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_4084367
_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 H41 Li N2 P2'
_chemical_formula_sum            'C25 H41 Li N2 P2'
_chemical_formula_weight         438.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 113.598(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2843(6)
_cell_length_b                   17.0975(7)
_cell_length_c                   9.3062(5)
_cell_measurement_reflns_used    5906
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.4368
_cell_measurement_theta_min      3.3675
_cell_volume                     1353.72(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0628387000
_diffrn_orient_matrix_UB_12      0.0192772000
_diffrn_orient_matrix_UB_13      0.0605001000
_diffrn_orient_matrix_UB_21      0.0449387000
_diffrn_orient_matrix_UB_22      -0.0349211000
_diffrn_orient_matrix_UB_23      0.0153951000
_diffrn_orient_matrix_UB_31      0.0313881000
_diffrn_orient_matrix_UB_32      0.0114108000
_diffrn_orient_matrix_UB_33      -0.0548881000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 2244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5295
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0342P)^2^+0.1433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                4998
_reflns_number_total             5295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5005995_si_002.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 4084362--4084367.cif.'
_cod_original_cell_volume        1353.72(14)
_cod_database_code               4084367
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.68
_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. Restrained distances
 C3A-C2 \\sim C3-C2 \\sim C4-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C3A)
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
 Fixed Sof: H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C3A(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B), C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
6.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)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), 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)
;
_shelx_res_checksum              15701
_shelx_hkl_checksum              16215