#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:08:57 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232195 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/71/4347162.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_4347162
loop_
_publ_author_name
'Gómez, Manuel'
'Hernández-Prieto, Cristina'
'Martín, Avelino'
'Mena, Miguel'
'Santamaría, Cristina'
_publ_section_title
;
 Systematic Approach for the Construction of Niobium and Tantalum Sulfide
 Clusters.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3815
_journal_page_last               3821
_journal_paper_doi               10.1021/acs.inorgchem.5b02816
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H56 Cl4 N8 S4 Ta4'
_chemical_formula_sum            'C36 H56 Cl4 N8 S4 Ta4'
_chemical_formula_weight         1594.72
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-06-01T15:12:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.542(4)
_cell_length_b                   17.542(3)
_cell_length_c                   23.549(3)
_cell_measurement_reflns_used    136
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     7247(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31863
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.241
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.322
_exptl_absorpt_correction_T_max  0.243
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.25
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+245.6880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0
_reflns_number_gt                2335
_reflns_number_total             3271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02816_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        7247(3)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4347162
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.6842(7) 0.4653(6) 0.4213(5) 0.051(3) Uani 1 1 d . .
C2 C 0.7489(8) 0.4571(8) 0.4640(6) 0.070(4) Uani 1 1 d . .
H2A H 0.7277 0.4455 0.5015 0.105 Uiso 1 1 calc R U
H2B H 0.7778 0.5048 0.4658 0.105 Uiso 1 1 calc R U
H2C H 0.7827 0.4156 0.452 0.105 Uiso 1 1 calc R U
C3 C 0.6334(9) 0.5306(8) 0.4392(8) 0.085(5) Uani 1 1 d . .
H3A H 0.5893 0.5334 0.4137 0.128 Uiso 1 1 calc R U
H3B H 0.662 0.5784 0.4373 0.128 Uiso 1 1 calc R U
H3C H 0.6158 0.5221 0.4782 0.128 Uiso 1 1 calc R U
C4 C 0.7146(8) 0.4778(8) 0.3615(6) 0.067(4) Uani 1 1 d . .
H4A H 0.7507 0.4371 0.352 0.101 Uiso 1 1 calc R U
H4B H 0.7406 0.5272 0.3596 0.101 Uiso 1 1 calc R U
H4C H 0.6722 0.4772 0.3345 0.101 Uiso 1 1 calc R U
C11 C 0.6035(8) 0.2409(8) 0.5524(6) 0.061(3) Uani 1 1 d . .
H11 H 0.6146 0.1934 0.5348 0.073 Uiso 1 1 calc R U
C12 C 0.6032(9) 0.2468(9) 0.6106(6) 0.075(4) Uani 1 1 d . .
H12 H 0.6156 0.2033 0.6329 0.09 Uiso 1 1 calc R U
C13 C 0.5856(9) 0.3138(10) 0.6372(6) 0.079(5) Uani 1 1 d . .
H13 H 0.5849 0.3174 0.6775 0.095 Uiso 1 1 calc R U
C14 C 0.5692(8) 0.3744(8) 0.6045(6) 0.064(4) Uani 1 1 d . .
H14 H 0.5566 0.4217 0.6218 0.077 Uiso 1 1 calc R U
C15 C 0.5705(7) 0.3690(7) 0.5468(5) 0.056(3) Uani 1 1 d . .
H15 H 0.5588 0.4126 0.5245 0.067 Uiso 1 1 calc R U
Cl1 Cl 0.71609(17) 0.23456(17) 0.44215(14) 0.0571(8) Uani 1 1 d . .
N1 N 0.6417(5) 0.3951(5) 0.4229(4) 0.045(2) Uani 1 1 d . .
N11 N 0.5882(5) 0.3023(5) 0.5204(4) 0.047(2) Uani 1 1 d . .
S1 S 0.53630(16) 0.15859(16) 0.42878(12) 0.0446(6) Uani 1 1 d . .
Ta1 Ta 0.60053(3) 0.30371(3) 0.42244(2) 0.04262(17) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 -3 0.137
3 0 1 0.133
-8 0 -7 0.136
-5 0 6 0.122
0 -9 -10 0.121
1 -14 17 0.189
0 5 6 0.211
-1 15 -17 0.151
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
N1 C1 C3 109.6(11) . .
N1 C1 C4 109.2(10) . .
C3 C1 C4 110.8(12) . .
N1 C1 C2 106.7(10) . .
C3 C1 C2 109.1(11) . .
C4 C1 C2 111.3(11) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N11 C11 C12 119.9(13) . .
N11 C11 H11 120 . .
C12 C11 H11 120 . .
C13 C12 C11 121.4(14) . .
C13 C12 H12 119.3 . .
C11 C12 H12 119.3 . .
C14 C13 C12 117.8(13) . .
C14 C13 H13 121.1 . .
C12 C13 H13 121.1 . .
C13 C14 C15 120.8(13) . .
C13 C14 H14 119.6 . .
C15 C14 H14 119.6 . .
N11 C15 C14 121.3(13) . .
N11 C15 H15 119.4 . .
C14 C15 H15 119.4 . .
C1 N1 Ta1 172.8(8) . .
C11 N11 C15 118.8(11) . .
C11 N11 Ta1 123.3(8) . .
C15 N11 Ta1 117.8(8) . .
Ta1 S1 Ta1 94.61(10) 11_666 6_554
Ta1 S1 Ta1 87.50(9) 11_666 .
Ta1 S1 Ta1 98.26(9) 6_554 .
N1 Ta1 N11 92.5(4) . .
N1 Ta1 Cl1 96.5(3) . .
N11 Ta1 Cl1 83.2(2) . .
N1 Ta1 S1 98.5(3) . 16_656
N11 Ta1 S1 167.9(2) . 16_656
Cl1 Ta1 S1 100.54(11) . 16_656
N1 Ta1 S1 98.8(3) . 6_554
N11 Ta1 S1 81.6(2) . 6_554
Cl1 Ta1 S1 158.80(11) . 6_554
S1 Ta1 S1 91.66(10) 16_656 6_554
N1 Ta1 S1 176.6(3) . .
N11 Ta1 S1 84.2(2) . .
Cl1 Ta1 S1 82.52(9) . .
S1 Ta1 S1 84.86(9) 16_656 .
S1 Ta1 S1 81.37(9) 6_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.440(14) .
C1 C3 1.511(17) .
C1 C4 1.521(17) .
C1 C2 1.522(18) .
C2 H2A 0.98 .
C2 H2B 0.98 .
C2 H2C 0.98 .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C4 H4A 0.98 .
C4 H4B 0.98 .
C4 H4C 0.98 .
C11 N11 1.340(15) .
C11 C12 1.376(18) .
C11 H11 0.95 .
C12 C13 1.37(2) .
C12 H12 0.95 .
C13 C14 1.35(2) .
C13 H13 0.95 .
C14 C15 1.363(18) .
C14 H14 0.95 .
C15 N11 1.360(15) .
C15 H15 0.95 .
Cl1 Ta1 2.408(3) .
N1 Ta1 1.759(9) .
N11 Ta1 2.318(10) .
S1 Ta1 2.409(3) 11_666
S1 Ta1 2.494(3) 6_554
S1 Ta1 2.788(3) .
Ta1 S1 2.409(3) 16_656
Ta1 S1 2.494(3) 6_554
