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_4084366
_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         'C25 H47 B2 Li N2 P2'
_chemical_formula_sum            'C25 H47 B2 Li N2 P2'
_chemical_formula_weight         466.14
_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
_audit_creation_date             2014-04-01
_audit_creation_method
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Olex2 1.2-alpha
(compiled 2014.03.19 svn.r2915 for OlexSys, GUI svn.r4811)
;
_cell_angle_alpha                78.471(3)
_cell_angle_beta                 79.092(3)
_cell_angle_gamma                76.368(3)
_cell_formula_units_Z            4
_cell_length_a                   12.4933(4)
_cell_length_b                   14.0993(5)
_cell_length_c                   17.8125(6)
_cell_measurement_reflns_used    10628
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5561
_cell_measurement_theta_min      2.9941
_cell_volume                     2954.24(18)
_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)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0553071000
_diffrn_orient_matrix_UB_12      -0.0037807000
_diffrn_orient_matrix_UB_13      -0.0198621000
_diffrn_orient_matrix_UB_21      -0.0062719000
_diffrn_orient_matrix_UB_22      -0.0396312000
_diffrn_orient_matrix_UB_23      -0.0167232000
_diffrn_orient_matrix_UB_31      -0.0198107000
_diffrn_orient_matrix_UB_32      0.0341705000
_diffrn_orient_matrix_UB_33      -0.0318607000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.817
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27195
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.619
_diffrn_reflns_theta_min         3.000
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97211
_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    1.048
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         12382
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_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^+1.1185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9669
_reflns_number_total             12382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5005995_si_002.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 4084362--4084367.cif.'
_cod_database_code               4084366
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C40 H50 P2 N2 B2 Li'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.82
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. 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
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C27(H27), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C47(H47A,H47B), C48(H48A,H48B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              21307
_shelx_hkl_checksum              30794