#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:15:14 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180496 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/65/7216583.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_7216583
loop_
_publ_author_name
'Burrows, Andrew D.'
'Harrington, Ross W.'
'Mahon, Mary F.'
'Teat, Simon J.'
_publ_section_title
;
 Structural manipulation through selective substitution of hydrogen
 bonding groups: the supramolecular structures of
 bis(thiosemicarbazidato)nickel complexes
;
_journal_issue                   89
_journal_name_full               CrystEngComm
_journal_page_first              539
_journal_paper_doi               10.1039/b208284e
_journal_volume                  4
_journal_year                    2002
_chemical_formula_sum            'C4 H12 N6 Ni S2'
_chemical_formula_weight         267.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.034(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.956(2)
_cell_length_b                   4.6144(10)
_cell_length_c                   10.907(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     470.76(16)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68980
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2950
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.88
_exptl_absorpt_coefficient_mu    2.466
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.8271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.004(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1218
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+0.3350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                1070
_reflns_number_total             1218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208284e.txt
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'multiscan'
changed to 'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        470.79(18)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7216583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.0000 0.5000 0.5000 0.00910(12) Uani 1 2 d S
S1 S -0.15281(5) 0.68597(10) 0.57972(4) 0.01244(13) Uani 1 1 d .
N1 N 0.14083(16) 0.7426(4) 0.61837(15) 0.0105(3) Uani 1 1 d D
H1A H 0.215(2) 0.644(5) 0.663(2) 0.031(7) Uiso 1 1 d D
H1B H 0.163(2) 0.881(4) 0.5719(19) 0.012(5) Uiso 1 1 d D
N2 N 0.10579(17) 0.9098(4) 0.71668(15) 0.0118(3) Uani 1 1 d .
N3 N -0.07917(18) 1.0332(4) 0.78619(17) 0.0157(3) Uani 1 1 d D
H3 H -0.1687(19) 1.008(6) 0.776(3) 0.021(7) Uiso 1 1 d D
C1 C -0.02853(19) 0.8907(4) 0.70252(17) 0.0113(3) Uani 1 1 d .
C2 C 0.0080(2) 1.2368(5) 0.8813(2) 0.0170(4) Uani 1 1 d .
H2A H 0.045(3) 1.385(6) 0.840(2) 0.018(6) Uiso 1 1 d .
H2B H -0.050(3) 1.323(7) 0.922(3) 0.030(7) Uiso 1 1 d .
H2C H 0.088(3) 1.138(6) 0.947(2) 0.022(7) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.00746(17) 0.01058(19) 0.00884(17) -0.00122(12) 0.00223(12) -0.00014(11)
S1 0.0086(2) 0.0152(2) 0.0136(2) -0.00377(17) 0.00372(16) -0.00138(16)
N1 0.0093(7) 0.0111(8) 0.0111(7) 0.0001(6) 0.0034(6) 0.0014(6)
N2 0.0112(7) 0.0136(7) 0.0103(7) -0.0031(6) 0.0035(5) -0.0009(6)
N3 0.0122(7) 0.0193(9) 0.0166(8) -0.0068(6) 0.0063(6) -0.0025(6)
C1 0.0133(8) 0.0105(8) 0.0097(7) 0.0017(7) 0.0036(6) 0.0009(7)
C2 0.0173(9) 0.0180(10) 0.0161(9) -0.0066(8) 0.0063(8) -0.0024(8)
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'
S S 0.1246 0.1234 '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'
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 Ni1 N1 180.0 3_566 .
N1 Ni1 S1 92.84(5) 3_566 .
N1 Ni1 S1 87.16(5) . .
N1 Ni1 S1 87.16(5) 3_566 3_566
N1 Ni1 S1 92.84(5) . 3_566
S1 Ni1 S1 180.0 . 3_566
C1 S1 Ni1 96.36(6) . .
N2 N1 Ni1 120.17(11) . .
C1 N2 N1 111.96(15) . .
C1 N3 C2 121.85(17) . .
N2 C1 N3 119.60(17) . .
N2 C1 S1 123.81(14) . .
N3 C1 S1 116.59(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.9093(16) 3_566
Ni1 N1 1.9093(16) .
Ni1 S1 2.1711(5) .
Ni1 S1 2.1711(5) 3_566
S1 C1 1.7557(19) .
N1 N2 1.457(2) .
N2 C1 1.296(2) .
N3 C1 1.355(2) .
N3 C2 1.447(2) .
