Insights into the Stability and Structures of Phosphine-Boranes and Their α-Metalated Derivatives
Izod, Keith; Wills, Corinne; Anderson, Emma; Harrington, Ross W.; Probert, Michael R.; Organometallics 33 (2014) 5283–; doi:10.1021/om5005995

data_4084364
_publ_section_title
;
 Insights into the Stability and Structures of Phosphine-Boranes and Their
 \a-Metalated Derivatives
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5283
_journal_paper_doi               10.1021/om5005995
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C27 H44 B Li O2 P2'
_chemical_formula_sum            'C27 H44 B Li O2 P2'
_chemical_formula_weight         480.31
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-01
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.19 svn.r2915 for OlexSys, GUI svn.r4811)
;
_cell_angle_alpha                74.945(4)
_cell_angle_beta                 77.243(4)
_cell_angle_gamma                76.944(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3112(5)
_cell_length_b                   11.9453(5)
_cell_length_c                   14.0786(7)
_cell_measurement_reflns_used    4376
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.4973
_cell_measurement_theta_min      2.9448
_cell_volume                     1451.01(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0559341000
_diffrn_orient_matrix_UB_12      -0.0513537000
_diffrn_orient_matrix_UB_13      0.0000768000
_diffrn_orient_matrix_UB_21      0.0395660000
_diffrn_orient_matrix_UB_22      0.0209798000
_diffrn_orient_matrix_UB_23      0.0274713000
_diffrn_orient_matrix_UB_31      -0.0401014000
_diffrn_orient_matrix_UB_32      -0.0287872000
_diffrn_orient_matrix_UB_33      0.0452833000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11266
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.951
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5541
_refine_ls_number_restraints     451
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0495P)^2^+0.9764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             5541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5005995_si_002.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 4084362--4084367.cif.'
_cod_database_code               4084364
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C14 H28 B Li P2'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C2 \\sim C4A-C2 \\sim C3-C2 \\sim C3A-C2
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A \\sim C22-C21 \\sim C22A-C21A \\sim C23-C22 \\sim
C23A-C22A \\sim C27-C26 ~
 C27-C26A \\sim C26A-C25A \\sim C26-C25 \\sim C25-C24 \\sim C25A-C24
 with sigma of 0.02
 O2-C27 \\sim O2-C24 \\sim O1-C20 \\sim O1A-C20A \\sim O1-C23 \\sim O1A-C23A
 with sigma of 0.02
 O1-Li1 \\sim O1A-Li1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C26A)
Uanis(C25) = Uanis(C25A)
Uanis(O1) = Uanis(O1A)
Uanis(C23) = Uanis(C23A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C20) = Uanis(C20A)
Uanis(C3) = Uanis(C3)
Uanis(C4) = Uanis(C4A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=
 Sof(H26D)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H27A)=Sof(H27B)=FVAR(1)
 Sof(O1A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(2)
 Sof(O1)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(2)
 Sof(H2B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=1-FVAR(3)
 Sof(H2A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B), C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,H21B), C21A(H21C,H21D), C22(H22A,
 H22B), C22A(H22C,H22D), C23(H23A,H23B), C23A(H23C,H23D), C24(H24A,H24B),
 C24(H24C,H24D), C25(H25A,H25B), C25A(H25C,H25D), C26(H26A,H26B), C26A(H26C,
 H26D), C27(H27A,H27B), C27(H27C,H27D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC),
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              23634
_shelx_hkl_checksum              16325