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

data_7712671
_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         'C45 H28 B F15 N P'
_chemical_formula_sum            'C45 H28 B F15 N P'
_chemical_formula_weight         909.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-04
_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                90
_cell_angle_beta                 90.842(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9807(8)
_cell_length_b                   17.4205(11)
_cell_length_c                   21.3172(13)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.19
_cell_volume                     4077.3(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1068
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67099
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.911
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0402P)^2^+2.3329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5119
_reflns_number_total             7177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00607g2.cif
_cod_data_source_block           final
_cod_database_code               7712671
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00T(H00T), C00W(H00W)
2.b Secondary CH2 refined with riding coordinates:
 C01G(H01C,H01G), C01M(H01J,H01K)
2.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C015(H015), C019(H019), C01A(H01A), C01B(H01B), C01D(H01D),
 C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I), C01L(H01L), C01N(H01N),
 C01O(H01O)
2.d Idealised Me refined as rotating group:
 C01P(H01M,H01P,H01Q), C01Q(H01R,H01S,H01T), C01R(H01U,H01V,H01W)
;
_shelx_res_checksum              52374
_shelx_hkl_checksum              19904
_olex2_submission_special_instructions 'No special instructions were received'