#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:45:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179392 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/89/4328972.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_4328972
loop_
_publ_author_name
'Yan-Yan Yin'
'Jian-Gong Ma'
'Zheng Niu'
'Xiao-Chang Cao'
'Wei Shi'
'Peng Cheng'
_publ_section_title
;
 Chiral Ni(II) Coordination Polymers: Structure-Driven Effects of
 Temperature and Polyvinylpyrrolidone
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4784
_journal_page_last               4790
_journal_paper_doi               10.1021/ic300106k
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C5 H11 N Ni O7 S'
_chemical_formula_weight         287.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8243(12)
_cell_length_b                   11.735(2)
_cell_length_c                   14.720(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.22
_cell_volume                     1006.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9320
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_T_max  0.6728
_exptl_absorpt_correction_T_min  0.4798
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0333
_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)+(0.0175P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                2206
_reflns_number_total             2394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300106k_si_001_1.cif
_cod_data_source_block           C5H11NNiO7S
_cod_database_code               4328972
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 0.88665(6) 0.36957(3) 0.63704(2) 0.00900(10) Uani 1 1 d .
S1 S 0.58374(14) 0.66235(7) 0.50609(5) 0.01690(18) Uani 1 1 d .
O2 O 0.7527(3) 0.35925(17) 0.50923(12) 0.0118(4) Uani 1 1 d .
O7 O 1.2037(3) 0.34210(18) 0.58177(13) 0.0145(5) Uani 1 1 d .
H7A H 1.3023 0.3509 0.6209 0.022 Uiso 1 1 calc R
H7B H 1.2307 0.2931 0.5496 0.017 Uiso 1 1 d R
O6 O 0.8332(3) 0.19965(17) 0.65155(13) 0.0166(5) Uani 1 1 d .
H6B H 0.9470 0.1648 0.6341 0.025 Uiso 1 1 calc R
H6A H 0.7610 0.1736 0.6895 0.020 Uiso 1 1 d R
N1 N 0.8895(4) 0.54541(19) 0.60799(13) 0.0093(5) Uani 1 1 d .
H8 H 1.0280 0.5759 0.6148 0.011 Uiso 1 1 d R
C3 C 0.7200(5) 0.6012(2) 0.66930(18) 0.0103(7) Uani 1 1 d .
H3 H 0.7996 0.6244 0.7250 0.012 Uiso 1 1 calc R
O4 O 0.3421(3) 0.55590(19) 0.72201(14) 0.0161(5) Uani 1 1 d .
O3 O 0.5731(3) 0.41096(17) 0.68886(12) 0.0109(4) Uani 1 1 d .
C2 C 0.7428(5) 0.4511(3) 0.46499(19) 0.0116(6) Uani 1 1 d .
C5 C 0.6298(5) 0.7079(2) 0.62213(17) 0.0129(6) Uani 1 1 d .
H5A H 0.7413 0.7692 0.6249 0.015 Uiso 1 1 calc R
H5B H 0.4874 0.7335 0.6496 0.015 Uiso 1 1 calc R
O5 O 1.0335(3) 0.39005(18) 0.76452(12) 0.0122(5) Uani 1 1 d .
H5C H 0.9373 0.4153 0.7998 0.018 Uiso 1 1 calc R
H5D H 1.1664 0.4455 0.7532 0.015 Uiso 1 1 d R
O1 O 0.6707(3) 0.45938(18) 0.38526(12) 0.0147(5) Uani 1 1 d .
C1 C 0.8245(5) 0.5610(2) 0.51121(18) 0.0098(6) Uani 1 1 d .
H1 H 0.9554 0.5922 0.4776 0.012 Uiso 1 1 calc R
C4 C 0.5305(5) 0.5168(3) 0.69495(18) 0.0117(7) 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
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O6 Ni1 O3 93.30(8)
O6 Ni1 O2 88.86(8)
O3 Ni1 O2 90.96(7)
O6 Ni1 O7 91.46(8)
O3 Ni1 O7 175.16(8)
O2 Ni1 O7 88.23(8)
O6 Ni1 O5 94.69(8)
O3 Ni1 O5 90.19(7)
O2 Ni1 O5 176.20(9)
O7 Ni1 O5 90.33(8)
O6 Ni1 N1 169.95(8)
O3 Ni1 N1 81.35(9)
O2 Ni1 N1 82.76(8)
O7 Ni1 N1 93.82(8)
O5 Ni1 N1 93.83(8)
C5 S1 C1 92.27(12)
C2 O2 Ni1 116.31(19)
C1 N1 C3 111.0(2)
C1 N1 Ni1 108.26(17)
C3 N1 Ni1 107.58(16)
N1 C3 C5 108.3(2)
N1 C3 C4 110.1(2)
C5 C3 C4 113.3(2)
C4 O3 Ni1 115.78(19)
O1 C2 O2 124.6(3)
O1 C2 C1 117.0(3)
O2 C2 C1 118.4(2)
C3 C5 S1 103.75(18)
N1 C1 C2 113.6(2)
N1 C1 S1 108.26(18)
C2 C1 S1 106.82(19)
O4 C4 O3 123.4(3)
O4 C4 C3 118.2(3)
O3 C4 C3 118.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 O6 2.029(2)
Ni1 O3 2.038(2)
Ni1 O2 2.0402(19)
Ni1 O7 2.0434(19)
Ni1 O5 2.0763(18)
Ni1 N1 2.108(2)
S1 C5 1.810(3)
S1 C1 1.840(3)
O2 C2 1.260(3)
N1 C1 1.485(3)
N1 C3 1.489(3)
C3 C5 1.526(4)
C3 C4 1.530(4)
O4 C4 1.254(3)
O3 C4 1.270(4)
C2 O1 1.250(3)
C2 C1 1.534(4)
