#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:15:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179621 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/85/4508599.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_4508599
loop_
_publ_author_name
'Goswami, Arijit'
'Bala, Sukhen'
'Pachfule, Pradip'
'Mondal, Raju'
_publ_section_title
;
 Comprehensive Study on Mutual Interplay of Multiple V-Shaped Ligands on
 the Helical Nature of a Series of Coordination Polymers and Their
 Properties
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5487
_journal_paper_doi               10.1021/cg401469f
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C25 H24 N4 Ni O6 S'
_chemical_formula_weight         567.25
_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                78.630(16)
_cell_angle_beta                 75.404(15)
_cell_angle_gamma                85.896(16)
_cell_formula_units_Z            2
_cell_length_a                   10.178(6)
_cell_length_b                   12.409(7)
_cell_length_c                   13.390(8)
_cell_measurement_reflns_used    2761
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.28
_cell_volume                     1604.0(16)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w 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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14724
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.731054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.03 (Bruker, 2001), R(int)=0.1624 before correction'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0538
_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)+(0.0759P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                3792
_reflns_number_total             6078
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg401469f_si_006.cif
_cod_data_source_block           12sbj005_0m
_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 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'Constr' changed
to 'constr' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1603.9(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4508599
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.18142(5) 0.32570(4) 0.46251(4) 0.03288(17) Uani 1 1 d .
S1 S 0.30853(12) 0.73491(8) 0.85967(7) 0.0455(3) Uani 1 1 d .
O1 O 0.1242(2) 0.3685(2) 0.61008(19) 0.0386(6) Uani 1 1 d .
N1 N -0.0077(3) 0.2769(2) 0.4689(2) 0.0357(7) Uani 1 1 d .
C1 C -0.0611(4) 0.2049(3) 0.4280(3) 0.0357(9) Uani 1 1 d .
O2 O 0.3284(3) 0.4067(2) 0.5109(2) 0.0418(7) Uani 1 1 d .
N2 N -0.1156(3) 0.3174(2) 0.5353(2) 0.0372(7) Uani 1 1 d .
H2A H -0.1096 0.3653 0.5722 0.045 Uiso 1 1 calc R
C2 C -0.2026(4) 0.1998(3) 0.4679(3) 0.0316(8) Uani 1 1 d .
C3 C -0.2332(4) 0.2731(3) 0.5361(3) 0.0363(9) Uani 1 1 d .
N3 N -0.2690(3) -0.1734(2) 0.5231(2) 0.0356(7) Uani 1 1 d .
O3 O 0.1481(3) 0.49049(19) 1.37216(18) 0.0395(6) Uani 1 1 d .
C4 C -0.2428(4) -0.0808(3) 0.4505(3) 0.0344(8) Uani 1 1 d .
N4 N -0.3488(3) -0.1405(2) 0.6100(2) 0.0385(8) Uani 1 1 d .
H4A H -0.3806 -0.1845 0.6682 0.046 Uiso 1 1 calc R
O4 O 0.2616(2) 0.35627(19) 1.30135(19) 0.0387(6) Uani 1 1 d .
C5 C -0.3044(3) 0.0112(3) 0.4929(3) 0.0322(8) Uani 1 1 d .
O5 O 0.4492(3) 0.7669(2) 0.8275(2) 0.0594(8) Uani 1 1 d .
O6 O 0.2046(4) 0.8194(2) 0.8602(2) 0.0652(9) Uani 1 1 d .
C6 C -0.3725(4) -0.0309(3) 0.5943(3) 0.0359(9) Uani 1 1 d .
C7 C -0.2995(4) 0.1310(3) 0.4396(3) 0.0351(9) Uani 1 1 d .
H7A H -0.2741 0.1345 0.3642 0.042 Uiso 1 1 calc R
H7B H -0.3901 0.1633 0.4572 0.042 Uiso 1 1 calc R
C8 C 0.0290(4) 0.1459(4) 0.3468(3) 0.0555(12) Uani 1 1 d .
