#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:19:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179407 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/04/4330415.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_4330415
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 Co N2 O6 S'
_chemical_formula_weight         482.34
_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                109.740(6)
_cell_angle_beta                 102.105(6)
_cell_angle_gamma                92.279(6)
_cell_formula_units_Z            2
_cell_length_a                   7.097(2)
_cell_length_b                   12.877(5)
_cell_length_c                   13.116(5)
_cell_measurement_reflns_used    2465
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      2.45
_cell_volume                     1095.1(7)
_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 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9320
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            'WINE RED''
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       PLATES
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0535P)²+3.3804P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                4207
_reflns_number_total             4919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301636z_si_002_3.cif
_cod_data_source_block           kl102mComp2Co
_cod_database_code               4330415
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
Co1 Co 0.31215(8) -0.02828(4) 0.42555(5) 0.00941(16) Uani 1 1 d .
S1 S 0.85884(16) 0.38283(8) 0.12965(9) 0.0150(2) Uani 1 1 d .
O1 O 0.4396(4) 0.0682(2) 0.3555(2) 0.0167(6) Uani 1 1 d .
O2 O 0.7343(4) 0.1089(2) 0.4707(2) 0.0157(6) Uani 1 1 d .
O3 O 0.7306(5) 0.3443(3) 0.0201(3) 0.0219(7) Uani 1 1 d .
O4 O 1.0648(5) 0.3838(2) 0.1409(3) 0.0204(7) Uani 1 1 d .
O5 O 0.4949(4) 0.8515(3) 0.3694(3) 0.0185(7) Uani 1 1 d .
O6 O 0.7877(4) 0.8880(2) 0.4853(2) 0.0171(7) Uani 1 1 d .
N1 N 0.0949(5) -0.1020(3) 0.2873(3) 0.0115(7) Uani 1 1 d .
N2 N -0.1984(5) -0.1392(3) 0.1777(3) 0.0126(7) Uani 1 1 d .
C1 C 0.6093(6) 0.1151(3) 0.3894(3) 0.0130(8) Uani 1 1 d .
C2 C 0.6726(6) 0.1826(3) 0.3255(3) 0.0140(8) Uani 1 1 d .
C3 C 0.5345(7) 0.2110(3) 0.2510(4) 0.0167(9) Uani 1 1 d .
H3 H 0.4036 0.1890 0.2415 0.020 Uiso 1 1 calc R
C4 C 0.5900(6) 0.2720(3) 0.1902(4) 0.0165(9) Uani 1 1 d .
H4 H 0.4973 0.2915 0.1404 0.020 Uiso 1 1 calc R
C5 C 0.7874(6) 0.3036(3) 0.2056(3) 0.0141(8) Uani 1 1 d .
C6 C 0.9272(7) 0.2747(4) 0.2790(4) 0.0163(9) Uani 1 1 d .
H6 H 1.0582 0.2956 0.2876 0.020 Uiso 1 1 calc R
C7 C 0.8702(6) 0.2141(3) 0.3397(3) 0.0152(9) Uani 1 1 d .
H7 H 0.9628 0.1946 0.3894 0.018 Uiso 1 1 calc R
C8 C 0.8071(6) 0.5175(3) 0.2030(3) 0.0130(8) Uani 1 1 d .
C9 C 0.6221(7) 0.5453(4) 0.1756(4) 0.0217(10) Uani 1 1 d .
H9 H 0.5295 0.4968 0.1151 0.026 Uiso 1 1 calc R
C10 C 0.5766(6) 0.6467(4) 0.2399(4) 0.0189(9) Uani 1 1 d .
H10 H 0.4520 0.6660 0.2229 0.023 Uiso 1 1 calc R
C11 C 0.7149(6) 0.7195(3) 0.3291(3) 0.0124(8) Uani 1 1 d .
C12 C 0.9035(6) 0.6921(3) 0.3531(3) 0.0141(8) Uani 1 1 d .
H12 H 0.9981 0.7422 0.4111 0.017 Uiso 1 1 calc R
C13 C 0.9491(6) 0.5908(4) 0.2907(3) 0.0144(9) Uani 1 1 d .
H13 H 1.0739 0.5716 0.3071 0.017 Uiso 1 1 calc R
C14 C 0.6620(7) 0.8282(3) 0.4003(4) 0.0153(9) Uani 1 1 d .
C15 C -0.0857(6) -0.0744(4) 0.2770(4) 0.0158(9) Uani 1 1 d .
H15 H -0.1275 -0.0185 0.3307 0.019 Uiso 1 1 calc R
C16 C 0.0935(6) -0.1884(3) 0.1887(4) 0.0151(9) Uani 1 1 d .
H16 H 0.2000 -0.2247 0.1720 0.018 Uiso 1 1 calc R
C17 C -0.0854(6) -0.2113(3) 0.1211(3) 0.0140(8) Uani 1 1 d .
H17 H -0.1251 -0.2653 0.0502 0.017 Uiso 1 1 calc R
C18 C -0.4042(6) -0.1337(4) 0.1392(4) 0.0162(9) Uani 1 1 d .
H18A H -0.4589 -0.1044 0.2036 0.019 Uiso 1 1 calc R
H18B H -0.4682 -0.2085 0.0968 0.019 Uiso 1 1 calc R
C19 C -0.4478(6) -0.0629(3) 0.0678(3) 0.0144(8) Uani 1 1 d .
