Synthesis and Structural Characterization of Phosphine‒Borane-Stabilized Dicarbanions with either Rigid or Flexible Spacers
Izod, Keith; Dixon, Casey M.; McMeekin, Emma; Rodgers, Lee; Harrington, Ross W.; Baisch, Ulrich; Organometallics 33 (2013) 378–; doi:10.1021/om4011142

data_4089649
_publ_section_title
;
 Synthesis and Structural Characterization of Phosphine--Borane-Stabilized
 Dicarbanions with either Rigid or Flexible Spacers
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              378
_journal_paper_doi               10.1021/om4011142
_journal_volume                  33
_journal_year                    2013
_chemical_formula_moiety         'C50 H102 B2 K2 N6 P2'
_chemical_formula_sum            'C50 H102 B2 K2 N6 P2'
_chemical_formula_weight         949.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.401(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8732(6)
_cell_length_b                   21.7626(7)
_cell_length_c                   14.3884(4)
_cell_measurement_reflns_used    11809
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.5000
_cell_measurement_theta_min      3.5000
_cell_volume                     5904.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.8513
_diffrn_measurement_details
;
  1 omega   -3.00   44.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819  -99.0000   30.0000 47

  2 omega   16.00   51.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819  -96.0000  -86.0000 35

  3 omega   25.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819 -133.0000   12.8373 44

  4 omega    6.00   35.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819  -99.0000    0.0000 29

  5 omega  -14.00   68.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819   57.0000  150.0000 82

  6 omega   37.00   66.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819   38.0000  -30.0000 29

  7 omega   15.00   41.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819  -99.0000 -150.0000 26

  8 omega  -16.00   13.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9819   38.0000   60.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0183654000
_diffrn_orient_matrix_UB_12      -0.0259456000
_diffrn_orient_matrix_UB_13      -0.0186174000
_diffrn_orient_matrix_UB_21      0.0325767000
_diffrn_orient_matrix_UB_22      -0.0160316000
_diffrn_orient_matrix_UB_23      -0.0024742000
_diffrn_orient_matrix_UB_31      -0.0040158000
_diffrn_orient_matrix_UB_32      -0.0114542000
_diffrn_orient_matrix_UB_33      0.0456536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.693
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.6850
_exptl_crystal_size_mid          0.2794
_exptl_crystal_size_min          0.1489
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         12984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+3.6093P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9745
_reflns_number_total             12984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4011142_si_001.cif
_cod_data_source_block           3d_kji130004_abs
_cod_database_code               4089649
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C50 H112 B2 K2 N6 P2'
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N65) = Uanis(N65A)
3. Others
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H64C)=
 Sof(H64D)=Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(H67C)=Sof(H67D)=Sof(N65)=1-FVAR(1)
 Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C63A)=Sof(H63C)=Sof(H63D)=
 Sof(H64A)=Sof(H64B)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(H67A)=Sof(H67B)=
 Sof(N65A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C21(H21), C22(H22), C28(H28), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
  C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C43(H43A,H43B), C44(H44A,H44B), C47(H47A,H47B), C48(H48A,H48B),
  C63(H63A,H63B), C63A(H63C,H63D), C64(H64C,H64D), C64(H64A,H64B), C67(H67C,
 H67D), C67(H67A,H67B), C68(H68A,H68B)
4.c Me refined with riding coordinates:
 C66(H66D,H66E,H66F), C66(H66A,H66B,H66C)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10)
4.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C62A(H62D,H62E,H62F), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C)
;