelx_res_checksum              83510
_shelx_hkl_checksum              5033
_olex2_submission_special_instructions 'No special instructions were received'