#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/46/4314612.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4314612
loop_
_publ_author_name
'Olga A. Egorova'
'Olga G. Tsay'
'Snehadrinarayan Khatua'
'Bhupal Meka'
'Nilkamal Maiti'
'Min-Kyu Kim'
'Seong Jung Kwon'
'Jung Oh Huh'
'Daniela Bucella'
'Sa-Ouk Kang'
'Juhyoun Kwak'
'David G. Churchill'
_publ_section_title
;
 Synthetic, Cyclic Voltammetric, Structural, EPR, and UV-Vis Spectroscopic
 Studies of Thienyl-Containing meso-A2B-cor(CrV=O) Systems: Consideration
 of Three Interrelated Molecular Detection Modalities
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              502
_journal_page_last               512
_journal_paper_doi               10.1021/ic9021432
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C35 H14 F10 N4 S'
_chemical_formula_weight         712.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.370(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4873(18)
_cell_length_b                   7.7533(8)
_cell_length_c                   25.313(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2830.8(6)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.1620
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14505
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0021(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.2130
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1072P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.2316
_reflns_number_gt                2505
_reflns_number_total             6390
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic9021432_si_002.cif
_cod_data_source_block           tpfps10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314612
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3363(4) -0.5070(7) 0.4847(2) 0.0341(13) Uani 1 1 d . . .
C2 C 0.2937(4) -0.4683(7) 0.5314(2) 0.0412(14) Uani 1 1 d . . .
H2B H 0.2979 -0.5330 0.5625 0.049 Uiso 1 1 calc R . .
C3 C 0.2456(4) -0.3187(7) 0.5224(2) 0.0393(14) Uani 1 1 d . . .
H3B H 0.2103 -0.2631 0.5462 0.047 Uiso 1 1 calc R . .
C4 C 0.2590(3) -0.2625(7) 0.4699(2) 0.0344(13) Uani 1 1 d . . .
C5 C 0.2353(3) -0.1096(7) 0.44169(19) 0.0324(13) Uani 1 1 d . . .
C6 C 0.2675(3) -0.0712(6) 0.39172(19) 0.0306(12) Uani 1 1 d . . .
C7 C 0.2569(3) 0.0808(7) 0.3613(2) 0.0349(13) Uani 1 1 d . . .
H7A H 0.2244 0.1788 0.3699 0.042 Uiso 1 1 calc R . .
C8 C 0.3020(4) 0.0592(7) 0.3175(2) 0.0365(13) Uani 1 1 d . . .
H8A H 0.3072 0.1416 0.2912 0.044 Uiso 1 1 calc R . .
C9 C 0.3404(3) -0.1105(7) 0.3179(2) 0.0324(13) Uani 1 1 d . . .
C10 C 0.3906(3) -0.1882(6) 0.27958(18) 0.0299(12) Uani 1 1 d . . .
C11 C 0.4322(3) -0.3538(6) 0.28321(18) 0.0301(12) Uani 1 1 d . . .
C12 C 0.4625(4) -0.4588(7) 0.2431(2) 0.0401(14) Uani 1 1 d . . .
H12A H 0.4566 -0.4320 0.2071 0.048 Uiso 1 1 calc R . .
C13 C 0.5015(4) -0.6049(7) 0.2644(2) 0.0377(13) Uani 1 1 d . . .
H13A H 0.5271 -0.6932 0.2456 0.045 Uiso 1 1 calc R . .
C14 C 0.4969(3) -0.6007(6) 0.3197(2) 0.0312(12) Uani 1 1 d . . .
C15 C 0.5289(3) -0.7229(6) 0.35884(19) 0.0289(12) Uani 1 1 d . . .
C16 C 0.4942(3) -0.7264(6) 0.4091(2) 0.0319(12) Uani 1 1 d . . .
C17 C 0.5220(4) -0.8054(7) 0.4586(2) 0.0356(13) Uani 1 1 d . . .
H17A H 0.5710 -0.8824 0.4652 0.043 Uiso 1 1 calc R . .
C18 C 0.4638(4) -0.7483(7) 0.4952(2) 0.0391(14) Uani 1 1 d . . .
H18A H 0.4668 -0.7811 0.5307 0.047 Uiso 1 1 calc R . .
C19 C 0.3994(4) -0.6325(7) 0.4699(2) 0.0336(13) Uani 1 1 d . . .
C21 C 0.1710(3) 0.0157(6) 0.46355(19) 0.0311(12) Uani 1 1 d . . .
C22 C 0.0861(4) 0.0569(7) 0.4363(2) 0.0381(14) Uani 1 1 d . . .
C23 C 0.0250(4) 0.1710(8) 0.4554(2) 0.0454(15) Uani 1 1 d . . .
C24 C 0.0450(4) 0.2438(7) 0.5049(2) 0.0448(15) Uani 1 1 d . . .
C25 C 0.1277(4) 0.2069(7) 0.5328(2) 0.0428(15) Uani 1 1 d . . .
C26 C 0.1893(4) 0.0972(7) 0.5118(2) 0.0390(14) Uani 1 1 d . . .
