#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325274.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_4325274
loop_
_publ_author_name
'Minao Tang'
'Dongfeng Li'
'Uma Prasad Mallik'
'Yuan-Zhu Zhang'
'Rodolphe Clérac'
'Gordon T. Yee'
'Myung-Hwan Whangbo'
'Amshumali Mungalimane'
'Stephen M. Holmes'
_publ_section_title
;
 Synthesis and Characterization of Di- and Trivalent Pyrazolylborate
 β-Diketonates and Cyanometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5153
_journal_page_last               5164
_journal_paper_doi               10.1021/ic200464t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C50 H38 Co2 F6 N14 O6 S2'
_chemical_formula_weight         1226.92
_chemical_name_common            Co(CN)2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 109.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.282(3)
_cell_length_b                   14.216(3)
_cell_length_c                   12.110(2)
_cell_measurement_temperature    90(2)
_cell_volume                     2478.8(9)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractor'
_diffrn_measurement_method       'ω scans at fixed χ = 55°'
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4183
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_correction_T_min  0.8493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'scalepack (otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0622
_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)+(0.0384P)²+24.3569P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                1637
_reflns_number_total             2194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200464t_si_002_8.cif
_cod_data_source_block           10_k06333
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4325274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.5000 0.30159(7) 0.7500 0.0184(3) Uani 1 2 d S
S1 S 0.23225(16) 0.69547(17) 0.46458(19) 0.0272(6) Uani 0.50 1 d P
O1 O 0.2852(3) 0.6265(3) 0.5465(3) 0.0445(11) Uani 0.50 1 d P
O2 O 0.1393(3) 0.6817(3) 0.4483(3) 0.0517(13) Uani 0.50 1 d P
O3 O 0.2518(3) 0.6883(3) 0.3643(3) 0.0458(11) Uani 0.50 1 d P
C1T C 0.23225(16) 0.69547(17) 0.46458(19) 0.0272(6) Uani 0.50 1 d P
F1 F 0.2852(3) 0.6265(3) 0.5465(3) 0.0445(11) Uani 0.50 1 d P
F2 F 0.1393(3) 0.6817(3) 0.4483(3) 0.0517(13) Uani 0.50 1 d P
F3 F 0.2518(3) 0.6883(3) 0.3643(3) 0.0458(11) Uani 0.50 1 d P
N1 N 0.4767(3) 0.2996(3) 0.5825(4) 0.0216(10) Uani 1 1 d .
N2 N 0.4040(3) 0.2038(3) 0.7108(4) 0.0199(10) Uani 1 1 d .
N3 N 0.3527(4) 0.4528(4) 0.7043(4) 0.0369(13) Uani 1 1 d .
C1 C 0.5147(4) 0.3572(4) 0.5236(5) 0.0283(14) Uani 1 1 d .
H1A H 0.5627 0.3988 0.5664 0.034 Uiso 1 1 calc R
C2 C 0.4864(5) 0.3580(5) 0.4027(5) 0.0357(16) Uani 1 1 d .
H2A H 0.5143 0.3997 0.3629 0.043 Uiso 1 1 calc R
C3 C 0.4175(5) 0.2976(5) 0.3410(5) 0.0381(16) Uani 1 1 d .
H3A H 0.3966 0.2976 0.2578 0.046 Uiso 1 1 calc R
C4 C 0.3785(4) 0.2367(5) 0.4003(5) 0.0328(15) Uani 1 1 d .
H4A H 0.3317 0.1935 0.3584 0.039 Uiso 1 1 calc R
C5 C 0.4085(4) 0.2394(4) 0.5214(5) 0.0235(12) Uani 1 1 d .
C6 C 0.3701(4) 0.1821(4) 0.5946(5) 0.0251(13) Uani 1 1 d .
C7 C 0.3043(4) 0.1126(4) 0.5533(6) 0.0308(14) Uani 1 1 d .
H7A H 0.2821 0.0969 0.4724 0.037 Uiso 1 1 calc R
C8 C 0.2710(4) 0.0662(4) 0.6312(6) 0.0332(15) Uani 1 1 d .
H8A H 0.2246 0.0191 0.6036 0.040 Uiso 1 1 calc R
C9 C 0.3046(4) 0.0877(4) 0.7481(5) 0.0304(14) Uani 1 1 d .
H9A H 0.2824 0.0558 0.8023 0.037 Uiso 1 1 calc R
C10 C 0.3721(4) 0.1575(4) 0.7859(5) 0.0248(13) Uani 1 1 d .
