2-Alkylphosphino-1-boraadamantanes.
Hoffmann, Kurt F.; Noriega, Rayni P.; Boyle, Paul D.; Drover, Marcus W.; Chemical communications (Cambridge, England) 60 (2024) 9222–9225; doi:10.1039/d4cc02665a

data_7133427
_publ_section_title
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 2-Alkylphosphino-1-boraadamantanes.
;
_journal_issue                   69
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9222
_journal_page_last               9225
_journal_paper_doi               10.1039/d4cc02665a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C26 H46 Au B Cl N2 P, 0.75(C4 H10 O)'
_chemical_formula_sum            'C29 H53.5 Au B Cl N2 O0.75 P'
_chemical_formula_weight         716.43
_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     direct
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
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_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                78.6195(18)
_cell_angle_beta                 86.0612(18)
_cell_angle_gamma                86.5573(18)
_cell_formula_units_Z            2
_cell_length_a                   7.1927(4)
_cell_length_b                   11.9175(6)
_cell_length_c                   19.1310(10)
_cell_measurement_reflns_used    9333
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.372
_cell_measurement_theta_min      2.842
_cell_volume                     1602.04(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            100956
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.643
_diffrn_reflns_theta_min         1.088
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.747
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.4353
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0663 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.5374.
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    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             727
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.072
_refine_diff_density_max         2.312
_refine_diff_density_min         -2.124
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9843
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+4.8044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8602
_reflns_number_total             9843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02665a3.cif
_cod_data_source_block           9tBu
_cod_depositor_comments
'Adding full bibliography for 7133423--7133430.cif.'
_cod_original_formula_sum        'C29 H53.50 Au B Cl N2 O0.75 P'
_cod_database_code               7133427
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.261
_olex2_refinement_description
;
1. Restrained distances
 O2DI-C35D \\sim O2DI-C31D \\sim O1-C29 \\sim O1-C27
 with sigma of 0.02
 C36D-C35D \\sim C34D-C31D \\sim C30-C29 \\sim C28-C27
 with sigma of 0.02
2. Rigid bond restraints
 O2DI, C35D, C35D, C34D, C34D, C31D, C31D, C36D, C36D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O2DI \\sim C35D \\sim C35D \\sim C34D \\sim C34D \\sim C31D \\sim C31D \\sim
C36D \\sim C36D: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C36D) \\sim Ueq, Uanis(C34D) \\sim Ueq, Uanis(C35D) \\sim Ueq,
Uanis(C31D) \\sim Ueq, Uanis(C35D) \\sim Ueq, Uanis(C31D) \\sim Ueq,
Uanis(C34D) \\sim Ueq, Uanis(C36D) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O1(0.5) C27(0.5) H27A(0.5) H27B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5)
 O2DI(0.25) C35D(0.25) H35A(0.25) H35B(0.25) C34D(0.25) H34A(0.25) H34B(0.25)
 H34C(0.25) C31D(0.25) H31A(0.25) H31B(0.25) C36D(0.25) H36A(0.25) H36B(0.25)
 H36C(0.25)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C10(H10), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C7(H7A,H7B), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,
 H2B), C9(H9A,H9B), C27(H27A,H27B), C29(H29A,H29B), C35D(H35A,H35B), C31D(H31A,
 H31B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C15(H15), C12(H12)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C25(H25A,H25B,
 H25C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C18(H18A,
 H18B,H18C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C34D(H34A,H34B,H34C),
 C36D(H36A,H36B,H36C)
;
_shelx_res_checksum              94146
_shelx_hkl_checksum              14967
_olex2_submission_special_instructions 'No special instructions were received'