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_4512722
_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'
_chemical_formula_sum            'C24 H4 F12 Hg3 S4'
_chemical_formula_weight         1250.28
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.743(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.292(2)
_cell_length_b                   42.819(14)
_cell_length_c                   17.234(6)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      19.991
_cell_measurement_theta_min      4.278
_cell_volume                     5370(3)
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.1558
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30814
_diffrn_reflns_theta_full        24.78
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         4.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.526
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0939 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.7272.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4480
_exptl_crystal_recrystallization_method
'Slow evaporation in a 1:1 mixture of dichlromethane and dichloroethane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.173
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.433
_refine_ls_extinction_coef       0.00140(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.1563
_refine_ls_R_factor_gt           0.0945
_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^)+(0.0604P)^2^+88.0365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1886
_reflns_number_gt                5540
_reflns_number_total             8890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501594t_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4512720--4512724.cif.'
_cod_original_cell_volume        5369(3)
_cod_database_code               4512722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) =
Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C42) =
Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15) = Uanis(C14) = Uanis(C13)
Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C31) = Uanis(C20) = Uanis(C21) =
Uanis(C22) = Uanis(C23) = Uanis(C1C) = Uanis(C19) = Uanis(C34) = Uanis(C33) =
Uanis(C32) = Uanis(C30) = Uanis(C35) = Uanis(C29) = Uanis(C24) = Uanis(C25)
Uanis(C43) = Uanis(C1) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) =
Uanis(C40) = Uanis(C41) = Uanis(C39) = Uanis(C38) = Uanis(C36) = Uanis(C37)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C36(H36), C47(H47), C46(H46), C37(H37), C43(H43), C41(H41), C40(H40)
;