#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310042.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_4310042
loop_
_publ_author_name
'Philip J. Bailey'
'Alice Dawson'
'Chiara McCormack'
'Stephen A. Moggach'
'Iain D. H. Oswald'
'Simon Parsons'
'David W. H. Rankin'
'Andrew Turner'
_publ_contact_author_email       S.Parsons@ed.ac.uk
_publ_contact_author_name        'Simon Parsons'
_publ_section_title
;
Barriers to Racemization in C3-Symmetric Complexes Containing the
Hydrotris(2-mercapto-1-ethylimidazolyl)borate (TmEt) Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8884
_journal_page_last               8898
_journal_paper_doi               10.1021/ic0505293
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H37 B1 Cu1 N6 P1 S3'
_chemical_formula_sum            'C33 H37 B Cu N6 P S3'
_chemical_formula_weight         719.23
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_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
_audit_creation_date             05-03-22
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.5870(16)
_cell_length_b                   15.5870(16)
_cell_length_c                   12.144(2)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     2555.2(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5114
_diffrn_reflns_theta_full        23.259
_diffrn_reflns_theta_max         23.259
_diffrn_reflns_theta_min         2.256
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.71
_refine_diff_density_min         -1.17
_refine_ls_abs_structure_details 'Flack, 31 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.058(10)
_refine_ls_extinction_coef       78(7)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0175
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1619
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001357
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 22.6 32.5 14.2 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0504
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0504
_reflns_limit_h_max              8
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                1606
_reflns_number_total             1619
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.4049(6)
_oxford_structure_analysis_title 'cm1051 in R3'
_cod_data_source_file            ic0505293si20050817_061150_3.cif
_cod_data_source_block           cm1051
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 
;
_cod_original_cell_volume        2555.1(6)
_cod_original_sg_symbol_H-M      'R 3 '
_cod_original_formula_sum        'C33 H37 B1 Cu1 N6 P1 S3'
_cod_database_code               4310042
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/3,y+2/3,z+2/3
x+2/3,y+1/3,z+1/3
-y,x-y,z
-y+1/3,x-y+2/3,z+2/3
-y+2/3,x-y+1/3,z+1/3
-x+y,-x,z
-x+y+1/3,-x+2/3,z+2/3
-x+y+2/3,-x+1/3,z+1/3
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.0000 1.0000 0.80581(4) 0.0215 1.0000 Uani S T . . . .
B1 B 0.0000 1.0000 0.4972(4) 0.0256 1.0000 Uani S T . . . .
P1 P 0.0000 1.0000 0.98933(8) 0.0207 1.0000 Uani S T . . . .
S2 S -0.08847(5) 0.84115(4) 0.72016(6) 0.0228 1.0000 Uani . . . . . .
C10 C 0.04278(17) 1.12186(19) 1.0534(2) 0.0236 1.0000 Uani . . . . . .
C11 C 0.0131(2) 1.1834(2) 1.0058(2) 0.0311 1.0000 Uani . . . . . .
C12 C 0.0428(2) 1.2764(2) 1.0491(2) 0.0392 1.0000 Uani . . . . . .
C13 C 0.1034(2) 1.3084(2) 1.1424(2) 0.0375 1.0000 Uani . . . . . .
C14 C 0.1331(2) 1.2481(2) 1.1895(2) 0.0340 1.0000 Uani . . . . . .
C15 C 0.10291(17) 1.15385(19) 1.1471(2) 0.0270 1.0000 Uani . . . . . .
C21 C -0.00140(19) 0.85985(19) 0.6214(2) 0.0240 1.0000 Uani . . . . . .
N22 N 0.02542(15) 0.92043(15) 0.53317(16) 0.0237 1.0000 Uani . . . . . .
C23 C 0.0983(2) 0.9119(2) 0.4771(2) 0.0299 1.0000 Uani . . . . . .
C24 C 0.1158(2) 0.8470(2) 0.5310(2) 0.0311 1.0000 Uani . . . . . .
N25 N 0.05233(15) 0.81349(16) 0.62078(17) 0.0266 1.0000 Uani . . . . . .
C26 C 0.0513(2) 0.7466(2) 0.7059(2) 0.0326 1.0000 Uani . . . . . .
C27 C 0.1057(2) 0.8032(2) 0.8086(2) 0.0368 1.0000 Uani . . . . . .
H1 H 0.0000 1.0000 0.4101 0.0500 1.0000 Uiso . . . . . .
H11 H -0.0272 1.1621 0.9415 0.0347 1.0000 Uiso . . . . . .
H12 H 0.0223 1.3184 1.0160 0.0485 1.0000 Uiso . . . . . .
H13 H 0.1250 1.3723 1.1714 0.0402 1.0000 Uiso . . . . . .
H14 H 0.1740 1.2695 1.2532 0.0355 1.0000 Uiso . . . . . .
H15 H 0.1233 1.1124 1.1811 0.0312 1.0000 Uiso . . . . . .
H23 H 0.1309 0.9457 0.4119 0.0326 1.0000 Uiso . . . . . .
H241 H 0.1629 0.8280 0.5118 0.0385 1.0000 Uiso . . . . . .
H261 H -0.0186 0.6987 0.7253 0.0398 1.0000 Uiso . . . . . .
H262 H 0.0846 0.7112 0.6765 0.0398 1.0000 Uiso . . . . . .
