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_7133429
_publ_section_title
;
 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         'C20 H38 B P'
_chemical_formula_sum            'C20 H38 B P'
_chemical_formula_weight         320.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.932(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.620(8)
_cell_length_b                   10.375(6)
_cell_length_c                   13.264(7)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    110
_cell_measurement_theta_max      35.090
_cell_measurement_theta_min      2.856
_cell_volume                     1869.9(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       Apex3
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            117764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.393
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0634 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.9138.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         9085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.2684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7023
_reflns_number_total             9085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02665a3.cif
_cod_data_source_block           2tBu
_cod_depositor_comments
'Adding full bibliography for 7133423--7133430.cif.'
_cod_original_cell_volume        1869.9(19)
_cod_database_code               7133429
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
;
_shelx_res_checksum              86667
_shelx_hkl_checksum              20450
_olex2_submission_special_instructions 'No special instructions were received'