#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/20/4332025.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332025
loop_
_publ_author_name
'Vaqueiro, Paz'
_publ_section_title
;
 From One-Dimensional Chains to Three-Dimensional Networks: 
 Solvothermal Synthesis of Thiogallates in Ethylenediamine
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4150
_journal_page_last               4156
_journal_paper_doi               10.1021/ic052043s
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source
;
see paper
;
_chemical_formula_moiety         'C3 H12 Ga1 N3 Ni0.50 S2'
_chemical_formula_sum            'C3 H12 Ga N3 Ni0.5 S2'
_chemical_formula_weight         253.36
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-09-24
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4510(10)
_cell_length_b                   15.1416(15)
_cell_length_c                   12.2387(11)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1751.4(3)
_computing_cell_refinement
; 
 Bruker X8 Apex 2 software 
;
_computing_data_collection
; 
 Bruker X8 Apex 2 software 
;
_computing_data_reduction
; 
 Bruker X8 Apex 2 software 
;
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
; 
Bruker X8 Apex 2
;
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10577
_diffrn_reflns_theta_full        30.658
_diffrn_reflns_theta_max         31.284
_diffrn_reflns_theta_min         2.540
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.591
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.7838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0726
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         763
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.000284
_refine_ls_structure_factor_coef F
_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: 
 0.606 -0.127 0.562E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0586
_refine_ls_wR_factor_gt          0.0232
_refine_ls_wR_factor_ref         0.0232
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                763
_reflns_number_total             1552
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.58
_oxford_diffrn_Wilson_scale      22.44
_oxford_refine_ls_scale          0.2346(4)
_oxford_structure_analysis_title 'Cmcm in Cmcm'
_cod_data_source_file            ic052043ssup1.cif
_cod_data_source_block           structure4
_cod_depositor_comments
;
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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C m c m '
_cod_original_formula_sum        'C3 H12 Ga1 N3 Ni0.50 S2'
_cod_database_code               4332025
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,z
x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
-x,-y,z+1/2
x,y,-z+1/2
-x+1/2,-y+1/2,z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ga1 Ga 0.0000 0.00644(4) 0.62410(4) 0.0094 1.0000 Uani S T
S1 S 0.0000 -0.10350(13) 0.7500 0.0128 1.0000 Uani S T
S2 S 0.0000 0.11965(11) 0.7500 0.0124 1.0000 Uani S T
S3 S 0.18190(10) 0.0000 0.5000 0.0151 1.0000 Uani S T
Ni1 Ni 0.0000 0.39109(6) 0.2500 0.0090 1.0000 Uani S T
N1 N 0.1459(4) 0.4980(3) 0.2500 0.0135(7) 1.0000 Uiso DS .
N2 N 0.0000 0.3814(3) 0.0760(3) 0.0152(8) 1.0000 Uiso DS .
N3 N 0.1623(5) 0.2954(3) 0.2267(4) 0.0112(11) 0.5000 Uiso D .
C1 C 0.0708(5) 0.5811(4) 0.2775(4) 0.0151(14) 0.5000 Uiso D .
C2 C 0.0476(6) 0.2915(4) 0.0472(5) 0.0158(13) 0.5000 Uiso D .
C3 C 0.1840(6) 0.2772(4) 0.1078(5) 0.0155(13) 0.5000 Uiso D .
H11 H 0.1274 0.6327 0.2500 0.0181 1.0000 Uiso S .
H12 H 0.0575 0.5849 0.3585 0.0181 0.5000 Uiso . .
H21 H 0.0639 0.2870 -0.0335 0.0191 0.5000 Uiso . .
H22 H -0.0241 0.2470 0.0701 0.0191 0.5000 Uiso . .
H31 H 0.2581 0.3180 0.0781 0.0188 0.5000 Uiso . .
H32 H 0.2155 0.2147 0.0977 0.0188 0.5000 Uiso . .
H13 H 0.2215 0.4867 0.3054 0.0162 0.5000 Uiso . .
H14 H 0.1897 0.5036 0.1759 0.0162 0.5000 Uiso . .
H23 H 0.0660 0.4263 0.0443 0.0184 0.5000 Uiso . .
H24 H -0.0976 0.3917 0.0472 0.0184 0.5000 Uiso . .
