Structural Diversity in the Complexes of Trimeric Perfluoro-o-phenylene Mercury with Tetrathia- and Tetramethyltetraselenafulvalene
Castañeda, Raúl; Yakovenko, Andrey A.; Draguta, Sergiu; Fonari, Marina S.; Antipin, Mikhail Yu.; Timofeeva, Tatiana V.; Crystal Growth & Design 15 (2015) 1022–; doi:10.1021/cg501594t

data_4512724
_publ_section_title
;
 Structural Diversity in the Complexes of Trimeric Perfluoro-o-phenylene
 Mercury with Tetrathia- and Tetramethyltetraselenafulvalene
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1022
_journal_paper_doi               10.1021/cg501594t
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C18 F12 Hg3, C10 H12 Se4'
_chemical_formula_sum            'C28 H12 F12 Hg3 Se4'
_chemical_formula_weight         1493.99
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                83.635(4)
_cell_angle_beta                 83.177(4)
_cell_angle_gamma                85.072(4)
_cell_formula_units_Z            2
_cell_length_a                   7.686(3)
_cell_length_b                   11.779(4)
_cell_length_c                   17.472(6)
_cell_measurement_reflns_used    5180
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.740
_cell_measurement_theta_min      4.106
_cell_volume                     1556.7(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17944
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         4.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.528
_exptl_absorpt_correction_T_max  0.0542
_exptl_absorpt_correction_T_min  0.0170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0916 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.3137.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method
'Liquid-liquid difussion of ethyl acetate on carbon disulfide'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.077
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                6689
_reflns_number_total             8980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501594t_si_001.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4512720--4512724.cif.'
_cod_original_cell_volume        1556.6(9)
_cod_database_code               4512724
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;