Trimethylsilylmethylcalcium Iodide, an Easily Accessible Grignard-Type Reagent of a Heavy Alkaline Earth Metal
Köhler, Mathias; Koch, Alexander; Görls, Helmar; Westerhausen, Matthias; Organometallics 35 (2016) 242–; doi:10.1021/acs.organomet.5b00956

data_4086388
_publ_section_title
;
 Trimethylsilylmethylcalcium Iodide, an Easily Accessible Grignard-Type
 Reagent of a Heavy Alkaline Earth Metal
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              242
_journal_paper_doi               10.1021/acs.organomet.5b00956
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety
'0.98 (C24 H51 Ca I O4 Si) * 0.02 (C20 H40 O4 Ca I2)'
_chemical_formula_sum            'C23.92 H50.77 Ca I1.02 O4 Si0.98'
_chemical_formula_weight         599.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 100.715(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6823(3)
_cell_length_b                   17.4313(3)
_cell_length_c                   10.0658(2)
_cell_measurement_temperature    133(2)
_cell_volume                     3048.44(10)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21354
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.3674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                6483
_reflns_number_total             6928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00956_si_001.cif
_cod_data_source_block           FO5728
_cod_depositor_comments          'Adding full bibliography for 4086388.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4086388