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_7115288
_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         'C16 H26 N4 Si, 2(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C20 H30 Cl4 F6 N4 O6 S2 Si'
_chemical_formula_weight         770.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                95.057(2)
_cell_angle_beta                 98.939(2)
_cell_angle_gamma                108.631(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1122(4)
_cell_length_b                   11.4867(6)
_cell_length_c                   18.7960(9)
_cell_measurement_reflns_used    6468
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.07
_cell_measurement_theta_min      4.11
_cell_volume                     1621.66(14)
_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 0.977
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART6K CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17672
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    5.574
_exptl_absorpt_correction_T_max  0.4629
_exptl_absorpt_correction_T_min  0.1285
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.724
_exptl_crystal_size_mid          0.571
_exptl_crystal_size_min          0.312
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5782
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.454
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4973
_reflns_number_total             5782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc01109k2.cif
_cod_data_source_block           JF1_0m
_cod_database_code               7115288
_shelx_estimated_absorpt_t_min   0.107
_shelx_estimated_absorpt_t_max   0.275
_shelxl_version_number           2013-3
_shelx_res_checksum              54282