#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330417.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_4330417
loop_
_publ_author_name
'Kamal Kumar Bisht'
'Eringathodi Suresh'
_publ_section_title
;
 Spontaneous Resolution of a Mixed-Ligand Nickel(II) Coordination Polymer
 with Achiral Precursors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9577
_journal_page_last               9579
_journal_paper_doi               10.1021/ic301636z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C21 H15 Cd N2 O6 S'
_chemical_formula_weight         535.81
_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                110.340(3)
_cell_angle_beta                 99.638(4)
_cell_angle_gamma                93.412(4)
_cell_formula_units_Z            2
_cell_length_a                   6.9316(16)
_cell_length_b                   13.157(3)
_cell_length_c                   13.476(3)
_cell_measurement_reflns_used    3640
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.73
_cell_volume                     1126.9(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4584
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.7782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       PLATES
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.799
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0403
_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)+(0.0666P)²+2.6667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3688
_reflns_number_total             3883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301636z_si_002_5.cif
_cod_data_source_block           kl106fComp4Cd
_cod_database_code               4330417
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
Cd1 Cd 0.20907(4) 0.53586(2) 0.07976(2) 0.01604(13) Uani 1 1 d .
S1 S -0.38271(18) 0.11491(8) 0.36793(8) 0.0213(2) Uani 1 1 d .
O1 O 0.0616(5) 0.4247(3) 0.1477(3) 0.0285(7) Uani 1 1 d .
O2 O -0.2379(5) 0.3845(2) 0.0401(2) 0.0245(7) Uani 1 1 d .
O3 O -0.2563(5) 0.1534(2) 0.4743(2) 0.0283(7) Uani 1 1 d .
O5 O -0.0031(5) -0.3444(3) 0.1379(3) 0.0259(7) Uani 1 1 d .
O4 O -0.5938(5) 0.1119(2) 0.3577(3) 0.0266(7) Uani 1 1 d .
O6 O -0.2974(5) -0.3823(2) 0.0262(3) 0.0291(8) Uani 1 1 d .
N1 N 0.4388(5) 0.6122(3) 0.2268(3) 0.0158(7) Uani 1 1 d .
N2 N 0.7289(5) 0.6452(3) 0.3331(3) 0.0176(7) Uani 1 1 d .
C1 C -0.1113(7) 0.3785(3) 0.1165(4) 0.0201(9) Uani 1 1 d .
C2 C -0.1808(7) 0.3124(3) 0.1787(3) 0.0196(9) Uani 1 1 d .
C3 C -0.0429(7) 0.2856(4) 0.2510(4) 0.0244(9) Uani 1 1 d .
H3 H 0.0906 0.3085 0.2603 0.029 Uiso 1 1 calc R
C4 C -0.1032(7) 0.2252(4) 0.3089(4) 0.0239(9) Uani 1 1 d .
H4 H -0.0116 0.2062 0.3561 0.029 Uiso 1 1 calc R
C5 C -0.3051(7) 0.1934(3) 0.2947(3) 0.0216(9) Uani 1 1 d .
C6 C -0.4419(7) 0.2201(3) 0.2245(4) 0.0231(9) Uani 1 1 d .
H6 H -0.5756 0.1982 0.2162 0.028 Uiso 1 1 calc R
C7 C -0.3802(7) 0.2795(3) 0.1659(4) 0.0217(9) Uani 1 1 d .
H7 H -0.4724 0.2974 0.1180 0.026 Uiso 1 1 calc R
C8 C -0.3273(7) -0.0164(3) 0.2959(3) 0.0185(9) Uani 1 1 d .
C9 C -0.1434(7) -0.0446(4) 0.3251(4) 0.0261(10) Uani 1 1 d .
H9 H -0.0537 0.0030 0.3849 0.031 Uiso 1 1 calc R
C10 C -0.0938(8) -0.1446(4) 0.2642(4) 0.0270(10) Uani 1 1 d .
H10 H 0.0293 -0.1646 0.2835 0.032 Uiso 1 1 calc R
C11 C -0.2280(7) -0.2148(3) 0.1744(3) 0.0200(9) Uani 1 1 d .
C12 C -0.4136(7) -0.1861(3) 0.1475(3) 0.0206(9) Uani 1 1 d .
H12 H -0.5049 -0.2345 0.0889 0.025 Uiso 1 1 calc R
C13 C -0.4637(7) -0.0862(3) 0.2072(4) 0.0221(9) Uani 1 1 d .
H13 H -0.5868 -0.0661 0.1881 0.026 Uiso 1 1 calc R
C14 C -0.1717(7) -0.3228(3) 0.1069(4) 0.0243(10) Uani 1 1 d .
C15 C 0.6149(6) 0.5813(3) 0.2386(3) 0.0164(8) Uani 1 1 d .
H15 H 0.6554 0.5226 0.1879 0.020 Uiso 1 1 calc R
C16 C 0.4377(7) 0.6991(3) 0.3205(3) 0.0190(8) Uani 1 1 d .
H16 H 0.3310 0.7374 0.3357 0.023 Uiso 1 1 calc R
C17 C 0.6170(7) 0.7200(3) 0.3871(3) 0.0203(9) Uani 1 1 d .
H17 H 0.6561 0.7741 0.4554 0.024 Uiso 1 1 calc R
C18 C 0.9340(7) 0.6355(4) 0.3702(4) 0.0240(9) Uani 1 1 d .
H18A H 1.0031 0.7081 0.4124 0.029 Uiso 1 1 calc R
H18B H 0.9936 0.6057 0.3076 0.029 Uiso 1 1 calc R
C19 C 0.9638(7) 0.5644(4) 0.4377(3) 0.0206(9) Uani 1 1 d .
