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_4084363
_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 H44 B Li N2 P2'
_chemical_formula_sum            'C25 H44 B Li N2 P2'
_chemical_formula_weight         452.31
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 103.595(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7737(6)
_cell_length_b                   16.1992(6)
_cell_length_c                   15.1880(7)
_cell_measurement_reflns_used    5401
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5092
_cell_measurement_theta_min      2.7886
_cell_volume                     2815.6(2)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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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 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0422763000
_diffrn_orient_matrix_UB_12      0.0295503000
_diffrn_orient_matrix_UB_13      0.0207988000
_diffrn_orient_matrix_UB_21      0.0442701000
_diffrn_orient_matrix_UB_22      -0.0305835000
_diffrn_orient_matrix_UB_23      0.0054290000
_diffrn_orient_matrix_UB_31      0.0097896000
_diffrn_orient_matrix_UB_32      0.0104517000
_diffrn_orient_matrix_UB_33      -0.0429504000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16487
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.794
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97884
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0391P)^2^+0.9516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3811
_reflns_number_total             4941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5005995_si_002.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 4084362--4084367.cif.'
_cod_database_code               4084363
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C25 H44 B Li P2 N2'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.967
_reflns_odcompleteness_completeness 99.79
_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.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
2.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)
2.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)
;
_shelx_res_checksum              11990
_shelx_hkl_checksum              76761