#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:34:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179413 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/10/4331094.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_4331094
loop_
_publ_author_name
'Ashley M. McDaniel'
'Anthony K. Rappé'
'Matthew P. Shores'
_publ_section_title
;
 Structural and Electronic Comparison of 1st Row Transition Metal
 Complexes of a Tripodal Iminopyridine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12493
_journal_page_last               12502
_journal_paper_doi               10.1021/ic301909u
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H33 F6 N7 O12 S2 Zn'
_chemical_formula_weight         951.14
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'Bruker SHELXTL'
_audit_update_record
;
2012-01-31 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.042(2)
_cell_length_b                   10.042(2)
_cell_length_c                   35.268(9)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.41
_cell_volume                     3080.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19212
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plates
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2979
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0423
_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)+(0.0957P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                2735
_reflns_number_total             2979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301909u_si_002_6.cif
_cod_data_source_block           msn301
_cod_original_cell_volume        3079.8(12)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4331094
#BEGIN Tags that were not found in dictionaries:
_publcif_info_exptl_table_max_cols 6
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Zn1 Zn 0.0000 0.0000 0.319360(10) 0.05000(18) Uani 1 3 d S
O1 O -0.3396(5) 0.0989(5) 0.48059(9) 0.0978(11) Uani 1 1 d .
N1 N 0.0000 0.0000 0.24297(13) 0.0677(13) Uani 1 3 d S
C1 C 0.1260(5) -0.0238(6) 0.23259(11) 0.0728(10) Uani 1 1 d .
H1C H 0.2197 0.0749 0.2303 0.087 Uiso 1 1 calc R
H1D H 0.1049 -0.0751 0.2082 0.087 Uiso 1 1 calc R
N2 N 0.1703(3) -0.0453(3) 0.29965(8) 0.0555(6) Uani 1 1 d .
O2 O -0.2735(5) -0.0800(5) 0.46766(9) 0.0928(10) Uani 1 1 d .
C2 C 0.1483(6) -0.1214(5) 0.26251(12) 0.0712(10) Uani 1 1 d .
H2A H 0.0587 -0.2237 0.2633 0.085 Uiso 1 1 calc R
H2B H 0.2374 -0.1306 0.2563 0.085 Uiso 1 1 calc R
N3 N -0.1164(3) 0.0881(3) 0.36268(8) 0.0486(6) Uani 1 1 d .
C3 C 0.2878(4) -0.0091(4) 0.31928(10) 0.0599(8) Uani 1 1 d .
H3A H 0.3611 -0.0334 0.3110 0.072 Uiso 1 1 calc R
C4 C -0.0719(4) 0.2366(4) 0.35537(9) 0.0510(6) Uani 1 1 d .
C5 C -0.0969(5) 0.3268(4) 0.38074(10) 0.0616(8) Uani 1 1 d .
H5A H -0.0676 0.4280 0.3747 0.074 Uiso 1 1 calc R
C6 C -0.1663(4) 0.2647(4) 0.41539(11) 0.0637(8) Uani 1 1 d .
H6A H -0.1825 0.3241 0.4330 0.076 Uiso 1 1 calc R
C7 C -0.2102(3) 0.1153(4) 0.42306(8) 0.0516(7) Uani 1 1 d .
C8 C -0.1860(4) 0.0276(4) 0.39566(9) 0.0500(6) Uani 1 1 d .
H8A H -0.2194 -0.0753 0.4007 0.060 Uiso 1 1 calc R
C9 C -0.2817(5) 0.0460(5) 0.46024(10) 0.0653(8) Uani 1 1 d .
C10 C -0.3488(11) -0.1600(10) 0.50256(17) 0.123(2) Uani 1 1 d .
H10A H -0.3363 -0.2482 0.5057 0.184 Uiso 1 1 calc R
H10B H -0.4563 -0.1926 0.5013 0.184 Uiso 1 1 calc R
H10C H -0.3033 -0.0919 0.5237 0.184 Uiso 1 1 calc R
S1 S 0.3333 -0.3333 0.36423(6) 0.0699(5) Uani 1 3 d S
F1 F 0.1955(4) -0.4355(5) 0.43009(12) 0.1175(11) Uani 1 1 d .
O3 O 0.4814(4) -0.2039(4) 0.35487(13) 0.0959(11) Uani 1 1 d .