H33 H 0.2529 0.3180 0.2500 0.0139 1.0000 Uiso S .
H34 H 0.1351 0.2392 0.2645 0.0139 0.5000 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'
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'
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'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135
1.7189 '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_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S3 2_556 Ga1 S1 . 114.72(3) yes
S3 2_556 Ga1 S2 . 118.28(3) yes
S1 . Ga1 S2 . 95.26(4) yes
S3 2_556 Ga1 S3 . 96.96(4) yes
S1 . Ga1 S3 . 114.72(3) yes
S2 . Ga1 S3 . 118.28(3) yes
Ga1 . S1 Ga1 10_556 85.58(8) yes
Ga1 . S2 Ga1 10_556 83.90(7) yes
Ga1 . S3 Ga1 2_556 83.04(4) yes
N2 14_555 Ni1 N3 14_555 79.61(14) yes
N2 14_555 Ni1 N3 5_555 95.01(15) yes
N3 14_555 Ni1 N3 5_555 94.3(3) yes
N2 14_555 Ni1 N3 10_555 79.61(14) yes
N3 14_555 Ni1 N3 10_555 92.2(3) yes
N3 5_555 Ni1 N3 10_555 15.4(2) yes
N2 14_555 Ni1 N1 10_555 92.99(8) yes
N3 14_555 Ni1 N1 10_555 170.10(14) yes
N3 5_555 Ni1 N1 10_555 92.90(16) yes
N3 10_555 Ni1 N1 10_555 92.90(16) yes
N2 14_555 Ni1 N1 . 92.99(8) yes
N3 14_555 Ni1 N1 . 92.90(16) yes
N3 5_555 Ni1 N1 . 170.10(14) yes
N3 10_555 Ni1 N1 . 170.10(14) yes
N1 10_555 Ni1 N1 . 80.9(2) yes
N2 14_555 Ni1 N2 . 172.2(2) yes
N3 14_555 Ni1 N2 . 95.01(15) yes
N3 5_555 Ni1 N2 . 79.61(14) yes
N3 10_555 Ni1 N2 . 95.01(15) yes
N1 10_555 Ni1 N2 . 92.99(8) yes
N2 14_555 Ni1 N3 . 95.01(15) yes
N3 14_555 Ni1 N3 . 15.4(2) yes
N3 5_555 Ni1 N3 . 92.2(3) yes
N3 10_555 Ni1 N3 . 94.3(3) yes
N1 10_555 Ni1 N3 . 170.10(14) yes
N1 . Ni1 N2 . 92.99(8) yes
N1 . Ni1 N3 . 92.90(16) yes
N2 . Ni1 N3 . 79.61(14) yes
C1 14_555 N1 H14 14_555 109.371 no
C1 14_555 N1 H13 14_555 109.495 no
H14 14_555 N1 H13 14_555 109.511 no
C1 14_555 N1 Ni1 . 109.6(3) yes
H14 14_555 N1 Ni1 . 109.427 no
H13 14_555 N1 Ni1 . 109.430 no
H14 14_555 N1 C1 . 85.453 no
H13 14_555 N1 C1 . 129.885 no
Ni1 . N1 C1 . 109.6(3) yes
C1 14_555 N1 H13 . 129.885 no
H13 14_555 N1 H13 . 85.432 no
Ni1 . N1 H13 . 109.430 no
C1 . N1 H13 . 109.495 no
C1 14_555 N1 H14 . 85.453 no
H14 14_555 N1 H14 . 130.057 no
Ni1 . N1 H14 . 109.427 no
C1 . N1 H14 . 109.371 no
H13 . N1 H14 . 109.511 no
C2 5_555 N2 H23 5_555 110.119 no
C2 5_555 N2 H24 5_555 109.950 no
H23 5_555 N2 H24 5_555 109.427 no
C2 5_555 N2 Ni1 . 107.5(3) yes
H23 5_555 N2 Ni1 . 109.893 no
H24 5_555 N2 Ni1 . 109.915 no
H23 5_555 N2 C2 . 136.377 no
H24 5_555 N2 C2 . 77.204 no