C31 C 0.4043(4) -0.0944(7) 0.2301(2) 0.0375(13) Uani 1 1 d . . .
C32 C 0.4965(3) -0.0743(6) 0.20829(18) 0.0248(11) Uiso 1 1 d . . .
H32 H 0.5540 -0.1130 0.2231 0.030 Uiso 1 1 calc R . .
C33 C 0.4762(5) 0.0182(8) 0.1593(2) 0.0581(18) Uani 1 1 d . . .
H33A H 0.5227 0.0438 0.1376 0.070 Uiso 1 1 calc R . .
C34 C 0.3886(5) 0.0662(8) 0.1460(2) 0.0578(18) Uani 1 1 d . . .
H34A H 0.3693 0.1264 0.1151 0.069 Uiso 1 1 calc R . .
C41 C 0.6015(4) -0.8458(6) 0.34602(19) 0.0309(12) Uani 1 1 d . . .
C42 C 0.6818(4) -0.7923(7) 0.3246(2) 0.0407(14) Uani 1 1 d . . .
C43 C 0.7492(4) -0.9015(8) 0.3106(2) 0.0497(16) Uani 1 1 d . . .
C44 C 0.7391(4) -1.0775(8) 0.3186(2) 0.0459(15) Uani 1 1 d . . .
C45 C 0.6625(4) -1.1347(7) 0.3406(2) 0.0389(14) Uani 1 1 d . . .
C46 C 0.5962(4) -1.0217(7) 0.3541(2) 0.0328(12) Uani 1 1 d . . .
N1 N 0.3137(3) -0.3822(5) 0.44833(17) 0.0379(11) Uani 1 1 d . . .
H1 H 0.3310 -0.3787 0.4167 0.046 Uiso 1 1 calc R . .
N2 N 0.3195(3) -0.1860(5) 0.36495(15) 0.0314(10) Uani 1 1 d . . .
N3 N 0.4507(3) -0.4484(5) 0.32946(15) 0.0334(11) Uani 1 1 d . . .
H3 H 0.4355 -0.4172 0.3601 0.040 Uiso 1 1 calc R . .
N4 N 0.4188(3) -0.6272(5) 0.41836(16) 0.0349(11) Uani 1 1 d . . .
H4 H 0.3873 -0.5682 0.3942 0.042 Uiso 1 1 calc R . .
F22 F 0.0599(2) -0.0201(4) 0.39014(12) 0.0523(9) Uani 1 1 d . . .
F23 F -0.0566(2) 0.2014(5) 0.42760(14) 0.0667(11) Uani 1 1 d . . .
F24 F -0.0164(2) 0.3461(4) 0.52566(14) 0.0671(11) Uani 1 1 d . . .
F25 F 0.1480(2) 0.2780(5) 0.58119(13) 0.0618(10) Uani 1 1 d . . .
F26 F 0.2723(2) 0.0704(4) 0.54106(12) 0.0515(9) Uani 1 1 d . . .
F42 F 0.6980(2) -0.6237(4) 0.31713(14) 0.0620(11) Uani 1 1 d . . .
F43 F 0.8244(2) -0.8447(5) 0.28989(16) 0.0765(12) Uani 1 1 d . . .
F44 F 0.8038(2) -1.1891(4) 0.30578(14) 0.0653(11) Uani 1 1 d . . .
F45 F 0.6523(2) -1.3041(4) 0.35061(13) 0.0588(10) Uani 1 1 d . . .
F46 F 0.5233(2) -1.0873(4) 0.37692(11) 0.0424(8) Uani 1 1 d . . .
S1 S 0.31651(12) 0.0055(2) 0.19135(7) 0.0613(5) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C19 115.9(4) . . ?
N1 C1 C2 108.6(5) . . ?
C19 C1 C2 135.3(5) . . ?
C3 C2 C1 107.3(5) . . ?
C2 C3 C4 107.6(5) . . ?
N1 C4 C5 119.5(4) . . ?
N1 C4 C3 107.4(4) . . ?
C5 C4 C3 132.8(5) . . ?
C4 C5 C6 122.8(5) . . ?
C4 C5 C21 119.5(4) . . ?
C6 C5 C21 117.6(5) . . ?
N2 C6 C7 107.9(4) . . ?
N2 C6 C5 122.8(5) . . ?
C7 C6 C5 129.3(5) . . ?
C8 C7 C6 108.0(5) . . ?
C7 C8 C9 109.0(5) . . ?
N2 C9 C10 125.6(4) . . ?
N2 C9 C8 106.2(4) . . ?
C10 C9 C8 128.1(5) . . ?
C9 C10 C11 126.1(4) . . ?
C9 C10 C31 119.7(4) . . ?
C11 C10 C31 114.2(4) . . ?
N3 C11 C12 104.8(4) . . ?
N3 C11 C10 125.5(4) . . ?
C12 C11 C10 129.6(4) . . ?
C13 C12 C11 110.1(5) . . ?
C12 C13 C14 108.7(5) . . ?
N3 C14 C13 105.3(4) . . ?
N3 C14 C15 125.1(4) . . ?
C13 C14 C15 129.5(5) . . ?
C16 C15 C14 121.5(4) . . ?
