Structural Diversity in Alkaline Earth Metal Complexes of a Phosphine-Borane-Stabilized 1,3-Dicarbanion
Izod, Keith; Wills, Corinne; El-Hamruni, Salima; Harrington, Ross W.; Waddell, Paul G.; Probert, Michael R.; Organometallics 34 (2015) 2406–; doi:10.1021/om501183p

data_4085573
_publ_section_title
;
 Structural Diversity in Alkaline Earth Metal Complexes of a
 Phosphine-Borane-Stabilized 1,3-Dicarbanion
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2406
_journal_paper_doi               10.1021/om501183p
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C22 H46.8 B Ba O2 P Si2'
_chemical_formula_sum            'C22 H47 B Ba O2 P Si2'
_chemical_formula_weight         578.89
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.11.20 svn.r3094 for OlexSys, GUI svn.r4947)
;
_cell_angle_alpha                100.457(3)
_cell_angle_beta                 103.592(3)
_cell_angle_gamma                116.449(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8258(3)
_cell_length_b                   11.8510(4)
_cell_length_c                   14.1952(4)
_cell_measurement_reflns_used    7669
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      29.6013
_cell_measurement_theta_min      2.9367
_cell_volume                     1496.77(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
  1 omega  -41.00  -10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.8627   77.0000   60.0000 31

  2 omega   -7.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.5815   77.0000  120.0000 98

  3 omega  -15.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.5815   77.0000    0.0000 106

  4 omega   -5.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.5815   77.0000 -120.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0697973491
_diffrn_orient_matrix_UB_12      -0.0510827915
_diffrn_orient_matrix_UB_13      -0.0369930109
_diffrn_orient_matrix_UB_21      -0.0319844006
_diffrn_orient_matrix_UB_22      -0.0015982234
_diffrn_orient_matrix_UB_23      0.0383755273
_diffrn_orient_matrix_UB_31      -0.0158676997
_diffrn_orient_matrix_UB_32      0.0490592770
_diffrn_orient_matrix_UB_33      -0.0113280588
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13108
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.671
_diffrn_reflns_theta_min         2.944
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
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    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7008
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5137
_reflns_number_total             7008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501183p_si_001.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4085571--4085574.cif.'
_cod_original_cell_volume        1496.77(9)
_cod_database_code               4085573
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C14 H28 B Ba P si2'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.650
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O1-C17 \\sim O1-C17A \\sim O1-C15 \\sim O1-C15A \\sim O2A-C21 \\sim O2A-C19
 with sigma of 0.02
 C20-C19 \\sim C22-C21 \\sim C16-C15 \\sim C16A-C15A \\sim C18-C17 \\sim
C18A-C17A
 with sigma of 0.02
 C22A-C21A \\sim C22A-C20A \\sim C20A-C19A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C15A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C16) = Uanis(C16A)
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: C15(0.7) H15A(0.7) H15B(0.7) C16(0.7) H16A(0.7) H16B(0.7)
 H16C(0.7) C17(0.7) H17A(0.7) H17B(0.7) C18(0.7) H18A(0.7) H18B(0.7) H18C(0.7)
 C19(0.4) H19A(0.4) H19B(0.4) C19A(0.6) H19C(0.6) H19D(0.6) C20A(0.6) H20A(0.6)
 H20B(0.6) C20(0.4) H20C(0.4) H20D(0.4) H20E(0.4) C21A(0.6) H21A(0.6) H21B(0.6)
 C22A(0.6) H22A(0.6) H22B(0.6) C15A(0.3) H15C(0.3) H15D(0.3) C17A(0.3)
 H17C(0.3) H17D(0.3) C18A(0.3) H18D(0.3) H18E(0.3) H18F(0.3) C16A(0.3)
 H16D(0.3) H16E(0.3) H16F(0.3) C21(0.4) H21C(0.4) H21D(0.4) C22(0.4) H22C(0.4)
 H22D(0.4) H22E(0.4)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C11(H11)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C19A(H19C,H19D), C20A(H20A,
 H20B), C21A(H21A,H21B), C22A(H22A,H22B), C15A(H15C,H15D), C17A(H17C,H17D),
 C21(H21C,H21D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20C,H20D,H20E), C18A(H18D,H18E,H18F), C16A(H16D,H16E,H16F),
 C22(H22C,H22D,H22E)
;
_shelx_res_checksum              85554
_shelx_hkl_checksum              6817
_olex2_submission_special_instructions 'No special instructions were received'