#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326996.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_4326996
loop_
_publ_author_name
'Luke J. Batchelor'
'Marco Sangalli'
'Régis Guillot'
'Nathalie Guihéry'
'Remi Maurice'
'Floriana Tuna'
'Talal Mallah'
_publ_contact_author_address
;Institut de Chimie Moléculaire et des Matériaux d'Orsay,
UMR8182,
CNRS, 
Université Paris-Sud 11, 
91405 Orsay,
France.
;
_publ_contact_author_email       talal.mallah@u-psud.fr
_publ_contact_author_fax         '(+33) 1 69 15 47 54'
_publ_contact_author_name        'Luke Batchelor'
_publ_contact_author_phone       '(+33) 1 69 15 47 49'
_publ_section_title
;
 Pentanuclear Cyanide-Bridged Complexes Based on Highly Anisotropic CoII
 Seven-Coordinate Building Blocks: Synthesis, Structure, and Magnetic
 Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12045
_journal_page_last               12052
_journal_paper_doi               10.1021/ic201534e
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C23 H23 Co I N5 O3, H2 O, I'
_chemical_formula_sum            'C23 H25 Co I2 N5 O4'
_chemical_formula_weight         748.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.069(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0749(5)
_cell_length_b                   14.2955(8)
_cell_length_c                   22.8291(14)
_cell_measurement_reflns_used    7234
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      34.34
_cell_measurement_theta_min      2.30
_cell_volume                     2602.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            45686
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.63
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    3.071
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         12364
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0274P)²+0.9055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                9146
_reflns_number_total             12364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201534e_si_002_1.cif
_cod_data_source_block           1239GuillotICMMO
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4326996
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C1 C -0.1279(2) 0.36571(12) -0.02020(8) 0.0118(3) Uani 1 1 d .
C2 C -0.2114(2) 0.45126(13) -0.02265(9) 0.0147(4) Uani 1 1 d .
H2 H -0.2206 0.4887 -0.0563 0.018 Uiso 1 1 calc R
C3 C -0.2806(2) 0.47920(13) 0.02657(9) 0.0159(4) Uani 1 1 d .
H3 H -0.3360 0.5363 0.0263 0.019 Uiso 1 1 calc R
C4 C -0.2671(2) 0.42187(13) 0.07599(9) 0.0145(4) Uani 1 1 d .
H4 H -0.3136 0.4395 0.1091 0.017 Uiso 1 1 calc R
C5 C -0.1820(2) 0.33707(13) 0.07505(8) 0.0119(3) Uani 1 1 d .
C6 C -0.1534(2) 0.27043(13) 0.12546(8) 0.0120(3) Uani 1 1 d .
C7 C -0.2265(3) 0.28557(14) 0.18073(9) 0.0163(4) Uani 1 1 d .
H7A H -0.2451 0.2262 0.1983 0.024 Uiso 1 1 calc R
H7B H -0.3312 0.3182 0.1713 0.024 Uiso 1 1 calc R
H7C H -0.1504 0.3220 0.2082 0.024 Uiso 1 1 calc R
C8 C -0.0447(2) 0.32839(13) -0.06873(8) 0.0120(3) Uani 1 1 d .
C9 C -0.0633(3) 0.37766(15) -0.12722(9) 0.0171(4) Uani 1 1 d .
H9A H -0.0219 0.3383 -0.1558 0.026 Uiso 1 1 calc R
H9B H -0.0004 0.4349 -0.1229 0.026 Uiso 1 1 calc R
H9C H -0.1795 0.3914 -0.1405 0.026 Uiso 1 1 calc R
C10 C 0.0912(2) 0.06717(13) 0.13896(8) 0.0115(3) Uani 1 1 d .
C11 C 0.1544(2) -0.00682(13) 0.18229(8) 0.0118(3) Uani 1 1 d .
C12 C 0.1486(3) 0.00241(14) 0.24280(9) 0.0157(4) Uani 1 1 d .
H12 H 0.1088 0.0573 0.2575 0.019 Uiso 1 1 calc R
C13 C 0.2026(3) -0.07068(15) 0.28091(9) 0.0190(4) Uani 1 1 d .
