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_7133428
_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         'C54 H98 B2 N4 P2 Pt, 0.5(C4 H8 O)'
_chemical_formula_sum            'C56 H102 B2 N4 O0.5 P2 Pt'
_chemical_formula_weight         1118.06
_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     dual
_audit_creation_date             2024-04-16
_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                101.270(3)
_cell_angle_beta                 98.789(3)
_cell_angle_gamma                90.250(3)
_cell_formula_units_Z            1
_cell_length_a                   10.6781(5)
_cell_length_b                   10.9251(5)
_cell_length_c                   12.9656(6)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.249
_cell_measurement_theta_min      3.157
_cell_volume                     1465.06(12)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.0900
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            91063
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.829
_diffrn_reflns_theta_min         3.079
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1058 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.7582.
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    1.267
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.352
_refine_diff_density_min         -2.287
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5569
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0574P)^2^+3.6288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5541
_reflns_number_total             5569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02665a3.cif
_cod_data_source_block           10tBu
_cod_depositor_comments
'Adding full bibliography for 7133423--7133430.cif.'
_cod_original_formula_sum        'C56 H102 B2 N4 O0.50 P2 Pt'
_cod_database_code               7133428
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Rigid bond restraints
 H7A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O28, C31, C29, C30, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(O28) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.2
3. Others
 Fixed Sof: O28(0.25) C31(0.25) H31A(0.25) H31B(0.25) C29(0.25) H29A(0.25)
 H29B(0.25) C30(0.25) H30A(0.25) H30B(0.25) C28(0.25) H28B(0.25) H28A(0.25)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), C6(H6)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B), C2(H2A,H2B), C3(H3A,
 H3B), C7(H7A,H7B), C31(H31A,H31B), C29(H29A,H29B), C30(H30A,H30B), C28(H28B,
 H28A)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C12(H12), C15(H15)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              55277
_shelx_hkl_checksum              16739
_olex2_submission_special_instructions 'No special instructions were received'