C20 C -0.3069(6) -0.0128(4) 0.0351(4) 0.0148(8) Uani 1 1 d .
H20 H -0.1770 -0.0209 0.0584 0.018 Uiso 1 1 calc R
C21 C -0.6415(6) -0.0496(4) 0.0324(4) 0.0166(9) Uani 1 1 d .
H21 H -0.7372 -0.0828 0.0540 0.020 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'
Co Co 0.3494 0.9721 '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 Co1 O6 104.97(13) . 2_666
N1 Co1 O2 103.05(13) . 2_656
O6 Co1 O2 92.68(12) 2_666 2_656
N1 Co1 O1 93.91(13) . .
O6 Co1 O1 87.12(13) 2_666 .
O2 Co1 O1 162.47(12) 2_656 .
N1 Co1 O5 92.30(13) . 1_545
O6 Co1 O5 162.37(13) 2_666 1_545
O2 Co1 O5 86.75(12) 2_656 1_545
O1 Co1 O5 88.18(13) . 1_545
N1 Co1 Co1 161.13(10) . 2_656
O6 Co1 Co1 92.99(9) 2_666 2_656
O2 Co1 Co1 81.44(9) 2_656 2_656
O1 Co1 Co1 81.06(9) . 2_656
O5 Co1 Co1 69.48(9) 1_545 2_656
O4 S1 O3 119.5(2) . .
O4 S1 C8 109.4(2) . .
O3 S1 C8 107.7(2) . .
O4 S1 C5 108.1(2) . .
O3 S1 C5 108.3(2) . .
C8 S1 C5 102.48(19) . .
C1 O1 Co1 125.8(3) . .
C1 O2 Co1 125.8(3) . 2_656
C14 O5 Co1 139.6(3) . 1_565
C14 O6 Co1 112.6(3) . 2_666
C15 N1 C16 105.9(3) . .
C15 N1 Co1 123.7(3) . .
C16 N1 Co1 130.4(3) . .
C15 N2 C17 108.0(3) . .
C15 N2 C18 125.1(4) . .
C17 N2 C18 126.8(3) . .
O1 C1 O2 125.9(4) . .
O1 C1 C2 116.9(4) . .
O2 C1 C2 117.2(4) . .
C3 C2 C7 120.3(4) . .
C3 C2 C1 119.6(4) . .
C7 C2 C1 120.1(4) . .
C2 C3 C4 120.5(4) . .
C3 C4 C5 118.7(4) . .
C6 C5 C4 121.3(4) . .
C6 C5 S1 119.8(3) . .
C4 C5 S1 118.9(3) . .
C5 C6 C7 119.5(4) . .
C6 C7 C2 119.7(4) . .
C9 C8 C13 121.2(4) . .
C9 C8 S1 118.9(3) . .
C13 C8 S1 119.7(3) . .
C8 C9 C10 118.9(4) . .
C11 C10 C9 120.6(4) . .
C10 C11 C12 119.8(4) . .
C10 C11 C14 120.1(4) . .
C12 C11 C14 120.1(4) . .
C13 C12 C11 119.9(4) . .
C12 C13 C8 119.5(4) . .
O5 C14 O6 125.2(4) . .
O5 C14 C11 116.9(4) . .
O6 C14 C11 117.9(4) . .
N1 C15 N2 110.2(4) . .
C17 C16 N1 109.5(4) . .
C16 C17 N2 106.4(4) . .
N2 C18 C19 114.2(4) . .
C20 C19 C21 119.1(4) . .
C20 C19 C18 123.6(4) . .
C21 C19 C18 117.3(4) . .
C19 C20 C21 120.4(4) . 2_455
C20 C21 C19 120.6(4) 2_455 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.028(3) .
Co1 O6 2.038(3) 2_666
Co1 O2 2.039(3) 2_656
Co1 O1 2.058(3) .
Co1 O5 2.100(3) 1_545
Co1 Co1 2.8557(13) 2_656
S1 O4 1.437(3) .
S1 O3 1.440(3) .
S1 C8 1.772(4) .
S1 C5 1.774(4) .
O1 C1 1.244(5) .
O2 C1 1.263(5) .
O2 Co1 2.039(3) 2_656
O5 C14 1.253(5) .
O5 Co1 2.100(3) 1_565
O6 C14 1.257(5) .
O6 Co1 2.038(3) 2_666
N1 C15 1.335(5) .
N1 C16 1.391(5) .
N2 C15 1.345(5) .
N2 C17 1.379(5) .
N2 C18 1.455(5) .
C1 C2 1.510(6) .
C2 C3 1.384(6) .
C2 C7 1.400(6) .
C3 C4 1.393(6) .
C4 C5 1.396(6) .
C5 C6 1.386(6) .
C6 C7 1.391(6) .
C8 C9 1.381(6) .
C8 C13 1.391(6) .
C9 C10 1.388(6) .
C10 C11 1.384(6) .
C11 C12 1.396(6) .
C11 C14 1.509(6) .
C12 C13 1.379(6) .
C16 C17 1.344(6) .
C18 C19 1.511(6) .
C19 C20 1.384(6) .
C19 C21 1.393(6) .
C20 C21 1.389(6) 2_455
C21 C20 1.389(6) 2_455
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 -0.056 0.500 0.500 144.5 30.7
