Trimethylsilylated Allyl Complexes of the Heavy Alkali Metals, M[1,3-(SiMe3)2C3H3](thf)n(M = K, Cs)
Quisenberry, Keith T.; Gren, Cameron K.; White, Rosemary E.; Hanusa, Timothy P.; Brennessel, William W.; Organometallics 26 (2007) 4354–; doi:10.1021/om700410a

data_4073509
_publ_section_title
;
 Trimethylsilylated Allyl Complexes of the Heavy Alkali Metals,
 M[1,3-(SiMe3)2C3H3](thf)n(M = K, Cs)
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4354
_journal_paper_doi               10.1021/om700410a
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C30 H66 K2 O3 Si4'
_chemical_formula_sum            'C30 H66 K2 O3 Si4'
_chemical_formula_weight         665.39
_chemical_name_common            04224
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.151(2)
_cell_length_b                   11.0862(9)
_cell_length_c                   16.9491(14)
_cell_measurement_reflns_used    3185
_cell_measurement_temperature    173(2)
_cell_volume                     4350.1(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31324
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_correction_T_min  0.8438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.174
_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   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7483
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+1.0073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                6288
_reflns_number_total             7483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700410a-file003.cif
_cod_data_source_block           04224
_cod_original_sg_symbol_H-M      Pna2~1~
_cod_database_code               4073509