#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179355 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/52/4325273.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_4325273
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            'C46 H40 Co4 Mn N6 O2'
_chemical_formula_weight         999.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   13.0256(18)
_cell_length_b                   13.0256(18)
_cell_length_c                   13.993(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2374.1(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_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  0.0832
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15192
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.8510
_exptl_absorpt_correction_T_min  0.7315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       Rhombohedron
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.855
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.94(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2094
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.1015
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2977
_refine_ls_wR_factor_ref         0.3156
_reflns_number_gt                1686
_reflns_number_total             2094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200464t_si_002_7.cif
_cod_data_source_block           9_k07265
_cod_original_cell_volume        2374.2(7)
_cod_database_code               4325273
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Mn1 Mn 0.0000 0.0000 0.0000 0.0332(7) Uani 1 4 d S
Co1 Co 0.28786(14) 0.71198(15) 0.17126(11) 0.0778(8) Uani 1 1 d .
N1 N 0.2403(6) -0.0008(7) -0.0007(10) 0.068(2) Uani 1 1 d .
N2 N 0.0000 0.0000 0.2243(11) 0.072(4) Uani 1 2 d S
C1 C 0.1521(6) 0.0001(6) 0.0011(9) 0.048(2) Uani 1 1 d .
C2 C 0.0000 0.0000 0.1421(9) 0.040(3) Uani 1 2 d S
C3 C 0.2874(11) 0.6921(12) 0.3138(10) 0.106(3) Uani 1 1 d GU
H3 H 0.3167 0.6336 0.3483 0.127 Uiso 1 1 calc R
C4 C 0.3390(11) 0.7842(12) 0.2907(12) 0.121(4) Uani 1 1 d GU
H4 H 0.4107 0.8004 0.3056 0.145 Uiso 1 1 calc R
C5 C 0.2709(14) 0.8465(11) 0.2375(12) 0.124(4) Uani 1 1 d GU
H5 H 0.2866 0.9141 0.2106 0.149 Uiso 1 1 calc R
C6 C 0.1772(12) 0.7928(13) 0.2278(10) 0.118(4) Uani 1 1 d GU
H6 H 0.1158 0.8176 0.1945 0.141 Uiso 1 1 calc R
C7 C 0.1874(11) 0.6974(13) 0.2749(11) 0.116(4) Uani 1 1 d GU
H7 H 0.1345 0.6442 0.2797 0.139 Uiso 1 1 calc R
C8 C 0.3176(17) 0.7534(16) 0.0346(14) 0.148(5) Uani 1 1 d GU
H8 H 0.2859 0.8108 0.0002 0.178 Uiso 1 1 calc R
C9 C 0.4054(17) 0.7544(17) 0.0750(16) 0.148(5) Uani 1 1 d GU
H9 H 0.4507 0.8141 0.0813 0.178 Uiso 1 1 calc R
C10 C 0.4222(16) 0.6649(17) 0.1087(13) 0.141(5) Uani 1 1 d GU
H10 H 0.4844 0.6429 0.1424 0.169 Uiso 1 1 calc R
C11 C 0.3449(18) 0.6087(13) 0.0891(14) 0.146(5) Uani 1 1 d GU
H11 H 0.3404 0.5343 0.0991 0.176 Uiso 1 1 calc R
C12 C 0.2802(14) 0.6633(17) 0.0433(13) 0.151(5) Uani 1 1 d GU
H12 H 0.2181 0.6378 0.0115 0.181 Uiso 1 1 calc R
O2 O 0.5000 0.0000 -0.2500 0.072(5) Uani 1 4 d S
O1 O 0.5000 1.0000 0.2500 0.059(4) Uani 1 4 d S
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3368 0.7283 '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
C1 Mn1 C1 90.001(6) 4 2
C1 Mn1 C1 179.1(8) 4 3
C1 Mn1 C1 90.006(6) 2 3
C1 Mn1 C1 90.005(6) 4 .
C1 Mn1 C1 179.1(8) 2 .
C1 Mn1 C1 90.002(6) 3 .
C1 Mn1 C2 89.5(4) 4 3
C1 Mn1 C2 90.5(4) 2 3
C1 Mn1 C2 89.5(4) 3 3
C1 Mn1 C2 90.5(4) . 3
C1 Mn1 C2 90.5(4) 4 .
C1 Mn1 C2 89.5(4) 2 .
C1 Mn1 C2 90.5(4) 3 .
C1 Mn1 C2 89.5(4) . .
C2 Mn1 C2 180.0 3 .
C12 Co1 C11 39.0(4) . .
