A metal and a metalloid Lewis acid bridged by a μ<sub>2</sub>-phosphinidene.
Biskup, David; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9670–9674; doi:10.1039/d4dt01276c

data_7716159
_publ_section_title
;
 A metal and a metalloid Lewis acid bridged by a
 &#x3bc;<sub>2</sub>-phosphinidene.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9670
_journal_page_last               9674
_journal_paper_doi               10.1039/d4dt01276c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H24 B N2 O5 P W, 2(C H2 Cl2)'
_chemical_formula_sum            'C30 H28 B Cl4 N2 O5 P W'
_chemical_formula_weight         863.97
_chemical_name_systematic        DB-630
_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   mixed
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                85.521(2)
_cell_angle_beta                 73.945(2)
_cell_angle_gamma                81.084(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0075(6)
_cell_length_b                   12.3330(7)
_cell_length_c                   12.9754(7)
_cell_measurement_reflns_used    8527
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.450
_cell_measurement_theta_min      2.857
_cell_volume                     1671.17(16)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9067
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.249
_diffrn_reflns_theta_min         2.942
_exptl_absorpt_coefficient_mu    3.865
_exptl_absorpt_correction_T_max  0.746427
_exptl_absorpt_correction_T_min  0.338087
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 188058 reflections, Rint = 0.0640
 (102821 with I > 3sig(I), Rint = 0.0531)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.44
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+1.6571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8719
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01276c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7716159--7716160.cif.'
_cod_database_code               7716159
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.205
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9653(10)
 0.0347(10)
2. 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
3. Restrained distances
 B-HB \\sim B-HC \\sim B-HA
 with sigma of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              21720
_olex2_submission_special_instructions 'No special instructions were received'