H8A H 0.1085 0.1882 0.3120 0.083 Uiso 1 1 calc R
H8B H -0.0196 0.1370 0.2962 0.083 Uiso 1 1 calc R
H8C H 0.0554 0.0750 0.3805 0.083 Uiso 1 1 calc R
C9 C -0.3647(4) 0.3092(3) 0.6027(3) 0.0509(11) Uani 1 1 d .
H9A H -0.3631 0.3867 0.6016 0.076 Uiso 1 1 calc R
H9B H -0.3764 0.2700 0.6735 0.076 Uiso 1 1 calc R
H9C H -0.4387 0.2941 0.5754 0.076 Uiso 1 1 calc R
C10 C -0.1577(5) -0.0875(3) 0.3419(3) 0.0589(12) Uani 1 1 d .
H10A H -0.1788 -0.1531 0.3217 0.088 Uiso 1 1 calc R
H10B H -0.0632 -0.0894 0.3418 0.088 Uiso 1 1 calc R
H10C H -0.1769 -0.0244 0.2930 0.088 Uiso 1 1 calc R
C11 C -0.4586(5) 0.0229(3) 0.6793(4) 0.0624(13) Uani 1 1 d .
H11A H -0.5121 -0.0315 0.7321 0.094 Uiso 1 1 calc R
H11B H -0.5175 0.0772 0.6503 0.094 Uiso 1 1 calc R
H11C H -0.4015 0.0575 0.7103 0.094 Uiso 1 1 calc R
C12 C 0.2530(4) 0.4938(3) 0.6599(3) 0.0348(9) Uani 1 1 d .
C13 C 0.1420(4) 0.5292(3) 0.7304(3) 0.0434(10) Uani 1 1 d .
H13A H 0.0563 0.5028 0.7373 0.052 Uiso 1 1 calc R
C14 C 0.1582(4) 0.6038(3) 0.7907(3) 0.0488(11) Uani 1 1 d .
H14A H 0.0834 0.6284 0.8373 0.059 Uiso 1 1 calc R
C15 C 0.2866(4) 0.6415(3) 0.7811(3) 0.0380(9) Uani 1 1 d .
C16 C 0.3983(4) 0.6067(3) 0.7107(3) 0.0407(9) Uani 1 1 d .
H16A H 0.4843 0.6318 0.7050 0.049 Uiso 1 1 calc R
C17 C 0.3807(4) 0.5350(3) 0.6498(3) 0.0404(9) Uani 1 1 d .
H17A H 0.4550 0.5134 0.6008 0.048 Uiso 1 1 calc R
C18 C 0.2351(4) 0.4177(3) 0.5914(3) 0.0344(8) Uani 1 1 d .
C19 C 0.2803(4) 0.6535(3) 0.9875(3) 0.0396(9) Uani 1 1 d .
C20 C 0.3337(5) 0.5474(4) 1.0001(3) 0.0604(13) Uani 1 1 d .
H20A H 0.3836 0.5192 0.9422 0.073 Uiso 1 1 calc R
C21 C 0.3122(5) 0.4838(4) 1.0997(3) 0.0575(12) Uani 1 1 d .
H21A H 0.3475 0.4123 1.1086 0.069 Uiso 1 1 calc R
C22 C 0.2382(4) 0.5256(3) 1.1864(3) 0.0352(9) Uani 1 1 d .
C23 C 0.1853(5) 0.6315(3) 1.1722(3) 0.0518(12) Uani 1 1 d .
H23A H 0.1356 0.6601 1.2299 0.062 Uiso 1 1 calc R
C24 C 0.2055(5) 0.6956(3) 1.0726(3) 0.0526(12) Uani 1 1 d .
H24A H 0.1687 0.7666 1.0634 0.063 Uiso 1 1 calc R
C25 C 0.2147(4) 0.4545(3) 1.2922(3) 0.0337(8) Uani 1 1 d .
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'
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
N3 Ni1 N1 96.46(12) 2_556 .
N3 Ni1 O4 91.61(11) 2_556 1_554
N1 Ni1 O4 100.15(11) . 1_554
N3 Ni1 O1 108.43(11) 2_556 .
