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_7115291
_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         'C12 H14 Ge N2, 2(C F3 O3 S)'
_chemical_formula_sum            'C14 H14 F6 Ge N2 O6 S2'
_chemical_formula_weight         556.98
_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                110.4190(10)
_cell_angle_beta                 95.6880(10)
_cell_angle_gamma                95.4360(10)
_cell_formula_units_Z            2
_cell_length_a                   7.7487(2)
_cell_length_b                   11.1678(3)
_cell_length_c                   12.4220(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.46
_cell_measurement_theta_min      3.08
_cell_volume                     992.76(4)
_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 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       18
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         1.767
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.7825
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.292
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_refine_diff_density_max         0.789
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0418P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           JF0006_0m
_cod_database_code               7115291
_shelx_estimated_absorpt_t_min   0.582
_shelx_estimated_absorpt_t_max   0.740
_shelxl_version_number           2013-3
_shelx_res_checksum              38759