#------------------------------------------------------------------------------
#$Date: 2017-02-10 18:21:58 +0200 (Fri, 10 Feb 2017) $
#$Revision: 191977 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/94/2009405.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009405
loop_
_publ_author_name
'Gallagher, John F.'
'Alyea, Elmer C.'
'Ferguson, George'
'Xu Zheng'
_publ_section_title
;
 Structure of the copper tripodal Schiff base complex
 {tris[4-(2-thienyl)-3-aza-κN-3-butenyl]amine-κN}copper(I)
 tetrafluoroborate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              16
_journal_page_last               18
_journal_paper_doi               10.1107/S0108270193007176
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C21 H24 Cu N4 S3 1+, B1 F4 1-'
_chemical_formula_sum            'C21 H24 B Cu F4 N4 S3'
_chemical_formula_weight         578.97
_chemical_name_systematic
;
{Tris-[4-(2-thienyl)-3-aza-3-butenyl]amine}copper(I) tetrafluoroborate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8400(10)
_cell_length_b                   19.5920(10)
_cell_length_c                   17.7160(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      9.0
_cell_volume                     5150.8(5)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
'NRCVAX DATRD2 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics    'NRCVAX and ORTEPII (Johnson, 1976)'
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5313
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.14
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.29
_refine_ls_goodness_of_fit_obs   1.30
_refine_ls_hydrogen_treatment    'H atoms riding, C-H 0.95 \%A'
_refine_ls_matrix_type           block-diagonal
_refine_ls_number_parameters     341
_refine_ls_number_reflns         1857
_refine_ls_R_factor_all          0.155
_refine_ls_R_factor_obs          0.040
_refine_ls_shift/esd_max         0.02
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0006F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.066
_refine_ls_wR_factor_obs         0.047
_reflns_number_observed          1857
_reflns_number_total             5313
_reflns_observed_criterion       I~net~>3.0\s(I~net~)
_cod_data_source_file            mu1057.cif
_cod_data_source_block           Copper-Schiff-Base
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 40 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F) + 0.0006F^2^]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(F) +
0.0006F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5151.0(10)
_cod_database_code               2009405
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2-x,1/2+y,z
1/2+x,1/2-y,-z
x,-y,1/2+z
-x,y,1/2-z
1/2-x,1/2-y,1/2+z
1/2+x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu 0.18341(5) 0.18869(3) 0.12864(4) 0.0624(4) Uani d . 1 Cu