H13 H 0.1979 -0.0650 0.3212 0.023 Uiso 1 1 calc R
C14 C 0.2635(3) -0.15201(15) 0.25929(9) 0.0202(4) Uani 1 1 d .
H14 H 0.2977 -0.2012 0.2850 0.024 Uiso 1 1 calc R
C15 C 0.2738(3) -0.16048(14) 0.19906(10) 0.0194(4) Uani 1 1 d .
H15 H 0.3175 -0.2145 0.1848 0.023 Uiso 1 1 calc R
C16 C 0.1905(2) 0.12353(13) -0.07366(8) 0.0113(3) Uani 1 1 d .
C17 C 0.2734(2) 0.06906(13) -0.11550(8) 0.0116(3) Uani 1 1 d .
C18 C 0.3879(2) 0.00004(13) -0.09244(9) 0.0145(3) Uani 1 1 d .
H18 H 0.4163 -0.0072 -0.0516 0.017 Uiso 1 1 calc R
C19 C 0.4594(2) -0.05793(14) -0.13073(10) 0.0190(4) Uani 1 1 d .
H19 H 0.5375 -0.1030 -0.1155 0.023 Uiso 1 1 calc R
C20 C 0.2184(2) -0.08787(13) 0.16060(9) 0.0146(4) Uani 1 1 d .
H20 H 0.2241 -0.0934 0.1204 0.018 Uiso 1 1 calc R
C21 C 0.4136(3) -0.04817(15) -0.19166(10) 0.0206(4) Uani 1 1 d .
H21 H 0.4586 -0.0882 -0.2172 0.025 Uiso 1 1 calc R
C22 C 0.3017(3) 0.02071(14) -0.21471(9) 0.0187(4) Uani 1 1 d .
H22 H 0.2730 0.0274 -0.2556 0.022 Uiso 1 1 calc R
C23 C 0.2318(2) 0.08020(13) -0.17683(8) 0.0140(3) Uani 1 1 d .
H23 H 0.1577 0.1271 -0.1923 0.017 Uiso 1 1 calc R
N2 N -0.11338(19) 0.31088(10) 0.02797(7) 0.0113(3) Uani 1 1 d .
N3 N -0.0580(2) 0.20217(11) 0.11541(7) 0.0122(3) Uani 1 1 d .
N4 N 0.03698(19) 0.25253(11) -0.05406(7) 0.0111(3) Uani 1 1 d .
N5 N -0.0088(2) 0.13543(11) 0.15705(7) 0.0122(3) Uani 1 1 d .
H5 H -0.0380 0.1360 0.1917 0.015 Uiso 1 1 calc R
N6 N 0.1236(2) 0.20777(11) -0.09287(7) 0.0117(3) Uani 1 1 d .
H6 H 0.1348 0.2310 -0.1268 0.014 Uiso 1 1 calc R
O1 O 0.12530(17) 0.06900(9) 0.08842(6) 0.0136(3) Uani 1 1 d .
O2 O 0.17316(17) 0.09373(9) -0.02391(6) 0.0127(2) Uani 1 1 d .
O3 O -0.17032(17) 0.10624(10) -0.00507(6) 0.016 Uani 1 1 d D
H100 H -0.272(2) 0.1358(14) -0.0124(10) 0.019 Uiso 1 1 d D
H101 H -0.173(3) 0.0454(10) 0.0000(10) 0.019 Uiso 1 1 d D
O4 O 0.54298(19) 0.20337(11) 0.96747(7) 0.022 Uani 1 1 d D
H102 H 0.528(3) 0.2403(16) 0.9345(8) 0.026 Uiso 1 1 d D
H103 H 0.495(3) 0.2332(17) 0.9969(8) 0.026 Uiso 1 1 d D
Co Co 0.03796(3) 0.186447(17) 0.031526(11) 0.01017(5) Uani 1 1 d .
I1 I 0.319853(15) 0.293300(8) 0.075475(5) 0.01374(3) Uani 1 1 d .
