#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/38/2003804.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_2003804
loop_
_publ_author_name
'Brooker, S.'
'Carter, B. M.'
_publ_section_title
;
 Synthesis and Structure of a Tetracopper(II) Complex of a
 Pyrrole-Containing Unsymmetrical Binucleating Ligand:
 [Cu₂L(NCS)₂]₂
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1522
_journal_page_last               1524
_journal_paper_doi               10.1107/S0108270195001363
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C50 H58 Cu4 N18 S4'
_chemical_formula_weight         1293.54
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                107.36(3)
_cell_angle_beta                 104.31(3)
_cell_angle_gamma                108.60(2)
_cell_formula_units_Z            1
_cell_length_a                   10.527(3)
_cell_length_b                   12.163(3)
_cell_length_c                   12.653(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    133
_cell_measurement_theta_max      13
_cell_measurement_theta_min      4
_cell_volume                     1356.5(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  'SHELXL-93 gamma release'
_computing_structure_refinement  'SHELXL-93 gamma release (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133
_diffrn_measurement_device       'Siemens P4 four circle'
_diffrn_measurement_method       '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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4809
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment
;H atoms riding; U~iso~ = 1.2 x atom to which H atom is
attached
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^) + (0.0390P)^2^ + 0.4546P]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.0966
_refine_ls_wR_factor_obs         0.0838
_reflns_number_observed          3244
_reflns_number_total             4533
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            kh1024.cif
_cod_data_source_block           cub1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1356.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2003804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
Cu1 1 0.04992(6) 0.40451(5) 0.08913(5) 0.0224(2) Uani d . Cu
Cu2 1 0.35027(6) 0.23857(5) 0.34829(5) 0.0243(2) Uani d . Cu
N1 1 0.0131(4) 0.3035(3) 0.2145(3) 0.0209(8) Uani d . N
C1 1 0.0232(5) 0.1981(4) 0.2191(4) 0.0212(10) Uani d . C
C2 1 -0.0188(5) 0.1481(5) 0.2954(5) 0.0318(12) Uani d . C
H2 1 -0.0123(5) 0.0719(5) 0.2950(5) 0.038 Uiso calc R H
C3 1 -0.0707(6) 0.2101(5) 0.3729(5) 0.0412(14) Uani d . C
H3 1 -0.0974(6) 0.1790(5) 0.4283(5) 0.049 Uiso calc R H
C4 1 -0.0824(5) 0.3176(5) 0.3675(4) 0.0317(12) Uani d . C
H4 1 -0.1182(5) 0.3618(5) 0.4193(4) 0.038 Uiso calc R H
C5 1 -0.0421(5) 0.3612(4) 0.2866(4) 0.0237(11) Uani d . C
C6 1 -0.0582(5) 0.4758(4) 0.2744(4) 0.0261(11) Uani d . C
H6A 1 -0.1566(5) 0.4492(4) 0.2169(4) 0.031 Uiso calc R H
H6B 1 -0.0460(5) 0.5360(4) 0.3527(4) 0.031 Uiso calc R H
N2 1 0.0504(4) 0.5395(4) 0.2323(3) 0.0254(9) Uani d . N
H2A 1 0.0179(4) 0.5915(4) 0.2034(3) 0.030 Uiso calc R H
C7 1 0.1895(5) 0.6254(4) 0.3364(4) 0.0297(12) Uani d . C
H7A 1 0.2126(5) 0.5775(4) 0.3835(4) 0.036 Uiso calc R H
H7B 1 0.1765(5) 0.6965(4) 0.3884(4) 0.036 Uiso calc R H
C8 1 0.3158(5) 0.6796(4) 0.3030(4) 0.0282(11) Uani d . C
H8A 1 0.3951(5) 0.7524(4) 0.3748(4) 0.034 Uiso calc R H
H8B 1 0.2859(5) 0.7122(4) 0.2427(4) 0.034 Uiso calc R H