H271 H 0.1031 0.7546 0.8644 0.0561 1.0000 Uiso . . . . . .
H272 H 0.0726 0.8388 0.8387 0.0561 1.0000 Uiso . . . . . .
H273 H 0.1758 0.8512 0.7898 0.0561 1.0000 Uiso . . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 4_675 Cu1 . S2 7_465 102.43(2) yes
S2 4_675 Cu1 . P1 . 115.83(2) yes
S2 7_465 Cu1 . P1 . 115.827(19) yes
S2 4_675 Cu1 . S2 . 102.43(2) yes
S2 7_465 Cu1 . S2 . 102.43(2) yes
P1 . Cu1 . S2 . 115.827(16) yes
N22 4_675 B1 . N22 7_465 112.30(16) yes
N22 4_675 B1 . N22 . 112.30(16) yes
N22 7_465 B1 . N22 . 112.30(16) yes
N22 4_675 B1 . H1 . 106.5 no
N22 7_465 B1 . H1 . 106.5 no
N22 . B1 . H1 . 106.5 no
C10 7_465 P1 . C10 4_675 103.42(10) yes
C10 7_465 P1 . Cu1 . 115.00(8) yes
C10 4_675 P1 . Cu1 . 115.00(8) yes
C10 7_465 P1 . C10 . 103.42(10) yes
C10 4_675 P1 . C10 . 103.42(10) yes
Cu1 . P1 . C10 . 115.00(8) yes
Cu1 . S2 . C21 . 97.48(9) yes
P1 . C10 . C11 . 117.7(2) yes
P1 . C10 . C15 . 123.0(2) yes
C11 . C10 . C15 . 119.3(2) yes
C10 . C11 . C12 . 121.0(3) yes
C10 . C11 . H11 . 119.5 no
C12 . C11 . H11 . 119.5 no
C11 . C12 . C13 . 119.6(3) yes
C11 . C12 . H12 . 120.6 no
C13 . C12 . H12 . 119.9 no
C12 . C13 . C14 . 119.7(3) yes
C12 . C13 . H13 . 120.0 no
C14 . C13 . H13 . 120.3 no
C13 . C14 . C15 . 121.2(3) yes
C13 . C14 . H14 . 119.9 no
C15 . C14 . H14 . 118.9 no
C10 . C15 . C14 . 119.2(2) yes
C10 . C15 . H15 . 120.4 no
C14 . C15 . H15 . 120.4 no
S2 . C21 . N22 . 127.84(19) yes
S2 . C21 . N25 . 124.0(2) yes
N22 . C21 . N25 . 108.2(2) yes
B1 . N22 . C21 . 132.4(2) yes
B1 . N22 . C23 . 119.4(2) yes
C21 . N22 . C23 . 107.7(2) yes
N22 . C23 . C24 . 108.5(2) yes
N22 . C23 . H23 . 126.4 no
C24 . C23 . H23 . 125.1 no
C23 . C24 . N25 . 107.0(2) yes
C23 . C24 . H241 . 126.6 no
N25 . C24 . H241 . 126.4 no
C24 . N25 . C21 . 108.5(2) yes
C24 . N25 . C26 . 125.2(2) yes
C21 . N25 . C26 . 126.0(2) yes
N25 . C26 . C27 . 111.2(2) yes
N25 . C26 . H261 . 108.7 no
C27 . C26 . H261 . 109.0 no
N25 . C26 . H262 . 108.6 no
C27 . C26 . H262 . 108.8 no
H261 . C26 . H262 . 110.5 no
C26 . C27 . H271 . 108.5 no
C26 . C27 . H272 . 109.3 no
H271 . C27 . H272 . 109.6 no
C26 . C27 . H273 . 109.5 no
H271 . C27 . H273 . 109.8 no
H272 . C27 . H273 . 110.2 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . S2 4_675 2.3873(6) yes
Cu1 . S2 7_465 2.3873(6) yes
Cu1 . P1 . 2.2286(12) yes
Cu1 . S2 . 2.3873(6) yes
B1 . N22 4_675 1.542(2) yes
B1 . N22 7_465 1.542(2) yes
B1 . N22 . 1.542(2) yes
B1 . H1 . 1.058 no
P1 . C10 7_465 1.842(3) yes
P1 . C10 4_675 1.842(3) yes
P1 . C10 . 1.842(3) yes
S2 . C21 . 1.723(2) yes
C10 . C11 . 1.382(4) yes
C10 . C15 . 1.398(4) yes
C11 . C12 . 1.387(4) yes
C11 . H11 . 0.952 no
C12 . C13 . 1.397(4) yes
C12 . H12 . 0.949 no
C13 . C14 . 1.365(4) yes
C13 . H13 . 0.945 no
C14 . C15 . 1.397(4) yes
C14 . H14 . 0.951 no
C15 . H15 . 0.945 no
C21 . N22 . 1.349(3) yes
C21 . N25 . 1.352(3) yes
N22 . C23 . 1.387(3) yes
C23 . C24 . 1.341(4) yes
C23 . H23 . 0.947 no
C24 . N25 . 1.387(4) yes
C24 . H241 . 0.948 no
N25 . C26 . 1.463(3) yes
C26 . C27 . 1.518(4) yes
C26 . H261 . 0.993 no
C26 . H262 . 0.995 no
C27 . H271 . 1.002 no
C27 . H272 . 0.997 no
C27 . H273 . 0.995 no
