Unusual stability of the coordinated triethylborohydride anion in an alkaline-earth metal complex: crystallographic characterization of [Ca(HBEt3){1,2,4-C5(SiMe3)3H2}(thf)2]
Harvey, Melanie J.; Hanusa, Timothy P.; Pink, Maren; Chemical Communications  (2000) 489–; doi:10.1039/a908674i

data_7110782
_publ_section_title
;
 Unusual stability of the coordinated triethylborohydride anion in an
 alkaline-earth metal complex: crystallographic characterization of
 [Ca(HBEt3){1,2,4-C5(SiMe3)3H2}(thf)2]
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_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              489
_journal_paper_doi               10.1039/a908674i
_journal_year                    2000
_chemical_compound_source        'Prof. Timothy P. Hanusa, Vanderbilt U'
_chemical_formula_sum            'C28 H61 B Ca O2 Si3'
_chemical_formula_weight         564.93
_chemical_name_common            99141
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.306(2)
_cell_length_b                   9.9944(9)
_cell_length_c                   16.0091(15)
_cell_measurement_reflns_used    5521
_cell_measurement_temperature    173(2)
_cell_volume                     3569.0(6)
_computing_cell_refinement       'SAINT, Siemens'
_computing_data_collection       'SMART, Siemens'
_computing_data_reduction        'SAINT, Siemens'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'SMART CCD system, Siemens'
_diffrn_measurement_method       'area detector, omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24468
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.767612
_exptl_absorpt_correction_type   'SADABS, Sheldrick (1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.963
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.967
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         -0.147
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1316
_refine_ls_wR_factor_obs         0.1175
_reflns_number_observed          4440
_reflns_number_total             6321
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908674isup1.cif
_cod_data_source_block           99141n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3568.9(6)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7110782