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_4086617
_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 F24 Hg6 I, C24 H20 P'
_chemical_formula_sum            'C60 H20 F24 Hg6 I P'
_chemical_formula_weight         2558.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7987(17)
_cell_length_b                   27.770(3)
_cell_length_c                   11.7368(11)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      2.54
_cell_volume                     5801.1(10)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0791
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            56614
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.359
_exptl_absorpt_coefficient_mu    16.499
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_description       prism
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.821
_refine_diff_density_min         -2.175
_refine_diff_density_rms         0.322
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.214(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         12556
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0366P)^2^+145.2516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10942
_reflns_number_total             12556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00231_si_002.cif
_cod_data_source_block           a
_cod_original_cell_volume        5801.1(9)
_cod_database_code               4086617
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.077
_shelx_estimated_absorpt_t_max   0.438
_shelx_res_checksum              91435
_shelx_hkl_checksum              24349