C9 1 0.3728(5) 0.5841(4) 0.2531(4) 0.0280(11) Uani d . C
H9A 1 0.4627(5) 0.6281(4) 0.2427(4) 0.034 Uiso calc R H
H9B 1 0.3965(5) 0.5464(4) 0.3104(4) 0.034 Uiso calc R H
N3 1 0.2662(4) 0.4835(3) 0.1386(3) 0.0231(9) Uani d . N
C10 1 0.3060(5) 0.4456(4) 0.0513(4) 0.0264(11) Uani d . C
H10 1 0.4047(5) 0.4816(4) 0.0608(4) 0.032 Uiso calc R H
C11 1 0.1994(5) 0.3492(5) -0.0586(4) 0.0257(11) Uani d . C
C12 1 0.1950(6) 0.2855(5) -0.1711(4) 0.0330(12) Uani d . C
H12 1 0.2747(6) 0.2989(5) -0.1959(4) 0.040 Uiso calc R H
C13 1 0.0530(6) 0.1987(5) -0.2405(4) 0.0334(12) Uani d . C
H13 1 0.0165(6) 0.1416(5) -0.3221(4) 0.040 Uiso calc R H
C14 1 -0.0262(5) 0.2108(4) -0.1681(4) 0.0294(12) Uani d . C
H14 1 -0.1272(5) 0.1621(4) -0.1924(4) 0.035 Uiso calc R H
N4 1 0.0627(4) 0.3029(3) -0.0573(3) 0.0237(9) Uani d . N
C15 1 0.0886(5) 0.1399(4) 0.1368(4) 0.0251(11) Uani d . C
H15A 1 0.0736(5) 0.0542(4) 0.1337(4) 0.030 Uiso calc R H
H15B 1 0.0390(5) 0.1303(4) 0.0550(4) 0.030 Uiso calc R H
N5 1 0.2451(4) 0.2198(4) 0.1783(3) 0.0228(9) Uani d . N
H5 1 0.2535(4) 0.3007(4) 0.1864(3) 0.027 Uiso calc R H
C16 1 0.3026(6) 0.1776(5) 0.0851(4) 0.0305(12) Uani d . C
H16A 1 0.3968(6) 0.2469(5) 0.1043(4) 0.037 Uiso calc R H
H16B 1 0.2354(6) 0.1637(5) 0.0072(4) 0.037 Uiso calc R H
C17 1 0.3235(6) 0.0574(5) 0.0719(4) 0.0309(12) Uani d . C
H17A 1 0.3478(6) 0.0304(5) 0.0005(4) 0.037 Uiso calc R H
H17B 1 0.2307(6) -0.0107(5) 0.0575(4) 0.037 Uiso calc R H
C18 1 0.4404(5) 0.0707(5) 0.1790(4) 0.0309(12) Uani d . C
H18A 1 0.4542(5) -0.0087(5) 0.1607(4) 0.037 Uiso calc R H
H18B 1 0.5331(5) 0.1412(5) 0.1966(4) 0.037 Uiso calc R H
N6 1 0.4001(4) 0.0963(4) 0.2823(3) 0.0261(9) Uani d . N
C19 1 0.3898(5) 0.0244(4) 0.3384(4) 0.0269(11) Uani d . C
H19 1 0.4111(5) -0.0473(4) 0.3149(4) 0.032 Uiso calc R H
C20 1 0.3458(5) 0.0541(4) 0.4364(4) 0.0264(11) Uani d . C
C21 1 0.3170(5) 0.0016(5) 0.5152(5) 0.0350(13) Uani d . C
H21 1 0.3250(5) -0.0732(5) 0.5181(5) 0.042 Uiso calc R H
C22 1 0.2739(5) 0.0789(5) 0.5896(4) 0.0346(13) Uani d . C
H22 1 0.2464(5) 0.0672(5) 0.6529(4) 0.042 Uiso calc R H
C23 1 0.2789(5) 0.1763(5) 0.5530(4) 0.0324(12) Uani d . C
H23 1 0.2551(5) 0.2436(5) 0.5885(4) 0.039 Uiso calc R H
N7 1 0.3219(4) 0.1624(4) 0.4610(3) 0.0257(9) Uani d . N
N30 1 -0.1599(5) 0.3470(4) 0.0072(4) 0.0337(10) Uani d . N
C30 1 -0.2832(6) 0.3058(5) -0.0193(4) 0.0290(12) Uani d . C
S30 1 -0.45692(15) 0.25082(14) -0.05797(14) 0.0437(4) Uani d . S
N40 1 0.3253(4) 0.3880(4) 0.4332(3) 0.0256(9) Uani d . N
C40 1 0.3500(4) 0.4751(4) 0.5170(4) 0.0214(10) Uani d . C
S40 1 0.38416(14) 0.59966(13) 0.63359(12) 0.0404(4) Uani d . S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033
S S 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.1234
Cu Cu 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3201 1.2651
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 Cu1 N30 . 91.5(2) yes
N4 Cu1 N3 . 81.3(2) yes
N30 Cu1 N3 . 164.0(2) yes
N4 Cu1 N2 . 168.7(2) yes
N30 Cu1 N2 . 90.1(2) yes
N3 Cu1 N2 . 94.4(2) yes
N4 Cu1 N1 . 114.76(15) yes
N30 Cu1 N1 . 92.1(2) yes
N3 Cu1 N1 . 103.92(14) yes
N2 Cu1 N1 . 76.34(14) yes
N7 Cu2 N40 . 94.2(2) yes
N7 Cu2 N6 . 82.5(2) yes
N40 Cu2 N6 . 172.0(2) yes
N7 Cu2 N5 . 141.2(2) yes
N40 Cu2 N5 . 96.0(2) yes
N6 Cu2 N5 . 91.1(2) yes
N7 Cu2 S40 2_666 124.57(12) yes
N40 Cu2 S40 2_666 88.42(12) yes
N6 Cu2 S40 2_666 87.49(12) yes
N5 Cu2 S40 2_666 93.12(12) yes
C1 N1 C5 . 118.2(4) ?