S(1) 0.12831(12) 0.30464(9) 0.00619(11) 0.0880(12) Uani d . 1 S
S(2) -0.01836(12) 0.16134(9) 0.05648(12) 0.0903(12) Uani d . 1 S
S(3) 0.19997(12) 0.13855(9) -0.04645(12) 0.0910(12) Uani d . 1 S
N(1) 0.1321(3) 0.2698(2) 0.1793(3) 0.067(3) Uani d . 1 N
N(2) 0.1395(3) 0.0950(2) 0.1521(3) 0.065(3) Uani d . 1 N
N(3) 0.3114(3) 0.1939(2) 0.0917(3) 0.071(3) Uani d . 1 N
N(4) 0.2552(3) 0.1769(2) 0.2429(3) 0.074(3) Uani d . 1 N
C(11) 0.2227(5) 0.2346(3) 0.2864(4) 0.093(5) Uani d . 1 C
C(12) 0.1293(5) 0.2556(3) 0.2611(4) 0.091(5) Uani d . 1 C
C(13) 0.1157(4) 0.3315(3) 0.1594(4) 0.070(4) Uani d . 1 C
C(14) 0.1168(4) 0.3554(3) 0.0825(4) 0.067(4) Uani d . 1 C
C(15) 0.1031(4) 0.4240(3) 0.0596(4) 0.084(5) Uani d . 1 C
C(16) 0.1013(5) 0.4295(3) -0.0173(5) 0.116(6) Uani d . 1 C
C(17) 0.1142(4) 0.3707(4) -0.0545(4) 0.096(5) Uani d . 1 C
C(21) 0.2244(4) 0.1100(3) 0.2689(4) 0.089(5) Uani d . 1 C
C(22) 0.2080(4) 0.0635(3) 0.2023(4) 0.088(5) Uani d . 1 C
C(23) 0.0720(4) 0.0591(3) 0.1347(4) 0.075(4) Uani d . 1 C
C(24) -0.0030(4) 0.0808(3) 0.0885(3) 0.070(4) Uani d . 1 C
C(25) -0.0718(4) 0.0389(3) 0.0660(4) 0.101(5) Uani d . 1 C
C(26) -0.1355(5) 0.0737(4) 0.0227(4) 0.111(6) Uani d . 1 C
C(27) -0.1155(4) 0.1387(4) 0.0123(4) 0.105(5) Uani d . 1 C
C(31) 0.3518(4) 0.1805(3) 0.2247(4) 0.090(5) Uani d . 1 C
C(32) 0.3667(4) 0.2225(3) 0.1535(4) 0.088(5) Uani d . 1 C
C(33) 0.3539(4) 0.1685(3) 0.0346(4) 0.081(4) Uani d . 1 C
C(34) 0.3131(4) 0.1390(3) -0.0310(4) 0.074(4) Uani d . 1 C
C(35) 0.3578(4) 0.1068(3) -0.0894(4) 0.085(5) Uani d . 1 C
C(36) 0.2994(5) 0.0830(3) -0.1436(4) 0.101(5) Uani d . 1 C
C(37) 0.2145(5) 0.0964(3) -0.1293(4) 0.095(5) Uani d . 1 C
H(11A) 0.221 0.222 0.338 0.1029 Uiso calc RT 1 H
H(11B) 0.263 0.272 0.280 0.1029 Uiso calc RT 1 H
H(12A) 0.111 0.295 0.288 0.1010 Uiso calc RT 1 H
H(12B) 0.088 0.220 0.271 0.1010 Uiso calc RT 1 H
H(13) 0.102 0.364 0.198 0.0802 Uiso calc RT 1 H
H(15) 0.096 0.461 0.093 0.0940 Uiso calc RT 1 H
H(16) 0.092 0.472 -0.042 0.1264 Uiso calc RT 1 H
H(17) 0.115 0.367 -0.108 0.1065 Uiso calc RT 1 H
H(21A) 0.269 0.090 0.301 0.0988 Uiso calc RT 1 H
H(21B) 0.170 0.115 0.296 0.0988 Uiso calc RT 1 H
H(22A) 0.187 0.021 0.220 0.0976 Uiso calc RT 1 H
H(22B) 0.263 0.057 0.175 0.0976 Uiso calc RT 1 H
H(23) 0.070 0.014 0.154 0.0848 Uiso calc RT 1 H
H(25) -0.076 -0.008 0.078 0.1111 Uiso calc RT 1 H
H(26) -0.188 0.053 0.003 0.1210 Uiso calc RT 1 H
H(27) -0.151 0.169 -0.017 0.1151 Uiso calc RT 1 H
H(31A) 0.383 0.201 0.266 0.1003 Uiso calc RT 1 H
H(31B) 0.374 0.136 0.217 0.1003 Uiso calc RT 1 H
H(32A) 0.429 0.221 0.140 0.0979 Uiso calc RT 1 H
H(32B) 0.349 0.268 0.162 0.0979 Uiso calc RT 1 H
H(33) 0.418 0.170 0.036 0.0913 Uiso calc RT 1 H
H(35) 0.421 0.102 -0.092 0.0951 Uiso calc RT 1 H
H(36) 0.319 0.059 -0.187 0.1111 Uiso calc RT 1 H
