Reactive FLP-alkyne addition products: strategy to anionic and zwitterionic phosphines
Kim, Hyehwang; Stephan, Douglas W.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00607G

data_7712668
_publ_section_title
;
 Reactive FLP-alkyne addition products: strategy to anionic and
 zwitterionic phosphines
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00607G
_journal_year                    2023
_chemical_formula_moiety         'C54 H42 B F15 P2, C7 H8'
_chemical_formula_sum            'C61 H50 B F15 P2'
_chemical_formula_weight         1140.76
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-22 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                102.523(9)
_cell_angle_beta                 105.847(9)
_cell_angle_gamma                106.974(9)
_cell_formula_units_Z            2
_cell_length_a                   12.8941(18)
_cell_length_b                   14.241(2)
_cell_length_c                   16.718(2)
_cell_measurement_reflns_used    4108
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      20.71
_cell_measurement_theta_min      3.29
_cell_volume                     2673.8(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_unetI/netI     0.1307
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41998
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus 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    0.174
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0784 after correction.
The Ratio of minimum to maximum transmission is 0.8900.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         9342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1911
_refine_ls_R_factor_gt           0.1309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+50.6183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3459
_refine_ls_wR_factor_ref         0.3844
_reflns_number_gt                5551
_reflns_number_total             9342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00607g2.cif
_cod_data_source_block           t1
_cod_original_cell_volume        2673.9(7)
_cod_database_code               7712668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C25(H25), C26(H26), C38(H38), C41(H41), C46(H46), C5(H5), C8(H8),
 C9(H9), C10(H10), C51(H51), C52(H52), C54(H54), C55(H55), C60(H60), C58(H58),
 C59(H59)
2.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C3(H3A,H3B,H3C), C50(H50A,H50B,H50C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C49(H49A,H49B,H49C), C13(H13A,
 H13B,H13C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C)
;
_olex2_submission_special_instructions 'No special instructions were received'