C1 N1 Cu1 . 132.9(3) ?
C5 N1 Cu1 . 108.5(3) ?
N1 C1 C2 . 122.6(4) ?
N1 C1 C15 . 115.0(4) ?
C2 C1 C15 . 122.3(4) ?
C1 C2 C3 . 119.2(4) ?
C4 C3 C2 . 118.2(5) ?
C3 C4 C5 . 119.8(5) ?
N1 C5 C4 . 121.9(4) ?
N1 C5 C6 . 116.5(4) ?
C4 C5 C6 . 121.6(4) ?
N2 C6 C5 . 110.6(3) ?
C6 N2 C7 . 109.2(4) ?
C6 N2 Cu1 . 108.4(3) ?
C7 N2 Cu1 . 118.9(3) ?
N2 C7 C8 . 114.3(4) ?
C7 C8 C9 . 113.6(4) ?
N3 C9 C8 . 110.9(4) ?
C10 N3 C9 . 119.9(4) ?
C10 N3 Cu1 . 112.4(3) ?
C9 N3 Cu1 . 127.3(3) ?
N3 C10 C11 . 118.2(4) ?
N4 C11 C12 . 109.2(4) ?
N4 C11 C10 . 114.3(4) ?
C12 C11 C10 . 136.5(5) ?
C13 C12 C11 . 107.2(5) ?
C12 C13 C14 . 107.0(4) ?
N4 C14 C13 . 109.6(4) ?
C14 N4 C11 . 107.1(4) ?
C14 N4 Cu1 . 139.3(3) ?
C11 N4 Cu1 . 112.6(3) ?
N5 C15 C1 . 111.2(3) ?
C15 N5 C16 . 111.0(4) ?
C15 N5 Cu2 . 109.8(3) ?
C16 N5 Cu2 . 117.8(3) ?
N5 C16 C17 . 115.0(4) ?
C16 C17 C18 . 114.4(4) ?
N6 C18 C17 . 110.1(4) ?
C19 N6 C18 . 121.9(4) ?
C19 N6 Cu2 . 113.0(3) ?
C18 N6 Cu2 . 125.0(3) ?
N6 C19 C20 . 118.4(4) ?
C21 C20 N7 . 109.1(4) ?
C21 C20 C19 . 136.9(4) ?
N7 C20 C19 . 114.0(4) ?
C20 C21 C22 . 106.9(4) ?
C23 C22 C21 . 106.4(5) ?
N7 C23 C22 . 110.5(4) ?
C23 N7 C20 . 107.0(4) ?
C23 N7 Cu2 . 140.7(3) ?
C20 N7 Cu2 . 112.1(3) ?
C30 N30 Cu1 . 164.4(4) ?
N30 C30 S30 . 178.4(5) ?
C40 N40 Cu2 . 153.8(4) ?
N40 C40 S40 . 178.8(4) ?
C40 S40 Cu2 2_666 99.4(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N4 . 1.960(4) yes
Cu1 N30 . 1.973(4) yes
Cu1 N3 . 2.010(4) yes
Cu1 N2 . 2.048(4) yes
Cu1 N1 . 2.310(4) yes
Cu2 N7 . 1.951(4) yes
Cu2 N40 . 1.951(4) yes
Cu2 N6 . 1.974(4) yes
Cu2 N5 . 2.068(4) yes
Cu2 S40 2_666 2.765(2) yes
N1 C1 . 1.337(5) ?
N1 C5 . 1.342(5) ?
C1 C2 . 1.374(7) ?
C1 C15 . 1.512(6) ?
C2 C3 . 1.383(7) ?
C3 C4 . 1.372(7) ?
C4 C5 . 1.381(6) ?
C5 C6 . 1.504(6) ?
C6 N2 . 1.474(6) ?
N2 C7 . 1.489(6) ?
C7 C8 . 1.505(7) ?
C8 C9 . 1.518(6) ?
C9 N3 . 1.455(6) ?
N3 C10 . 1.287(6) ?
C10 C11 . 1.409(7) ?
C11 N4 . 1.374(6) ?
C11 C12 . 1.384(6) ?
C12 C13 . 1.383(7) ?
C13 C14 . 1.390(7) ?
C14 N4 . 1.357(6) ?
C15 N5 . 1.477(6) ?
N5 C16 . 1.487(6) ?
C16 C17 . 1.513(6) ?
C17 C18 . 1.515(7) ?
C18 N6 . 1.450(6) ?
N6 C19 . 1.275(6) ?
C19 C20 . 1.416(7) ?
C20 C21 . 1.378(7) ?
C20 N7 . 1.379(6) ?
C21 C22 . 1.390(7) ?
C22 C23 . 1.386(7) ?
C23 N7 . 1.334(6) ?
N30 C30 . 1.148(6) ?
C30 S30 . 1.616(6) ?
N40 C40 . 1.154(6) ?
C40 S40 . 1.630(5) ?
S40 Cu2 2_666 2.765(2) ?