H10A H 0.3962 0.1727 0.8669 0.030 Uiso 1 1 calc R
C11 C 0.4090(4) 0.3960(4) 0.7210(5) 0.0219(12) Uani 1 1 d .
N1S N 0.5000 0.0000 1.0000 0.014(2) Uani 0.50 2 d SPU
C1S C 0.5040(10) 0.0545(9) 1.2184(10) 0.034(3) Uani 0.50 1 d PU
H1SA H 0.5353 0.1134 1.2424 0.051 Uiso 0.50 1 d PR
H1SD H 0.4411 0.0596 1.2174 0.051 Uiso 0.50 1 d PR
H1SB H 0.5355 0.0062 1.2725 0.051 Uiso 0.50 1 d PR
C2S C 0.5053(8) 0.0299(9) 1.0963(11) 0.033(2) Uani 0.50 1 d PU
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'
F F 0.0171 0.0103 '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
C11 Co1 C11 88.8(3) 2_656 .
C11 Co1 N1 94.1(2) 2_656 .
C11 Co1 N1 87.1(2) . .
C11 Co1 N1 87.1(2) 2_656 2_656
C11 Co1 N1 94.1(2) . 2_656
N1 Co1 N1 178.3(3) . 2_656
C11 Co1 N2 177.0(2) 2_656 .
C11 Co1 N2 90.8(2) . .
N1 Co1 N2 82.91(18) . .
N1 Co1 N2 95.90(18) 2_656 .
C11 Co1 N2 90.8(2) 2_656 2_656
C11 Co1 N2 177.0(2) . 2_656
N1 Co1 N2 95.90(18) . 2_656
N1 Co1 N2 82.91(18) 2_656 2_656
N2 Co1 N2 89.7(2) . 2_656
O3 S1 O2 112.8(3) . .
O3 S1 O1 109.1(3) . .
O2 S1 O1 108.5(3) . .
O3 S1 C1T 112.3(3) . 7_566
O2 S1 C1T 109.1(3) . 7_566
O1 S1 C1T 104.7(3) . 7_566
O3 S1 S1 112.3(3) . 7_566
O2 S1 S1 109.1(3) . 7_566
O1 S1 S1 104.7(3) . 7_566
C1T S1 S1 0.00(16) 7_566 7_566
C1 N1 C5 119.1(5) . .
C1 N1 Co1 126.0(4) . .
C5 N1 Co1 114.6(4) . .
C10 N2 C6 119.5(5) . .
C10 N2 Co1 126.6(4) . .
C6 N2 Co1 113.9(4) . .
N1 C1 C2 122.2(6) . .
C3 C2 C1 118.9(6) . .
C2 C3 C4 119.8(6) . .
C3 C4 C5 119.1(6) . .
N1 C5 C4 121.0(5) . .
N1 C5 C6 114.3(5) . .
C4 C5 C6 124.7(5) . .
N2 C6 C7 121.0(5) . .
N2 C6 C5 114.2(5) . .
C7 C6 C5 124.8(5) . .
C6 C7 C8 119.1(6) . .
C9 C8 C7 120.2(5) . .
C8 C9 C10 118.6(6) . .
N2 C10 C9 121.6(5) . .
N3 C11 Co1 178.9(5) . .
C2S N1S C2S 179.997(5) 5_657 .
C1S C1S C2S 164.9(14) 2_657 .
N1S C2S C1S 171.6(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 C11 1.880(6) 2_656
Co1 C11 1.880(6) .
Co1 N1 1.939(4) .
Co1 N1 1.939(4) 2_656
Co1 N2 1.961(4) .
Co1 N2 1.961(4) 2_656
S1 O3 1.348(4) .
S1 O2 1.381(5) .
S1 O1 1.436(4) .
S1 C1T 1.767(5) 7_566
S1 S1 1.767(5) 7_566
N1 C1 1.338(7) .
N1 C5 1.360(7) .
N2 C10 1.338(7) .
N2 C6 1.362(7) .
N3 C11 1.147(7) .
C1 C2 1.381(8) .
C2 C3 1.370(9) .
C3 C4 1.381(9) .
C4 C5 1.383(8) .
C5 C6 1.463(8) .
C6 C7 1.379(8) .
C7 C8 1.381(9) .
C8 C9 1.369(8) .
C9 C10 1.394(8) .
N1S C2S 1.219(13) 5_657
N1S C2S 1.219(14) .
C1S C1S 0.81(2) 2_657
C1S C2S 1.526(16) .
