Exploring structural trends for complexes of Me2E(OSO2CF3)2 (E = Si, Ge, Sn) with pyridine derivatives
Alasdair P. M. Robertson; Jordan N. Friedmann; Hilary A. Jenkins; Neil Burford; Chem.Commun. 50 (2014) 7979–; doi:10.1039/C4CC01109K

data_7115289
_publ_section_title
;
 Exploring structural trends for complexes of Me2E(OSO2CF3)2 (E = Si, Ge,
 Sn) with pyridine derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              7979
_journal_paper_doi               10.1039/C4CC01109K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C13 H14 F3 N2 O3 S Si, C F3 O3 S'
_chemical_formula_sum            'C14 H14 F6 N2 O6 S2 Si'
_chemical_formula_weight         512.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 118.801(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1596(18)
_cell_length_b                   22.794(3)
_cell_length_c                   7.3679(9)
_cell_measurement_reflns_used    6972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.91
_cell_volume                     2083.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.758
_diffrn_reflns_theta_min         1.787
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_correction_T_min  0.9087
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
; 
 Flack x determined using 2424 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.005(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.1622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5301
_reflns_number_total             5944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01109k2.cif
_cod_data_source_block           JF0004_0m
_cod_database_code               7115289
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2013-3
_shelx_res_checksum              57715