I2 I 0.399533(16) 0.351184(9) 0.841108(6) 0.01671(3) 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
C C 0.0031 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 0.0109 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3495 0.9722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4743 1.8119 '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
N2 C1 C2 121.68(17)
N2 C1 C8 114.30(15)
C2 C1 C8 124.01(17)
C3 C2 C1 118.26(18)
C4 C3 C2 119.88(17)
C3 C4 C5 118.53(18)
N2 C5 C4 121.52(17)
N2 C5 C6 114.19(16)
C4 C5 C6 124.25(17)
N3 C6 C5 111.91(16)
N3 C6 C7 126.12(17)
C5 C6 C7 121.95(16)
N4 C8 C1 112.52(16)
N4 C8 C9 127.20(17)
C1 C8 C9 120.27(16)
O1 C10 N5 119.84(17)
O1 C10 C11 122.54(17)
N5 C10 C11 117.62(16)
C20 C11 C12 120.21(17)
C20 C11 C10 117.68(17)
C12 C11 C10 122.11(17)
C13 C12 C11 119.61(18)
C14 C13 C12 120.27(19)
C13 C14 C15 120.27(19)
C20 C15 C14 119.69(19)
O2 C16 N6 120.08(16)
O2 C16 C17 122.70(16)
N6 C16 C17 117.13(16)
C18 C17 C23 119.92(17)
C18 C17 C16 118.07(17)
C23 C17 C16 121.85(17)
C19 C18 C17 119.89(19)
C21 C19 C18 119.82(19)
C15 C20 C11 119.90(18)
C22 C21 C19 120.48(19)
C21 C22 C23 120.16(19)
C22 C23 C17 119.69(18)
C5 N2 C1 120.12(16)
C5 N2 Co 120.37(12)
C1 N2 Co 119.32(12)
C6 N3 N5 121.62(16)
C6 N3 Co 122.61(13)
N5 N3 Co 115.76(11)
C8 N4 N6 121.22(16)
C8 N4 Co 122.06(12)
N6 N4 Co 116.69(11)
N3 N5 C10 114.17(15)
C16 N6 N4 114.90(15)
C10 O1 Co 118.61(12)
C16 O2 Co 116.77(12)
O3 Co N2 91.26(6)
O3 Co N4 89.45(6)
N2 Co N4 71.62(6)
O3 Co O1 88.85(5)
N2 Co O1 142.24(6)
N4 Co O1 146.13(5)
O3 Co N3 91.85(6)
N2 Co N3 70.77(6)
N4 Co N3 142.39(6)
O1 Co N3 71.48(5)
O3 Co O2 83.26(5)
N2 Co O2 142.62(6)
N4 Co O2 71.38(5)
O1 Co O2 74.83(5)
N3 Co O2 146.04(5)
O3 Co I1 177.53(4)
N2 Co I1 89.27(4)
N4 Co I1 88.42(4)
O1 Co I1 92.21(4)
N3 Co I1 90.60(4)
O2 Co I1 94.86(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N2 1.340(2)
C1 C2 1.394(3)
C1 C8 1.482(3)
C2 C3 1.390(3)
C3 C4 1.385(3)
C4 C5 1.395(3)
C5 N2 1.338(2)
C5 C6 1.484(3)
C6 N3 1.286(2)
C6 C7 1.491(3)
C8 N4 1.286(2)
C8 C9 1.496(3)
C10 O1 1.228(2)
C10 N5 1.371(2)
C10 C11 1.483(3)
C11 C20 1.391(3)
C11 C12 1.396(3)
C12 C13 1.385(3)
C13 C14 1.383(3)
C14 C15 1.396(3)
C15 C20 1.387(3)
C16 O2 1.241(2)
C16 N6 1.364(2)
C16 C17 1.473(3)
C17 C18 1.397(3)
C17 C23 1.397(3)
C18 C19 1.394(3)
C19 C21 1.389(3)
C21 C22 1.383(3)
C22 C23 1.394(3)
N2 Co 2.1524(15)
N3 N5 1.361(2)
N3 Co 2.1877(16)
N4 N6 1.371(2)
N4 Co 2.1690(16)
O1 Co 2.1712(13)
O2 Co 2.2329(13)
O3 Co 2.0972(14)
Co I1 2.7931(3)
