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_7133425
_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 H37 B2 O P'
_chemical_formula_sum            'C26 H37 B2 O P'
_chemical_formula_weight         418.14
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                78.769(2)
_cell_angle_beta                 77.719(3)
_cell_angle_gamma                67.258(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1755(6)
_cell_length_b                   11.3395(7)
_cell_length_c                   12.5538(8)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.276
_cell_measurement_theta_min      2.435
_cell_volume                     1167.84(13)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44609
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.327
_diffrn_reflns_theta_min         1.963
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1111 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.9324.
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    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0497P)^2^+0.5328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5187
_reflns_number_total             5809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02665a3.cif
_cod_data_source_block           7Ph
_cod_depositor_comments
'Adding full bibliography for 7133423--7133430.cif.'
_cod_database_code               7133425
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8), C4(H4), C6(H6)
1.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B), C9(H9A,H9B), C24(H24A,
 H24B), C26(H26A,H26B), C25(H25A,H25B), C23(H23A,H23B), C7(H7A,H7B)
1.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C18(H18), C13(H13), C14(H14), C22(H22), C15(H15),
 C19(H19), C20(H20), C21(H21)
;
_shelx_res_checksum              44749
_shelx_hkl_checksum              6
_olex2_submission_special_instructions 'No special instructions were received'