Stabilization of Low Valent Silicon Fluorides in the Coordination Sphere of Transition Metals
Ramachandran Azhakar; Rajendra S. Ghadwal; Herbert W. Roesky; Hilke Wolf; Dietmar Stalke; Journal of the American Chemical Society 134 (2012) 2423–2428; doi:10.1021/ja210697p

data_4117397
_publ_section_title
;
 Stabilization of Low Valent Silicon Fluorides in the Coordination Sphere
 of Transition Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2423
_journal_page_last               2428
_journal_paper_doi               10.1021/ja210697p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C20 H23 Cl Mo N2 O5 Si'
_chemical_formula_sum            'C20 H23 Cl Mo N2 O5 Si'
_chemical_formula_weight         530.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   9.791(2)
_cell_length_b                   13.307(2)
_cell_length_c                   18.432(2)
_cell_measurement_reflns_used    3431
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      2.22
_cell_volume                     2401.5(7)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.5608
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17349
_diffrn_reflns_theta_full        20.09
_diffrn_reflns_theta_max         20.09
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.044
_exptl_absorpt_correction_T_max  0.7490
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.095(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                3998
_reflns_number_total             4609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210697p_si_003.cif
_cod_data_source_block           rh
_cod_database_code               4117397