N1 Ni1 O1 93.76(11) . .
O4 Ni1 O1 154.17(10) 1_554 .
N3 Ni1 O2 97.44(12) 2_556 .
N1 Ni1 O2 155.30(11) . .
O4 Ni1 O2 99.76(10) 1_554 .
O1 Ni1 O2 62.45(10) . .
N3 Ni1 O3 152.73(11) 2_556 1_554
N1 Ni1 O3 92.50(11) . 1_554
O4 Ni1 O3 61.41(9) 1_554 1_554
O1 Ni1 O3 96.57(10) . 1_554
O2 Ni1 O3 84.34(10) . 1_554
N3 Ni1 C18 108.00(12) 2_556 .
N1 Ni1 C18 124.24(12) . .
O4 Ni1 C18 127.38(12) 1_554 .
O1 Ni1 C18 31.36(10) . .
O2 Ni1 C18 31.34(10) . .
O3 Ni1 C18 87.63(11) 1_554 .
N3 Ni1 C25 122.42(12) 2_556 1_554
N1 Ni1 C25 97.26(12) . 1_554
O4 Ni1 C25 30.90(10) 1_554 1_554
O1 Ni1 C25 125.99(11) . 1_554
O2 Ni1 C25 92.36(11) . 1_554
O3 Ni1 C25 30.51(10) 1_554 1_554
C18 Ni1 C25 109.12(13) . 1_554
O6 S1 O5 118.60(19) . .
O6 S1 C15 109.64(19) . .
O5 S1 C15 107.97(18) . .
O6 S1 C19 108.16(18) . .
O5 S1 C19 108.01(18) . .
C15 S1 C19 103.40(18) . .
C18 O1 Ni1 90.0(2) . .
C1 N1 N2 104.8(3) . .
C1 N1 Ni1 136.7(3) . .
N2 N1 Ni1 118.3(2) . .
N1 C1 C2 111.1(3) . .
N1 C1 C8 120.0(3) . .
C2 C1 C8 128.8(3) . .
C18 O2 Ni1 86.7(2) . .
C3 N2 N1 111.9(3) . .
C3 N2 H2A 124.1 . .
N1 N2 H2A 124.1 . .
C3 C2 C1 104.9(3) . .
C3 C2 C7 127.9(3) . .
C1 C2 C7 127.2(3) . .
N2 C3 C2 107.4(3) . .
N2 C3 C9 119.9(3) . .
C2 C3 C9 132.7(4) . .
C4 N3 N4 105.1(3) . .
C4 N3 Ni1 133.7(2) . 2_556
N4 N3 Ni1 119.0(2) . 2_556
C25 O3 Ni1 86.3(2) . 1_556
N3 C4 C5 110.4(3) . .
N3 C4 C10 119.4(3) . .
C5 C4 C10 130.2(3) . .
C6 N4 N3 112.1(3) . .
C6 N4 H4A 124.0 . .
N3 N4 H4A 124.0 . .
C25 O4 Ni1 92.2(2) . 1_556
C6 C5 C4 105.2(3) . .
C6 C5 C7 126.6(3) . .
C4 C5 C7 128.2(3) . .
N4 C6 C5 107.1(3) . .
N4 C6 C11 121.1(3) . .
C5 C6 C11 131.8(3) . .
C2 C7 C5 115.1(3) . .
C2 C7 H7A 108.5 . .
C5 C7 H7A 108.5 . .
C2 C7 H7B 108.5 . .
C5 C7 H7B 108.5 . .
H7A C7 H7B 107.5 . .
C1 C8 H8A 109.5 . .
C1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C3 C9 H9A 109.5 . .
C3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C4 C10 H10A 109.5 . .
C4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C6 C11 H11A 109.5 . .
C6 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C6 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C13 C12 C17 119.2(3) . .
C13 C12 C18 120.4(3) . .
C17 C12 C18 120.4(3) . .
C12 C13 C14 120.2(4) . .
C12 C13 H13A 119.9 . .
C14 C13 H13A 119.9 . .
