The structures of three Hg~2~<i>X</i>~4~<i>L</i>~2~ macrocycles {<i>X</i> = Cl, Br and I, and <i>L</i> = 1,2-bis[4-(pyridin-3-yl)phenoxy]ethane} assembled from ether-bridged dipyridyl ligands
Wu, Dan; Qin, Na; Liu, Qi-Kui; Ma, Jian-Ping; Dong, Yu-Bin; Acta Crystallographica Section C 68 (2012) m156–m160; doi:10.1107/S0108270112019075

data_2018500
_publ_section_title
;
 The structures of three Hg~2~<i>X</i>~4~<i>L</i>~2~ macrocycles {<i>X</i>
 = Cl, Br and I, and <i>L</i> = 1,2-bis[4-(pyridin-3-yl)phenoxy]ethane}
 assembled from ether-bridged dipyridyl ligands
;
_journal_coeditor_code           GZ3208
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m156
_journal_page_last               m160
_journal_paper_doi               10.1107/S0108270112019075
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Hg2 Br4 (C24 H20 N2 O2)2]'
_chemical_formula_moiety         'C48 H40 Br4 Hg2 N4 O4'
_chemical_formula_sum            'C48 H40 Br4 Hg2 N4 O4'
_chemical_formula_weight         1457.66
_chemical_name_systematic
;
bis{\m-1,2-bis[4-(pyridin-3-yl)phenoxy]ethane-
\k^2^<i>N</i>:<i>N</i>'}bis[dibromidomercury(II)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.812(5)
_cell_angle_beta                 78.764(5)
_cell_angle_gamma                81.635(5)
_cell_formula_units_Z            1
_cell_length_a                   9.021(4)
_cell_length_b                   11.096(4)
_cell_length_c                   11.914(5)
_cell_measurement_reflns_used    2261
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.178
_cell_measurement_theta_min      2.320
_cell_volume                     1149.2(8)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6112
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    10.198
_exptl_absorpt_correction_T_max  0.3507
_exptl_absorpt_correction_T_min  0.3100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                3491
_reflns_number_total             4234
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3208.cif
_cod_data_source_block           II
_cod_original_cell_volume        1149.1(8)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               2018500
_cod_database_fobs_code          2018500