C12 Co1 C6 121.5(8) . .
C11 Co1 C6 155.0(9) . .
C12 Co1 C7 128.9(7) . .
C11 Co1 C7 129.2(7) . .
C6 Co1 C7 42.3(3) . .
C12 Co1 C5 136.4(8) . .
C11 Co1 C5 159.6(8) . .
C6 Co1 C5 42.0(3) . .
C7 Co1 C5 70.6(5) . .
C12 Co1 C3 153.0(8) . .
C11 Co1 C3 120.3(7) . .
C6 Co1 C3 70.4(5) . .
C7 Co1 C3 41.6(3) . .
C5 Co1 C3 69.6(5) . .
C12 Co1 C8 37.8(4) . .
C11 Co1 C8 63.1(6) . .
C6 Co1 C8 112.3(7) . .
C7 Co1 C8 148.4(7) . .
C5 Co1 C8 103.1(8) . .
C3 Co1 C8 166.3(8) . .
C12 Co1 C4 161.2(7) . .
C11 Co1 C4 133.7(9) . .
C6 Co1 C4 70.0(5) . .
C7 Co1 C4 69.8(5) . .
C5 Co1 C4 41.1(3) . .
C3 Co1 C4 40.9(3) . .
C8 Co1 C4 126.2(8) . .
C12 Co1 C10 62.8(6) . .
C11 Co1 C10 37.3(4) . .
C6 Co1 C10 164.6(9) . .
C7 Co1 C10 148.8(7) . .
C5 Co1 C10 123.7(8) . .
C3 Co1 C10 112.8(7) . .
C8 Co1 C10 60.9(6) . .
C4 Co1 C10 102.1(7) . .
C12 Co1 C9 61.6(6) . .
C11 Co1 C9 61.4(6) . .
C6 Co1 C9 130.7(8) . .
C7 Co1 C9 168.4(7) . .
C5 Co1 C9 98.4(8) . .
C3 Co1 C9 131.9(7) . .
C8 Co1 C9 35.9(4) . .
C4 Co1 C9 99.5(7) . .
C10 Co1 C9 35.7(4) . .
N1 C1 Mn1 178.2(11) . .
N2 C2 Mn1 180.000(1) . .
C7 C3 C4 108.0 . .
C7 C3 Co1 67.3(6) . .
C4 C3 Co1 70.3(6) . .
C5 C4 C3 108.0 . .
C5 C4 Co1 68.1(5) . .
C3 C4 Co1 68.8(6) . .
C4 C5 C6 108.0 . .
C4 C5 Co1 70.8(5) . .
C6 C5 Co1 67.4(6) . .
C7 C6 C5 108.0 . .
C7 C6 Co1 69.2(6) . .
C5 C6 Co1 70.6(6) . .
C3 C7 C6 108.0 . .
C3 C7 Co1 71.0(6) . .
C6 C7 Co1 68.4(5) . .
C12 C8 C9 108.0 . .
C12 C8 Co1 65.9(8) . .
C9 C8 Co1 75.8(8) . .
C10 C9 C8 108.0 . .
C10 C9 Co1 69.5(7) . .
C8 C9 Co1 68.3(7) . .
C9 C10 C11 108.0 . .
C9 C10 Co1 74.8(8) . .
C11 C10 Co1 65.8(8) . .
C12 C11 C10 108.0 . .
C12 C11 Co1 69.8(8) . .
C10 C11 Co1 76.9(8) . .
C8 C12 C11 108.0 . .
C8 C12 Co1 76.3(9) . .
C11 C12 Co1 71.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 C1 1.982(8) 4
Mn1 C1 1.982(8) 2
Mn1 C1 1.982(8) 3
Mn1 C1 1.982(8) .
Mn1 C2 1.989(12) 3
Mn1 C2 1.989(12) .
Co1 C12 1.902(17) .
Co1 C11 1.919(17) .
Co1 C6 1.952(14) .
Co1 C7 1.962(15) .
Co1 C5 1.994(15) .
Co1 C3 2.011(14) .
Co1 C8 2.02(2) .
Co1 C4 2.031(16) .
Co1 C10 2.050(19) .
Co1 C9 2.11(2) .
N1 C1 1.149(12) .
N2 C2 1.150(19) .
C3 C7 1.413(10) .
C3 C4 1.413(10) .
C4 C5 1.413(10) .
C5 C6 1.413(10) .
C6 C7 1.413(10) .
C8 C12 1.276(13) .
C8 C9 1.276(13) .
C9 C10 1.276(13) .
C10 C11 1.276(13) .
C11 C12 1.276(13) .
