Alkaline Earth Metal Complexes of a Phosphine-Borane-Stabilized Carbanion: Synthesis, Structures, and Stabilities
Keith Izod; Corinne Wills; William Clegg; Ross W. Harrington; Inorganic Chemistry 46 (2007) 4320–4325; doi:10.1021/ic062459l

data_4307975
_publ_section_title
;
Alkaline Earth Metal Complexes of a Phosphine-Borane-Stabilized
Carbanion: Synthesis, Structures, and Stabilities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4320
_journal_page_last               4325
_journal_paper_doi               10.1021/ic062459l
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H54 B2 Mg P2 Si4'
_chemical_formula_sum            'C18 H54 B2 Mg P2 Si4'
_chemical_formula_weight         490.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.972(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.800(2)
_cell_length_b                   8.9292(13)
_cell_length_c                   44.332(7)
_cell_measurement_reflns_used    9207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.6
_cell_volume                     6208.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            22041
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.106
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+21.1477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                10211
_reflns_number_total             10685
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic062459l-file002_1.cif
_cod_data_source_block           ki256_compound_3
_cod_original_cell_volume        6208.3(16)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4307975