C11 C 0.3333 -0.3333 0.4161(3) 0.085(2) Uani 1 3 d S
S2 S -0.5704(5) -0.2491(5) 0.59154(13) 0.0919(11) Uani 0.33 1 d P
F2 F -0.8165(7) -0.3325(8) 0.6306(2) 0.181(3) Uani 1 1 d .
O4 O -0.5162(9) -0.3404(11) 0.5739(2) 0.181(3) Uani 1 1 d .
C12 C -0.7329(11) -0.4031(11) 0.6116(2) 0.0470(17) Uani 0.33 1 d P
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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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
N2 Zn1 N2 109.56(8) 3 2
N2 Zn1 N2 109.56(8) 3 .
N2 Zn1 N2 109.56(8) 2 .
N2 Zn1 N3 155.66(10) 3 3
N2 Zn1 N3 91.02(10) 2 3
N2 Zn1 N3 73.66(10) . 3
N2 Zn1 N3 73.66(10) 3 2
N2 Zn1 N3 155.66(10) 2 2
N2 Zn1 N3 91.02(10) . 2
N3 Zn1 N3 82.25(10) 3 2
N2 Zn1 N3 91.02(10) 3 .
N2 Zn1 N3 73.66(10) 2 .
N2 Zn1 N3 155.66(10) . .
N3 Zn1 N3 82.25(10) 3 .
N3 Zn1 N3 82.25(10) 2 .
C1 N1 C1 113.83(19) 3 2
C1 N1 C1 113.83(19) 3 .
C1 N1 C1 113.83(19) 2 .
N1 C1 C2 110.5(3) . .
N1 C1 H1C 109.5 . .
C2 C1 H1C 109.5 . .
N1 C1 H1D 109.5 . .
C2 C1 H1D 109.5 . .
H1C C1 H1D 108.1 . .
C3 N2 C2 121.0(3) . .
C3 N2 Zn1 120.4(2) . .
C2 N2 Zn1 118.6(2) . .
C9 O2 C10 115.3(5) . .
N2 C2 C1 108.2(3) . .
N2 C2 H2A 110.1 . .
C1 C2 H2A 110.1 . .
N2 C2 H2B 110.1 . .
C1 C2 H2B 110.1 . .
H2A C2 H2B 108.4 . .
C8 N3 C4 118.5(3) . .
C8 N3 Zn1 129.8(2) . .
C4 N3 Zn1 109.9(2) . .
N2 C3 C4 119.4(3) . 3
N2 C3 H3A 120.3 . .
C4 C3 H3A 120.3 3 .
N3 C4 C5 122.1(3) . .
N3 C4 C3 115.5(3) . 2
C5 C4 C3 122.4(3) . 2
C4 C5 C6 119.3(3) . .
C4 C5 H5A 120.3 . .
C6 C5 H5A 120.3 . .
C7 C6 C5 118.8(3) . .
C7 C6 H6A 120.6 . .
C5 C6 H6A 120.6 . .
C6 C7 C8 119.4(3) . .
C6 C7 C9 120.3(3) . .
C8 C7 C9 120.3(3) . .
N3 C8 C7 121.8(3) . .
N3 C8 H8A 119.1 . .
C7 C8 H8A 119.1 . .
O1 C9 O2 125.1(4) . .
O1 C9 C7 123.1(4) . .
O2 C9 C7 111.8(3) . .
O2 C10 H10A 109.5 . .
O2 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O2 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O3 S1 O3 114.91(16) 2_545 .
O3 S1 O3 114.91(16) 2_545 3_655
O3 S1 O3 114.91(16) . 3_655
O3 S1 C11 103.2(2) 2_545 .
O3 S1 C11 103.2(2) . .
O3 S1 C11 103.2(2) 3_655 .
F1 C11 F1 107.2(5) 3_655 .
F1 C11 F1 107.2(5) 3_655 2_545
F1 C11 F1 107.2(5) . 2_545
F1 C11 S1 111.6(5) 3_655 .
F1 C11 S1 111.6(5) . .
F1 C11 S1 111.6(5) 2_545 .
C12 S2 C12 65.6(11) 2_455 3_445
C12 S2 O4 79.7(7) 2_455 .
C12 S2 O4 138.0(7) 3_445 .