H(37) 0.166 0.084 -0.162 0.1052 Uiso calc RT 1 H
B(1) 0.0000 0.5120(5) 0.2500 0.085(8) Uani d S 1 B
F(11) 0.0000 0.4441(3) 0.2500 0.164(6) Uani d S 1 F
F(12) 0.0037(8) 0.5461(5) 0.1891(5) 0.155(8) Uani d . 0.5 F
F(13) 0.0905(6) 0.5090(5) 0.2209(6) 0.157(8) Uani d . 0.5 F
F(14) -0.0510(7) 0.5391(4) 0.1973(5) 0.149(7) Uani d . 0.5 F
B(21) 0.5000 0.3207(13) 0.2500 0.11(2) Uani d S 0.5 B
B(22) 0.5000 0.3738(7) 0.2500 0.077(14) Uani d S 0.5 B
F(21) 0.5000 0.4310(4) 0.2500 0.317(15) Uani d S 1 F
F(22) 0.4602(6) 0.3244(4) 0.2893(6) 0.148(9) Uani d . 0.5 F
F(23) 0.4075(6) 0.3883(5) 0.2173(6) 0.145(7) Uani d . 0.5 F
F(24) 0.4966(9) 0.3722(7) 0.3243(8) 0.230(12) Uani d . 0.5 F
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
B 0.000 0.001 'International Tables Vol. IV Table 2.2B'
N 0.004 0.003 'International Tables Vol. IV Table 2.2B'
O 0.008 0.006 'International Tables Vol. IV Table 2.2B'
F 0.014 0.010 'International Tables Vol. IV Table 2.2B'
S 0.110 0.124 'International Tables Vol. IV Table 2.2B'
Cu 0.263 1.266 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
7 2 1
4 8 2
7 2 6
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) Cu N(2) 121.34(19) yes
N(1) Cu N(3) 118.08(19) yes
N(1) Cu N(4) 81.93(18) yes
N(2) Cu N(3) 115.05(19) yes
N(2) Cu N(4) 82.64(17) yes
N(3) Cu N(4) 81.63(19) yes
C(14) S(1) C(17) 92.6(3) no
C(24) S(2) C(27) 91.5(3) no
C(34) S(3) C(37) 90.9(3) no
Cu N(1) C(12) 107.8(3) yes
Cu N(1) C(13) 134.9(4) yes
C(12) N(1) C(13) 116.2(5) no
Cu N(2) C(22) 106.5(3) yes
Cu N(2) C(23) 136.3(4) yes
C(22) N(2) C(23) 117.2(4) no
Cu N(3) C(32) 107.5(4) yes
Cu N(3) C(33) 134.2(4) yes
C(32) N(3) C(33) 117.0(5) no
Cu N(4) C(11) 115.3(5) yes
Cu N(4) C(21) 113.7(5) yes
Cu N(4) C(31) 114.7(4) yes
C(11) N(4) C(21) 115.3(5) no
C(11) N(4) C(31) 113.7(5) no
C(21) N(4) C(31) 114.7(4) no
N(4) C(11) C(12) 111.1(5) no
N(1) C(12) C(11) 108.4(5) no
N(1) C(13) C(14) 124.3(5) no
S(1) C(14) C(13) 124.6(4) no
S(1) C(14) C(15) 110.1(5) no
C(13) C(14) C(15) 125.2(5) no
C(14) C(15) C(16) 111.3(6) no
C(15) C(16) C(17) 114.8(6) no
S(1) C(17) C(16) 111.2(6) no
N(4) C(21) C(22) 110.2(5) no
N(2) C(22) C(21) 109.1(5) no
N(2) C(23) C(24) 125.8(5) no
S(2) C(24) C(23) 124.6(4) no
S(2) C(24) C(25) 111.1(5) no
C(23) C(24) C(25) 124.2(5) no
C(24) C(25) C(26) 111.9(6) no
C(25) C(26) C(27) 113.3(6) no
S(2) C(27) C(26) 112.2(5) no
N(4) C(31) C(32) 110.5(5) no
N(3) C(32) C(31) 109.2(5) no
N(3) C(33) C(34) 125.7(5) no
S(3) C(34) C(33) 123.4(5) no
S(3) C(34) C(35) 110.6(5) no
C(33) C(34) C(35) 126.1(5) no
C(34) C(35) C(36) 112.0(6) no
C(35) C(36) C(37) 113.8(6) no
S(3) C(37) C(36) 112.7(5) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu N(1) . . 1.977(4) yes
Cu N(2) . . 1.992(4) yes
Cu N(3) . . 2.012(5) yes
Cu N(4) . . 2.300(5) yes
S(1) C(14) . . 1.687(6) no
S(1) C(17) . . 1.695(6) no
