#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:07:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179827 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/23/7012335.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_7012335
loop_
_publ_author_name
'Beer, Paul D.'
'Cheetham, Andrew G.'
'Drew, Michael G. B.'
'Fox, O. Danny'
'Hayes, Elizabeth J.'
'Rolls, Toby D.'
_publ_section_title
;
 Pyrrole-based metallo-macrocycles and cryptands
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              603
_journal_paper_doi               10.1039/b210099a
_journal_year                    2003
_chemical_formula_sum            'C28 H26 N2 Ni S4'
_chemical_formula_weight         577.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.747(10)
_cell_angle_beta                 93.284(10)
_cell_angle_gamma                106.730(10)
_cell_formula_units_Z            1
_cell_length_a                   6.294(10)
_cell_length_b                   10.323(14)
_cell_length_c                   10.909(17)
_cell_measurement_temperature    293(2)
_cell_volume                     662.2(17)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2120
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1552
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1798P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2298
_refine_ls_wR_factor_ref         0.2688
_reflns_number_gt                1240
_reflns_number_total             2120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210099a.txt
_cod_data_source_block           2-Ni
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.1798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012335
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.0000 0.0599(5) Uani 1 d S . .
S1 S 0.1287(3) -0.02695(19) -0.18404(19) 0.0642(6) Uani 1 d . . .
S2 S 0.3375(3) 0.1495(2) 0.04741(19) 0.0669(6) Uani 1 d . . .
C3 C 0.3719(11) 0.0978(7) -0.1083(7) 0.0539(17) Uani 1 d . . .
N4 C 0.5509(10) 0.1443(6) -0.1592(6) 0.0457(14) Uani 1 d . . .
C41 C 0.7531(13) 0.2434(8) -0.0824(8) 0.071(2) Uani 1 d . . .
H41A H 0.8563 0.1935 -0.0645 0.085 Uiso 1 calc R . .
H41B H 0.7117 0.2828 -0.0030 0.085 Uiso 1 calc R . .
C42 C 0.8719(12) 0.3600(7) -0.1433(7) 0.0581(18) Uani 1 d . . .
C43 C 1.0685(12) 0.3646(8) -0.1912(8) 0.070(2) Uani 1 d . . .
H43 H 1.1305 0.2931 -0.1902 0.084 Uiso 1 calc R . .
C44 C 1.1711(17) 0.4720(11) -0.2394(12) 0.095(3) Uani 1 d . . .
H44 H 1.3086 0.4780 -0.2690 0.114 Uiso 1 calc R . .
C45 C 1.073(3) 0.5737(15) -0.2453(16) 0.139(6) Uani 1 d . . .
H45 H 1.1454 0.6473 -0.2809 0.166 Uiso 1 calc R . .
C46 C 0.882(3) 0.5710(14) -0.2026(15) 0.128(5) Uani 1 d . . .
H46 H 0.8133 0.6386 -0.2093 0.153 Uiso 1 calc R . .
C47 C 0.7930(17) 0.4679(10) -0.1503(9) 0.082(3) Uani 1 d . . .
H47 H 0.6629 0.4682 -0.1142 0.099 Uiso 1 calc R . .
C51 C 0.5689(13) 0.0865(8) -0.2935(8) 0.070(2) Uani 1 d . . .
H51A H 0.7227 0.0884 -0.3005 0.084 Uiso 1 calc R . .
H51B H 0.4778 -0.0098 -0.3145 0.084 Uiso 1 calc R . .
C52 C 0.5019(12) 0.1573(8) -0.3879(7) 0.0597(18) Uani 1 d . . .
C53 C 0.637(2) 0.2541(10) -0.4408(11) 0.104(4) Uani 1 d . . .
H53 H 0.7924 0.2859 -0.4241 0.124 Uiso 1 calc R . .
C54 C 0.497(5) 0.3048(16) -0.5336(14) 0.201(11) Uani 1 d . . .
H54 H 0.5425 0.3688 -0.5840 0.242 Uiso 1 calc R . .
C55 C 0.266(3) 0.2198(14) -0.5175(11) 0.109(4) Uani 1 d . . .
H55 H 0.1330 0.2224 -0.5574 0.131 Uiso 1 calc R . .
N56 N 0.2831(15) 0.1390(11) -0.4357(8) 0.100(3) Uani 1 d . . .
H56 H 0.1693 0.0816 -0.4151 0.120 Uiso 1 calc R . .
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'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
S2 Ni1 S2 180.0 2 . ?
S2 Ni1 S1 100.52(9) 2 . ?
S2 Ni1 S1 79.48(9) . . ?
S2 Ni1 S1 79.48(9) 2 2 ?
S2 Ni1 S1 100.52(10) . 2 ?
S1 Ni1 S1 180.0 . 2 ?
C3 S1 Ni1 85.6(3) . . ?
C3 S2 Ni1 85.9(2) . . ?
N4 C3 S2 125.2(5) . . ?
N4 C3 S1 125.8(6) . . ?
S2 C3 S1 109.0(4) . . ?
C3 N4 C41 120.6(7) . . ?
C3 N4 C51 121.1(6) . . ?
C41 N4 C51 117.9(7) . . ?
N4 C41 C42 114.3(7) . . ?
C47 C42 C43 116.1(9) . . ?
C47 C42 C41 122.2(8) . . ?
C43 C42 C41 121.7(7) . . ?
C44 C43 C42 119.5(8) . . ?
C43 C44 C45 119.7(12) . . ?
C46 C45 C44 122.3(18) . . ?
C47 C46 C45 115.9(14) . . ?
C46 C47 C42 126.4(12) . . ?
C52 C51 N4 116.4(6) . . ?
C53 C52 N56 107.4(10) . . ?
C53 C52 C51 127.3(9) . . ?
N56 C52 C51 125.3(9) . . ?
C52 C53 C54 110.5(13) . . ?
C55 C54 C53 99.4(12) . . ?
N56 C55 C54 108.8(12) . . ?
C55 N56 C52 113.8(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.202(3) 2 ?
Ni1 S2 2.202(3) . ?
Ni1 S1 2.207(4) . ?
Ni1 S1 2.207(4) 2 ?
S1 C3 1.734(7) . ?
S2 C3 1.728(8) . ?
C3 N4 1.292(11) . ?
N4 C41 1.475(10) . ?
N4 C51 1.499(11) . ?
C41 C42 1.512(12) . ?
C42 C47 1.357(13) . ?
C42 C43 1.362(10) . ?
C43 C44 1.329(14) . ?
C44 C45 1.371(17) . ?
C45 C46 1.31(2) . ?
C46 C47 1.299(19) . ?
C51 C52 1.477(12) . ?
C52 C53 1.356(14) . ?
C52 N56 1.391(11) . ?
C53 C54 1.56(2) . ?
C54 C55 1.51(2) . ?
C55 N56 1.349(15) . ?