Ni1 . N2 C2 . 107.5(3) yes
C2 5_555 N2 H23 . 136.376 no
H23 5_555 N2 H23 . 77.089 no
Ni1 . N2 H23 . 109.893 no
C2 . N2 H23 . 110.119 no
C2 5_555 N2 H24 . 77.204 no
H24 5_555 N2 H24 . 134.697 no
Ni1 . N2 H24 . 109.915 no
C2 . N2 H24 . 109.950 no
H23 . N2 H24 . 109.427 no
H34 14_555 N3 Ni1 . 115.028 no
H34 14_555 N3 C3 . 88.898 no
Ni1 . N3 C3 . 110.8(3) yes
H34 14_555 N3 H33 . 123.774 no
Ni1 . N3 H33 . 111.010 no
C3 . N3 H33 . 103.433 no
Ni1 . N3 H34 . 109.281 no
C3 . N3 H34 . 109.165 no
H33 . N3 H34 . 113.040 no
C1 10_555 C1 N1 . 109.0(3) yes
N1 . C1 C1 5_555 118.6(2) yes
C1 10_555 C1 H11 . 108.970 no
N1 . C1 H11 . 109.253 no
C1 5_555 C1 H11 . 122.117 no
C1 10_555 C1 H12 . 109.379 no
N1 . C1 H12 . 109.465 no
C1 5_555 C1 H12 . 82.768 no
H11 . C1 H12 . 110.717 no
N2 . C2 H22 5_555 129.706 no
N2 . C2 C3 . 106.1(4) yes
H22 5_555 C2 C3 . 86.600 no
N2 . C2 H21 . 110.170 no
H22 5_555 C2 H21 . 110.214 no
C3 . C2 H21 . 110.177 no
N2 . C2 H22 . 110.486 no
C3 . C2 H22 . 110.302 no
H21 . C2 H22 . 109.560 no
C2 . C3 N3 . 109.6(5) yes
C2 . C3 H31 . 109.369 no
N3 . C3 H31 . 109.508 no
C2 . C3 H32 . 109.386 no
N3 . C3 H32 . 109.613 no
H31 . C3 H32 . 109.324 no
C2 . H22 H22 5_555 47.140 no
C2 . H22 C2 5_555 59.762 no
H22 5_555 H22 C2 5_555 106.902 no
N1 . H13 H14 14_555 76.823 no
N1 . H14 H13 14_555 76.804 no
H24 5_555 H23 N2 . 72.376 no
H23 5_555 H24 N2 . 72.461 no
N3 . H34 H34 14_555 62.455 no
N3 14_555 H34 H34 14_555 96.911 no
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
Ga1 S3 2_556 2.2960(8) yes
Ga1 S1 . 2.2683(17) yes
Ga1 S2 . 2.3049(15) yes
Ga1 S3 . 2.2960(8) yes
Ni1 N2 14_555 2.135(4) yes
Ni1 N3 14_555 2.129(5) yes
Ni1 N3 5_555 2.129(5) yes
Ni1 N3 10_555 2.129(5) yes
Ni1 N1 10_555 2.127(4) yes
Ni1 N1 . 2.127(4) yes
Ni1 N2 . 2.135(4) yes
Ni1 N3 . 2.129(5) yes
N1 C1 14_555 1.483(6) yes
N1 H14 14_555 1.000 no
N1 H13 14_555 1.000 no
N1 C1 . 1.483(6) yes
N1 H13 . 1.000 no
N1 H14 . 1.000 no
N2 C2 5_555 1.476(6) yes
N2 H23 5_555 1.000 no
N2 H24 5_555 1.000 no
N2 C2 . 1.476(6) yes
N2 H23 . 1.000 no
N2 H24 . 1.000 no
N3 H34 14_555 0.896 no
N3 C3 . 1.495(6) yes
N3 H33 . 0.965 no
N3 H34 . 1.003 no
C1 C1 10_555 1.498(8) yes
C1 C1 5_555 1.339(9) yes
C1 H11 . 1.005 no
C1 H12 . 1.002 no
C2 H22 5_555 0.764 no
C2 C3 . 1.502(7) yes
C2 H21 . 1.002 no
C2 H22 . 0.997 no
C3 H31 . 1.002 no
C3 H32 . 1.000 no
H22 H22 5_555 0.456 no
H13 H14 14_555 0.456 no
H23 H24 5_555 0.604 no
H34 H34 14_555 0.356 no