C13 C14 C15 119.6(4) . .
C13 C14 H14A 120.2 . .
C15 C14 H14A 120.2 . .
C16 C15 C14 120.6(4) . .
C16 C15 S1 119.5(3) . .
C14 C15 S1 119.8(3) . .
C17 C16 C15 119.3(4) . .
C17 C16 H16A 120.4 . .
C15 C16 H16A 120.4 . .
C16 C17 C12 121.1(4) . .
C16 C17 H17A 119.5 . .
C12 C17 H17A 119.5 . .
O1 C18 O2 119.9(3) . .
O1 C18 C12 120.2(3) . .
O2 C18 C12 119.7(3) . .
O1 C18 Ni1 58.66(18) . .
O2 C18 Ni1 62.00(19) . .
C12 C18 Ni1 168.2(3) . .
C24 C19 C20 120.7(4) . .
C24 C19 S1 120.1(3) . .
C20 C19 S1 119.1(3) . .
C21 C20 C19 119.3(4) . .
C21 C20 H20A 120.3 . .
C19 C20 H20A 120.3 . .
C20 C21 C22 120.6(4) . .
C20 C21 H21A 119.7 . .
C22 C21 H21A 119.7 . .
C23 C22 C21 119.2(3) . .
C23 C22 C25 121.5(3) . .
C21 C22 C25 119.3(3) . .
C22 C23 C24 120.6(4) . .
C22 C23 H23A 119.7 . .
C24 C23 H23A 119.7 . .
C19 C24 C23 119.5(4) . .
C19 C24 H24A 120.2 . .
C23 C24 H24A 120.2 . .
O3 C25 O4 120.0(3) . .
O3 C25 C22 120.6(3) . .
O4 C25 C22 119.4(3) . .
O3 C25 Ni1 63.16(19) . 1_556
O4 C25 Ni1 56.88(18) . 1_556
C22 C25 Ni1 176.2(3) . 1_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 2.026(3) 2_556
Ni1 N1 2.035(3) .
Ni1 O4 2.074(3) 1_554
Ni1 O1 2.078(3) .
Ni1 O2 2.152(3) .
Ni1 O3 2.212(3) 1_554
Ni1 C18 2.433(4) .
Ni1 C25 2.474(4) 1_554
S1 O6 1.434(3) .
S1 O5 1.448(3) .
S1 C15 1.771(4) .
S1 C19 1.774(4) .
O1 C18 1.266(4) .
N1 C1 1.344(4) .
N1 N2 1.361(4) .
C1 C2 1.405(5) .
C1 C8 1.508(5) .
O2 C18 1.267(4) .
N2 C3 1.349(4) .
N2 H2A 0.8600 .
C2 C3 1.379(5) .
C2 C7 1.511(5) .
C3 C9 1.502(5) .
N3 C4 1.345(4) .
N3 N4 1.357(4) .
N3 Ni1 2.026(3) 2_556
O3 C25 1.259(4) .
O3 Ni1 2.212(3) 1_556
C4 C5 1.412(5) .
C4 C10 1.508(5) .
N4 C6 1.349(4) .
N4 H4A 0.8600 .
O4 C25 1.271(4) .
O4 Ni1 2.074(3) 1_556
C5 C6 1.376(5) .
C5 C7 1.516(5) .
C6 C11 1.491(5) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.383(5) .
C12 C17 1.395(5) .
C12 C18 1.490(5) .
C13 C14 1.385(5) .
C13 H13A 0.9300 .
C14 C15 1.387(5) .
C14 H14A 0.9300 .
C15 C16 1.384(5) .
C16 C17 1.369(5) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
C19 C24 1.375(5) .
C19 C20 1.383(5) .
C20 C21 1.382(6) .
C20 H20A 0.9300 .
C21 C22 1.388(5) .
C21 H21A 0.9300 .
C22 C23 1.380(5) .
C22 C25 1.486(5) .
C23 C24 1.385(5) .
C23 H23A 0.9300 .
C24 H24A 0.9300 .
C25 Ni1 2.474(4) 1_556
