Coordination Chemistry of Anticrowns. Synthesis and Structures of Double-Decker Sandwich Complexes of the Three-Mercury Anticrown (o-C6F4Hg)3with Halide Anions Containing and Not Containing Coordinated Dibromomethane Molecules
Tugashov, Kirill I.; Gribanyov, Dmitry A.; Dolgushin, Fedor M.; Smol’yakov, Alexander F.; Peregudov, Alexander S.; Minacheva, Marija Kh.; Tikhonova, Irina A.; Shur, Vladimir B.; Organometallics 35 (2016) 2197–; doi:10.1021/acs.organomet.6b00231

data_4086616
_publ_section_title
;
 Coordination Chemistry of Anticrowns. Synthesis and Structures of
 Double-Decker Sandwich Complexes of the Three-Mercury Anticrown
 (o-C6F4Hg)3with Halide Anions Containing and Not Containing Coordinated
 Dibromomethane Molecules
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2197
_journal_paper_doi               10.1021/acs.organomet.6b00231
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C36 Br F24 Hg6, C16 H36 N, 2(C H2 Br2)'
_chemical_formula_sum            'C54 H40 Br5 F24 Hg6 N'
_chemical_formula_weight         2761.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.9460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4130(8)
_cell_length_b                   16.6253(8)
_cell_length_c                   23.5287(12)
_cell_measurement_reflns_used    7483
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.35
_cell_volume                     6358.7(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0846
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79797
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.623
_exptl_absorpt_coefficient_mu    17.683
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.885
_exptl_crystal_description       prism
_exptl_crystal_F_000             4968
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.956
_refine_diff_density_min         -2.520
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         18509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12027
_reflns_number_total             18509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00231_si_002.cif
_cod_data_source_block           sada
_cod_database_code               4086616
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.143
_shelx_estimated_absorpt_t_max   0.225
_shelx_res_checksum              49954
_shelx_hkl_checksum              74041