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_4085574
_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         'C80 H164 B4 K2 O6 P4 Si8 Sr3, C4 H10 O'
_chemical_formula_sum            'C84 H174 B4 K2 O7 P4 Si8 Sr3'
_chemical_formula_weight         2029.12
_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
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Olex2 1.2-alpha
(compiled 2014.11.07 svn.r3078 for OlexSys, GUI svn.r4941)
;
_cell_angle_alpha                69.048(3)
_cell_angle_beta                 79.922(3)
_cell_angle_gamma                77.400(3)
_cell_formula_units_Z            1
_cell_length_a                   13.3139(4)
_cell_length_b                   13.8721(4)
_cell_length_c                   17.1954(6)
_cell_measurement_reflns_used    13573
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      28.9550
_cell_measurement_theta_min      2.9120
_cell_volume                     2878.00(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'XT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0426724000
_diffrn_orient_matrix_UB_12      0.0254143000
_diffrn_orient_matrix_UB_13      -0.0212327000
_diffrn_orient_matrix_UB_21      -0.0345001000
_diffrn_orient_matrix_UB_22      0.0471346000
_diffrn_orient_matrix_UB_23      -0.0169742000
_diffrn_orient_matrix_UB_31      0.0017331000
_diffrn_orient_matrix_UB_32      0.0147821000
_diffrn_orient_matrix_UB_33      0.0351338000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51004
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.680
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         14316
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0383P)^2^+1.7842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10434
_reflns_number_total             14316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501183p_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085571--4085574.cif.'
_cod_original_cell_volume        2878.00(18)
_cod_database_code               4085574
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C84 H174 P4 B4 Sr3 Si8 O7 K2'
_reflns_odcompleteness_completeness 99.86
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C23A-C24A = C23-C24 = C26A-C25A = C26-C25
 1.54 with sigma of 0.02
 Si4-C14B \\sim Si4-C14A \\sim Si4-C13A \\sim Si4-C13B \\sim Si4-C12A \\sim
Si4-C12B
 with sigma of 0.02
 C14B-C13A \\sim C14A-C13B \\sim C13A-C12A \\sim C13B-C12B \\sim C12A-C14B
\\sim C12B-C14A
 with sigma of 0.02
 B2-H2B \\sim B2-H2C \\sim B2-H2D \\sim B1-H1A \\sim B1-H1B \\sim B1-H1C
 with sigma of 0.02
 H1A-H1C \\sim H2C-H2D \\sim H2D-H2B \\sim H1B-H1C \\sim H1A-H1B \\sim H2B-H2C
 with sigma of 0.02
 C2SA-C3S \\sim C2S-C3S
 with sigma of 0.02
 O1S-C2SA \\sim O1S-C2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13B) = Uanis(C13A)
Uanis(C12B) = Uanis(C12A)
Uanis(C14A) = Uanis(C14B)
Uanis(C20) = Uanis(C20A)
Uanis(C15) = Uanis(C15A)
Uanis(C2S) = Uanis(C2SA)
Uanis(C24) = Uanis(C24A)
Uanis(C23) = Uanis(C23A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
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: C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5) C12B(0.5) H12G(0.5)
 H12H(0.5) H12I(0.5) C13A(0.5) H13D(0.5) H13E(0.5) H13F(0.5) C13B(0.5)
 H13G(0.5) H13H(0.5) H13I(0.5) C14B(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
 C14A(0.5) H14G(0.5) H14H(0.5) H14I(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C23(0.5) H23A(0.5) H23B(0.5) C23A(0.5)
 H23C(0.5) H23D(0.5) C25(0.5) H25A(0.5) H25B(0.5) C25A(0.5) H25C(0.5) H25D(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C26A(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
 H19A(0.5) H19B(0.5) H19C(0.5) H19D(0.5) C20(0.5) H20A(0.5) H20B(0.5) C20A(0.5)
 H20C(0.5) H20D(0.5) H21A(0.5) H21B(0.5) H21C(0.5) H21D(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) C15A(0.5) H15C(0.5) H15D(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 H16D(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) C2SA(0.5) H2SC(0.5) H2SD(0.5) H3SD(0.5)
 H3SE(0.5) H3SF(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C7(H7), C7A(H7A), C11A(H11A)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23A(H23C,H23D), C25(H25A,H25B), C25A(H25C,H25D), C19(H19A,
 H19B), C19(H19C,H19D), C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,H21B),
 C21(H21C,H21D), C22(H22A,H22B), C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,
 H16B), C16(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B), C2S(H2SA,H2SB),
 C2SA(H2SC,H2SD)
6.c Me refined with riding coordinates:
 C3S(H3SD,H3SE,H3SF), C3S(H3SA,H3SB,H3SC)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C2A(H2A), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,
 H10F), C8A(H8AA,H8AB,H8AC), C12A(H12D,H12E,H12F), C12B(H12G,H12H,H12I),
 C13A(H13D,H13E,H13F), C13B(H13G,H13H,H13I), C14B(H14D,H14E,H14F), C14A(H14G,
 H14H,H14I), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F), C26(H26A,H26B,H26C),
 C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              82754
_shelx_hkl_checksum              20396
_olex2_submission_special_instructions 'No special instructions were received'