C16 C15 C41 120.4(4) . . ?
C14 C15 C41 118.1(4) . . ?
N4 C16 C15 119.9(4) . . ?
N4 C16 C17 104.9(4) . . ?
C15 C16 C17 135.1(5) . . ?
C18 C17 C16 108.2(5) . . ?
C17 C18 C19 108.6(5) . . ?
N4 C19 C18 105.6(4) . . ?
N4 C19 C1 115.5(5) . . ?
C18 C19 C1 137.7(5) . . ?
C26 C21 C22 115.0(5) . . ?
C26 C21 C5 123.6(5) . . ?
C22 C21 C5 121.4(5) . . ?
F22 C22 C23 117.1(5) . . ?
F22 C22 C21 119.8(5) . . ?
C23 C22 C21 123.0(5) . . ?
F23 C23 C22 119.8(6) . . ?
F23 C23 C24 120.3(5) . . ?
C22 C23 C24 119.7(5) . . ?
F24 C24 C25 120.5(6) . . ?
F24 C24 C23 120.5(6) . . ?
C25 C24 C23 118.9(5) . . ?
F25 C25 C24 119.3(5) . . ?
F25 C25 C26 120.6(6) . . ?
C24 C25 C26 120.1(5) . . ?
F26 C26 C25 117.0(5) . . ?
F26 C26 C21 119.8(5) . . ?
C25 C26 C21 123.2(5) . . ?
C10 C31 C32 123.9(4) . . ?
C10 C31 S1 123.7(4) . . ?
C32 C31 S1 112.4(4) . . ?
C33 C32 C31 104.5(4) . . ?
C34 C33 C32 118.0(5) . . ?
C33 C34 S1 112.6(5) . . ?
C46 C41 C42 114.3(5) . . ?
C46 C41 C15 123.6(5) . . ?
C42 C41 C15 122.1(5) . . ?
F42 C42 C43 115.3(5) . . ?
F42 C42 C41 120.6(5) . . ?
C43 C42 C41 124.1(5) . . ?
F43 C43 C42 122.1(5) . . ?
F43 C43 C44 119.0(5) . . ?
C42 C43 C44 119.0(5) . . ?
F44 C44 C45 120.3(5) . . ?
F44 C44 C43 121.0(5) . . ?
C45 C44 C43 118.7(5) . . ?
F45 C45 C44 120.2(5) . . ?
F45 C45 C46 119.0(5) . . ?
C44 C45 C46 120.8(5) . . ?
F46 C46 C45 117.5(5) . . ?
F46 C46 C41 119.4(5) . . ?
C45 C46 C41 123.1(5) . . ?
C1 N1 C4 109.1(4) . . ?
C6 N2 C9 108.8(4) . . ?
C11 N3 C14 110.9(4) . . ?
C19 N4 C16 112.6(4) . . ?
C34 S1 C31 92.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.354(6) . ?
C1 C19 1.409(7) . ?
C1 C2 1.418(7) . ?
C2 C3 1.362(7) . ?
C3 C4 1.431(7) . ?
C4 N1 1.366(6) . ?
C4 C5 1.409(7) . ?
C5 C6 1.420(7) . ?
C5 C21 1.488(7) . ?
C6 N2 1.383(6) . ?
C6 C7 1.408(7) . ?
C7 C8 1.350(7) . ?
C8 C9 1.428(7) . ?
C9 N2 1.385(6) . ?
C9 C10 1.402(7) . ?
C10 C11 1.418(7) . ?
C10 C31 1.478(7) . ?
C11 N3 1.386(6) . ?
C11 C12 1.404(7) . ?
C12 C13 1.355(7) . ?
C13 C14 1.408(7) . ?
C14 N3 1.391(6) . ?
C14 C15 1.417(7) . ?
C15 C16 1.412(7) . ?
C15 C41 1.478(7) . ?
C16 N4 1.374(6) . ?
C16 C17 1.417(7) . ?
C17 C18 1.384(7) . ?
C18 C19 1.405(7) . ?
C19 N4 1.361(6) . ?
C21 C26 1.379(7) . ?
C21 C22 1.389(7) . ?
C22 F22 1.336(6) . ?
C22 C23 1.371(7) . ?
C23 F23 1.338(6) . ?
C23 C24 1.382(8) . ?
C24 F24 1.336(6) . ?
C24 C25 1.362(8) . ?
C25 F25 1.351(6) . ?
C25 C26 1.375(7) . ?
C26 F26 1.367(6) . ?
C31 C32 1.500(7) . ?
C31 S1 1.716(5) . ?
C32 C33 1.439(7) . ?
C33 C34 1.336(8) . ?
C34 S1 1.689(6) . ?
C41 C46 1.382(7) . ?
C41 C42 1.392(7) . ?
C42 F42 1.344(6) . ?
C42 C43 1.364(7) . ?
C43 F43 1.328(6) . ?
C43 C44 1.389(8) . ?
C44 F44 1.338(6) . ?
C44 C45 1.362(8) . ?
C45 F45 1.349(6) . ?
C45 C46 1.367(7) . ?
C46 F46 1.350(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660954
