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_4512723
_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, C6 H4 S4, C2 H4 Cl2'
_chemical_formula_sum            'C26 H8 Cl2 F12 Hg3 S4'
_chemical_formula_weight         1349.31
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                76.545(4)
_cell_angle_beta                 83.377(4)
_cell_angle_gamma                82.796(4)
_cell_formula_units_Z            2
_cell_length_a                   7.476(2)
_cell_length_b                   13.463(4)
_cell_length_c                   16.074(5)
_cell_measurement_reflns_used    1610
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      23.55
_cell_measurement_theta_min      4.28
_cell_volume                     1554.8(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9940
_diffrn_measured_fraction_theta_max 0.9940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.1415
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15578
_diffrn_reflns_theta_full        24.9994
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.311
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.8818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1209.5958
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.2700
_refine_diff_density_min         -2.6417
_refine_diff_density_rms         0.5970
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             4.8611
_refine_ls_goodness_of_fit_ref   0.9912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.9888
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.0015
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+38.8991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                3612
_reflns_number_total             5431
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            cg501594t_si_001.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4512720--4512724.cif.'
_cod_database_code               4512723
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl1) = Uanis(Cl2) = Uanis(Cl1A) = Uanis(Cl2A)
Uanis(F5) = Uanis(F6) = Uanis(F7) = Uanis(F8)
Uanis(C21) = Uanis(C22)
Uanis(C19) = Uanis(C20)
Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
3. Others
 Sof(C25A)=Sof(H25c)=Sof(H25d)=Sof(C26A)=Sof(H26c)=Sof(H26d)=Sof(Cl1A)=
 Sof(Cl2A)=1-FVAR(1)
 Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(Cl1)=Sof(Cl2)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C26(H26a,H26b), C25A(H25c,H25d), C26A(H26c,H26d)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C23(H23), C24(H24)
;