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_4089646
_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         'C29 H64 B2 K N3 P2'
_chemical_formula_sum            'C29 H64 B2 K N3 P2'
_chemical_formula_weight         577.49
_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             2013-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.357(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4751(10)
_cell_length_b                   11.6808(5)
_cell_length_c                   19.7554(9)
_cell_measurement_reflns_used    7550
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      28.6634
_cell_measurement_theta_min      2.9259
_cell_volume                     3564.3(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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      150.15
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -84.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.0288  -38.0000   60.0000 102

  2 omega   -3.00   23.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.0288   38.0000   30.0000 26

  3 omega   -2.00   25.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.0288  -83.0000  -65.0000 27

  4 omega  -69.00   20.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257  -77.0000   60.0000 89

  5 omega   -6.00   19.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        9.8257   83.0000 -114.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0326079000
_diffrn_orient_matrix_UB_12      0.0136380000
_diffrn_orient_matrix_UB_13      0.0334388000
_diffrn_orient_matrix_UB_21      -0.0235412000
_diffrn_orient_matrix_UB_22      0.0494189000
_diffrn_orient_matrix_UB_23      0.0029290000
_diffrn_orient_matrix_UB_31      -0.0222245000
_diffrn_orient_matrix_UB_32      -0.0325423000
_diffrn_orient_matrix_UB_33      0.0183984000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.8179P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4907
_reflns_number_total             6260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4011142_si_001.cif
_cod_data_source_block           1c_ki486
_cod_database_code               4089646
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C40 H50 K P2 B2 N3'
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.926
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.034) H4(0.039) H5(0.039) H6(0.034) H9(0.032) H10A(0.053)
 H10B(0.053) H10C(0.053) H11A(0.05) H11B(0.05) H11C(0.05) H12(0.033)
 H13A(0.054) H13B(0.054) H13C(0.054) H14A(0.053) H14B(0.053) H14C(0.053)
 H15(0.058) H16A(0.096) H16B(0.096) H16C(0.096) H17A(0.129) H17B(0.129)
 H17C(0.129) H18(0.037) H19A(0.072) H19B(0.072) H19C(0.072) H20A(0.064)
 H20B(0.064) H20C(0.064) H21A(0.099) H21B(0.099) H21C(0.099) H22A(0.104)
 H22B(0.104) H22C(0.104) H23A(0.043) H23B(0.043) H24A(0.039) H24B(0.039)
 H25A(0.085) H25B(0.085) H25C(0.085) H26A(0.046) H26B(0.046) H27A(0.053)
 H27B(0.053) H28A(0.085) H28B(0.085) H28C(0.085) H29A(0.1) H29B(0.1) H29C(0.1)
 H23C(0.056) H23D(0.056) H24C(0.05) H24D(0.05)
 Fixed X: H3(0.6978) H4(0.8416) H5(0.9211) H6(0.8566) H9(0.4206) H10A(0.3788)
 H10B(0.4707) H10C(0.4659) H11A(0.3346) H11B(0.4215) H11C(0.3844) H12(0.5215)
 H13A(0.5003) H13B(0.5422) H13C(0.4514) H14A(0.6401) H14B(0.6719) H14C(0.6815)
 H15(0.7368) H16A(0.6356) H16B(0.5938) H16C(0.6105) H17A(0.7892) H17B(0.7739)
 H17C(0.8456) H18(0.5853) H19A(0.6038) H19B(0.6558) H19C(0.7066) H20A(0.5822)
 H20B(0.6836) H20C(0.6172) H21A(0.8643) H21B(0.8326) H21C(0.9242) H22A(0.9771)
 H22B(1.0401) H22C(1.0226) H23A(1.0036) H23B(0.9921) H24A(0.8427) H24B(0.913)
 H25A(0.7392) H25B(0.7744) H25C(0.7369) H26A(0.9668) H26B(0.9054) H27A(0.815)
 H27B(0.912) H28A(0.9763) H28B(0.9857) H28C(0.9429) H29A(0.7622) H29B(0.8199)
 H29C(0.8533) H23C(0.8558) H23D(0.9574) H24C(0.9874) H24D(0.9369)
 Fixed Y: H3(-0.178) H4(-0.2341) H5(-0.183) H6(-0.0834) H9(-0.0093)
 H10A(0.1069) H10B(0.0481) H10C(0.18) H11A(0.1619) H11B(0.2236) H11C(0.1157)
 H12(0.1089) H13A(-0.0666) H13B(-0.1326) H13C(-0.0681) H14A(0.043) H14B(0.124)
 H14C(-0.0119) H15(-0.1183) H16A(-0.2666) H16B(-0.1425) H16C(-0.1902) H17A(-
 0.2865) H17B(-0.2415) H17C(-0.1824) H18(0.0418) H19A(0.1442) H19B(0.0258)
 H19C(0.143) H20A(0.2425) H20B(0.2449) H20C(0.1902) H21A(0.0489) H21B(0.1635)
 H21C(0.1084) H22A(0.0519) H22B(0.1157) H22C(0.1698) H23A(0.3262) H23B(0.2932)
 H24A(0.3606) H24B(0.4609) H25A(0.4748) H25B(0.535) H25C(0.4074) H26A(0.4737)
 H26B(0.5745) H27A(0.5546) H27B(0.5704) H28A(0.3411) H28B(0.42) H28C(0.2957)
 H29A(0.4641) H29B(0.3695) H29C(0.499) H23C(0.2923) H23D(0.2818) H24C(0.3839)
 H24D(0.4584)
 Fixed Z: H3(0.9012) H4(0.9356) H5(0.8619) H6(0.7564) H9(0.752) H10A(0.647)
 H10B(0.6599) H10C(0.6802) H11A(0.7468) H11B(0.7969) H11C(0.8268) H12(0.9141)
 H13A(0.9591) H13B(0.9083) H13C(0.8735) H14A(1.011) H14B(0.9598) H14C(0.9562)
 H15(0.5274) H16A(0.5289) H16B(0.5063) H16C(0.586) H17A(0.587) H17B(0.6582)
 H17C(0.6321) H18(0.5476) H19A(0.4517) H19B(0.4633) H19C(0.4916) H20A(0.552)
 H20B(0.5981) H20C(0.6319) H21A(0.9334) H21B(0.961) H21C(1.0067) H22A(0.8901)
 H22B(0.9605) H22C(0.8823) H23A(0.9263) H23B(1.0013) H24A(0.9503) H24B(0.9626)
 H25A(0.7956) H25B(0.8732) H25C(0.8655) H26A(0.8497) H26B(0.8583) H27A(0.7397)
 H27B(0.7412) H28A(0.7745) H28B(0.7114) H28C(0.693) H29A(0.6277) H29B(0.607)
 H29C(0.6213) H23C(0.9711) H23D(1.0181) H24C(0.927) H24D(0.9678)
;