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_4089652
_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 H90 B2 K2 N6 P2 Si2'
_chemical_formula_sum            'C50 H90 B2 K2 N6 P2 Si2'
_chemical_formula_weight         993.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4801(12)
_cell_length_b                   48.364(4)
_cell_length_c                   10.4193(5)
_cell_measurement_reflns_used    5298
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      28.4629
_cell_measurement_theta_min      3.3631
_cell_volume                     11832.1(13)
_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
;
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 0.996
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
  1 omega  -51.00   22.50   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  -19.0000 -180.0000 98

  2 omega  -28.00   35.00   0.7500   15.0000
omega____ theta____ kappa____ phi______ frames
    -        9.9038  -38.0000   90.0000 84
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0073935000
_diffrn_orient_matrix_UB_12      0.0243843000
_diffrn_orient_matrix_UB_13      -0.0208548000
_diffrn_orient_matrix_UB_21      -0.0106199000
_diffrn_orient_matrix_UB_22      -0.0177918000
_diffrn_orient_matrix_UB_23      -0.0243794000
_diffrn_orient_matrix_UB_31      -0.0068984000
_diffrn_orient_matrix_UB_32      0.0012448000
_diffrn_orient_matrix_UB_33      0.0600311000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.818
_diffrn_reflns_point_group_measured_fraction_max 0.661
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.525
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71992
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1415 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4965
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0550P)^2^+28.8846P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.462
_reflns_Friedel_fraction_full    0.618
_reflns_Friedel_fraction_max     0.441
_reflns_number_gt                4454
_reflns_number_total             4965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om4011142_si_001.cif
_cod_data_source_block           5c_kji120003new
_cod_original_cell_volume        11832.1(12)
_cod_database_code               4089652
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C32 H44 B2 K2 P2 Si2'
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.55
_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. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(C2)=Sof(H1B)=Sof(H2)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H1B,H2), C2A(H2AA,H2AB), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B),
 C23(H23A,H23B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;