S(2) C(24) . . 1.693(6) no
S(2) C(27) . . 1.699(7) no
S(3) C(34) . . 1.701(6) no
S(3) C(37) . . 1.698(7) no
N(1) C(12) . . 1.477(8) no
N(1) C(13) . . 1.284(7) no
N(2) C(22) . . 1.486(7) no
N(2) C(23) . . 1.262(7) no
N(3) C(32) . . 1.479(8) no
N(3) C(33) . . 1.291(9) no
N(4) C(11) . . 1.450(8) no
N(4) C(21) . . 1.461(8) no
N(4) C(31) . . 1.471(9) no
C(11) C(12) . . 1.513(10) no
C(13) C(14) . . 1.441(9) no
C(14) C(15) . . 1.419(8) no
C(15) C(16) . . 1.366(11) no
C(16) C(17) . . 1.342(11) no
C(21) C(22) . . 1.512(10) no
C(23) C(24) . . 1.445(9) no
C(24) C(25) . . 1.369(8) no
C(25) C(26) . . 1.395(10) no
C(26) C(27) . . 1.322(11) no
C(31) C(32) . . 1.522(9) no
C(33) C(34) . . 1.433(9) no
C(34) C(35) . . 1.382(9) no
C(35) C(36) . . 1.375(10) no
C(36) C(37) . . 1.312(10) no
B(1) F(11) . . 1.331(12) no
B(1) F(12) . . 1.270(9) no
B(1) F(13) . . 1.440(8) no
B(1) F(14) . . 1.315(8) no
B(21) F(22) . . 0.916(10) no
B(21) F(23) . . 1.993(19) no
B(21) F(24) . . 1.66(2) no
B(22) F(21) . . 1.122(16) no
B(22) F(22) . . 1.330(13) no
B(22) F(23) . . 1.517(9) no
B(22) F(24) . . 1.318(14) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
Cu S(1) 3.246(2) yes
Cu S(2) 3.300(2) yes
Cu S(3) 3.263(2) yes
S(1) S(2) 3.662(3) yes
S(1) S(3) 3.548(3) yes
S(2) S(3) 3.745(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
N(4) Cu N(1) C(12) -28.7(3) yes
N(4) Cu N(1) C(13) 138.3(4) yes
N(4) Cu N(2) C(22) -26.6(3) yes
N(4) Cu N(2) C(23) 154.0(4) yes
N(4) Cu N(3) C(32) -28.8(3) yes
N(4) Cu N(3) C(33) 137.8(4) yes
N(2) Cu N(1) C(12) 47.8(3) no
N(2) Cu N(1) C(13) -145.2(4) no
N(3) Cu N(1) C(12) -104.6(4) no
N(3) Cu N(1) C(13) 62.4(3) no
N(1) Cu N(2) C(22) -102.6(4) no
N(1) Cu N(2) C(23) 78.0(4) no
N(3) Cu N(2) C(22) 50.7(3) no
N(3) Cu N(2) C(23) -128.8(4) no
N(1) Cu N(3) C(32) 47.4(3) no
N(1) Cu N(3) C(33) -146.0(5) no
N(2) Cu N(3) C(32) -106.8(4) no
N(2) Cu N(3) C(33) 59.8(4) no
Cu N(1) C(12) C(11) 53.9(4) no
Cu N(1) C(13) C(14) 12.8(2) no
Cu N(2) C(22) C(21) 53.5(3) no
Cu N(2) C(23) C(24) -2.4(2) no
Cu N(3) C(32) C(31) 53.7(3) no
Cu N(3) C(33) C(34) 15.0(3) no
C(13) N(1) C(12) C(11) -115.9(7) no
C(12) N(1) C(13) C(14) 179.0(7) no
C(23) N(2) C(22) C(21) -126.9(7) no
C(22) N(2) C(23) C(24) 178.2(7) no
C(33) N(3) C(32) C(31) -115.6(7) no
C(32) N(3) C(33) C(34) -179.4(7) no
C(21) N(4) C(11) C(12) -83.0(6) no
C(31) N(4) C(11) C(12) 141.6(7) no
C(11) N(4) C(21) C(22) 143.7(7) no
C(31) N(4) C(21) C(22) -81.3(5) no
C(11) N(4) C(31) C(32) -85.1(6) no
C(21) N(4) C(31) C(32) 139.2(7) no
N(4) C(11) C(12) N(1) -55.8(4) no
N(1) C(13) C(14) S(1) 7.1(2) no
N(1) C(13) C(14) C(15) -176.8(8) no
N(4) C(21) C(22) N(2) -58.8(4) no
N(2) C(23) C(24) S(2) -6.3(2) no
N(2) C(23) C(24) C(25) 174.7(8) no
N(4) C(31) C(32) N(3) -54.7(4) no
N(3) C(33) C(34) S(3) 4.8(2) no
N(3) C(33) C(34) C(35) -174.3(8) no