C20 C 0.8088(7) 0.5164(4) 0.4657(4) 0.0245(9) Uani 1 1 d .
H20 H 0.6799 0.5271 0.4429 0.029 Uiso 1 1 calc R
C21 C 1.1537(7) 0.5473(4) 0.4722(4) 0.0240(9) Uani 1 1 d .
H21 H 1.2583 0.5793 0.4535 0.029 Uiso 1 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'
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'
H H 0.0000 0.0000 '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'
Cd Cd -0.8075 1.2024 '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 Cd1 O6 109.89(13) . 2
N1 Cd1 O2 110.65(12) . 2_565
O6 Cd1 O2 91.18(12) 2 2_565
N1 Cd1 O5 94.03(13) . 1_565
O6 Cd1 O5 155.22(14) 2 1_565
O2 Cd1 O5 86.15(11) 2_565 1_565
N1 Cd1 O1 93.46(12) . .
O6 Cd1 O1 83.91(13) 2 .
O2 Cd1 O1 155.58(13) 2_565 .
O5 Cd1 O1 88.41(12) 1_565 .
N1 Cd1 Cd1 161.43(9) . 2_565
O6 Cd1 Cd1 86.44(10) 2 2_565
O2 Cd1 Cd1 76.68(9) 2_565 2_565
O5 Cd1 Cd1 68.95(9) 1_565 2_565
O1 Cd1 Cd1 79.15(9) . 2_565
O4 S1 O3 119.8(2) . .
O4 S1 C8 109.1(2) . .
O3 S1 C8 107.5(2) . .
O4 S1 C5 108.1(2) . .
O3 S1 C5 108.5(2) . .
C8 S1 C5 102.57(19) . .
C1 O1 Cd1 126.7(3) . .
C1 O2 Cd1 130.6(3) . 2_565
C14 O5 Cd1 140.3(3) . 1_545
C14 O6 Cd1 117.4(3) . 2
C15 N1 C16 106.0(3) . .
C15 N1 Cd1 123.5(3) . .
C16 N1 Cd1 130.4(3) . .
C15 N2 C17 107.6(4) . .
C15 N2 C18 125.4(4) . .
C17 N2 C18 127.0(4) . .
O1 C1 O2 126.5(4) . .
O1 C1 C2 117.1(4) . .
O2 C1 C2 116.3(4) . .
C7 C2 C3 119.8(4) . .
C7 C2 C1 120.5(4) . .
C3 C2 C1 119.6(4) . .
C4 C3 C2 120.6(4) . .
C3 C4 C5 118.5(4) . .
C6 C5 C4 121.4(4) . .
C6 C5 S1 120.1(4) . .
C4 C5 S1 118.6(3) . .
C5 C6 C7 119.8(4) . .
C6 C7 C2 119.9(4) . .
C9 C8 C13 121.4(4) . .
C9 C8 S1 119.0(3) . .
C13 C8 S1 119.5(3) . .
C8 C9 C10 119.4(4) . .
C9 C10 C11 119.9(4) . .
C12 C11 C10 120.0(4) . .
C12 C11 C14 120.3(4) . .
C10 C11 C14 119.7(4) . .
C13 C12 C11 120.5(4) . .
C12 C13 C8 118.9(4) . .
O6 C14 O5 126.3(4) . .
O6 C14 C11 117.0(4) . .
O5 C14 C11 116.7(4) . .
N1 C15 N2 111.2(4) . .
C17 C16 N1 109.2(4) . .
C16 C17 N2 106.0(4) . .
N2 C18 C19 114.6(4) . .
C21 C19 C20 119.1(4) . .
C21 C19 C18 118.2(4) . .
C20 C19 C18 122.7(4) . .
C21 C20 C19 119.8(4) 2_766 .
C19 C21 C20 121.2(4) . 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N1 2.200(3) .
Cd1 O6 2.221(3) 2
Cd1 O2 2.237(3) 2_565
Cd1 O5 2.249(3) 1_565
Cd1 O1 2.255(3) .
Cd1 Cd1 3.1765(8) 2_565
S1 O4 1.443(4) .
S1 O3 1.449(3) .
S1 C8 1.764(4) .
S1 C5 1.775(4) .
O1 C1 1.245(6) .
O2 C1 1.264(5) .
O2 Cd1 2.237(3) 2_565
O5 C14 1.257(6) .
O5 Cd1 2.249(3) 1_545
O6 C14 1.250(6) .
O6 Cd1 2.221(3) 2
N1 C15 1.311(6) .
N1 C16 1.380(5) .
N2 C15 1.339(5) .
N2 C17 1.371(5) .
N2 C18 1.454(6) .
C1 C2 1.513(6) .
C2 C7 1.387(6) .
C2 C3 1.398(7) .
C3 C4 1.384(6) .
C4 C5 1.398(7) .
C5 C6 1.374(7) .
C6 C7 1.386(6) .
C8 C9 1.382(7) .
C8 C13 1.386(6) .
C9 C10 1.385(6) .
C10 C11 1.388(7) .
C11 C12 1.388(7) .
C11 C14 1.511(6) .
C12 C13 1.381(6) .
C16 C17 1.356(6) .
C18 C19 1.516(6) .
C19 C21 1.380(7) .
C19 C20 1.384(6) .
C20 C21 1.383(6) 2_766
C21 C20 1.383(6) 2_766
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.006 0.000 0.000 150.3 27.3
2 0.389 0.433 0.306 7.3 -0.1
3 0.611 0.567 0.694 7.3 -0.1