C12 S2 F2 66.5(6) 2_455 3_445
C12 S2 F2 66.9(5) 3_445 3_445
O4 S2 F2 120.6(6) . 3_445
C12 S2 O4 133.1(8) 2_455 2_455
C12 S2 O4 70.1(6) 3_445 2_455
O4 S2 O4 129.2(7) . 2_455
F2 S2 O4 109.2(5) 3_445 2_455
C12 S2 S2 81.4(6) 2_455 2_455
O4 S2 S2 115.2(5) . 2_455
F2 S2 S2 106.4(4) 3_445 2_455
O4 S2 S2 54.1(4) 2_455 2_455
C12 S2 S2 47.4(6) 2_455 3_445
C12 S2 S2 77.1(5) 3_445 3_445
O4 S2 S2 61.8(5) . 3_445
F2 S2 S2 113.1(3) 3_445 3_445
O4 S2 S2 108.4(4) 2_455 3_445
S2 S2 S2 60.000(4) 2_455 3_445
O4 S2 C12 95.5(5) . .
F2 S2 C12 89.5(4) 3_445 .
O4 S2 C12 94.5(5) 2_455 .
C12 F2 C12 47.4(8) 3_445 .
C12 F2 S2 45.6(4) . 2_455
S2 O4 S2 64.2(4) . 3_445
S2 C12 S2 93.1(8) 3_445 2_455
S2 C12 C12 105.0(7) 3_445 3_445
S2 C12 C12 50.7(7) 2_455 3_445
S2 C12 C12 63.7(9) 3_445 2_455
S2 C12 C12 95.6(7) 2_455 2_455
C12 C12 C12 60.000(10) 3_445 2_455
S2 C12 F2 73.7(7) 3_445 2_455
S2 C12 F2 162.9(9) 2_455 2_455
C12 C12 F2 121.5(8) 3_445 2_455
C12 C12 F2 69.0(9) 2_455 2_455
S2 C12 F2 160.5(10) 3_445 .
S2 C12 F2 67.5(6) 2_455 .
C12 C12 F2 63.6(9) 3_445 .
C12 C12 F2 116.7(8) 2_455 .
F2 C12 F2 125.5(9) 2_455 .
S2 C12 O4 61.7(6) 3_445 3_445
S2 C12 O4 66.3(6) 2_455 3_445
C12 C12 O4 115.3(7) 3_445 3_445
C12 C12 O4 120.7(5) 2_455 3_445
F2 C12 O4 114.3(8) 2_455 3_445
F2 C12 O4 107.3(7) . 3_445
S2 C12 S2 63.8(5) 3_445 .
S2 C12 S2 62.2(5) 2_455 .
F2 C12 S2 101.6(6) 2_455 .
F2 C12 S2 105.0(6) . .
O4 C12 S2 99.1(6) 3_445 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N2 2.095(3) 3
Zn1 N2 2.095(3) 2
Zn1 N2 2.095(3) .
Zn1 N3 2.348(3) 3
Zn1 N3 2.348(3) 2
Zn1 N3 2.348(3) .
O1 C9 1.202(5) .
N1 C1 1.447(5) 3
N1 C1 1.447(5) 2
N1 C1 1.447(5) .
C1 C2 1.530(7) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
N2 C3 1.255(5) .
N2 C2 1.476(5) .
O2 C9 1.334(6) .
O2 C10 1.458(6) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
N3 C8 1.337(4) .
N3 C4 1.350(4) .
C3 C4 1.468(5) 3
C3 H3A 0.9300 .
C4 C5 1.383(5) .
C4 C3 1.468(5) 2
C5 C6 1.390(5) .
C5 H5A 0.9300 .
C6 C7 1.363(5) .
C6 H6A 0.9300 .
C7 C8 1.408(4) .
C7 C9 1.490(5) .
C8 H8A 0.9300 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
S1 O3 1.441(3) 2_545
S1 O3 1.441(3) .
S1 O3 1.441(3) 3_655
S1 C11 1.829(11) .
F1 C11 1.338(5) .
C11 F1 1.338(5) 3_655
C11 F1 1.338(5) 2_545
S2 O4 1.422(8) .
S2 F2 1.506(7) 3_445
S2 O4 1.546(7) 2_455
S2 S2 1.579(8) 2_455
S2 S2 1.579(8) 3_445
S2 C12 1.741(10) .
F2 C12 1.439(10) 3_445
F2 C12 1.501(10) .
F2 S2 1.506(7) 2_455
O4 S2 1.546(7) 3_445
O4 C12 1.588(11) 2_455
C12 F2 1.439(10) 2_455
C12 O4 1.588(11) 3_445
#BEGIN Loops that were not found in dictionaries:
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
msn235 y y y
msn279 y y y
msn285 y y y
msn226_c y y y
msn284 y y y
msn301 y y y
#END Loops that were not found in dictionaries
