#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:11:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180172 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/68/7106810.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_7106810
loop_
_publ_author_name
'Robert J. Less'
'Thomas C. Wilson'
'Mary McPartlin'
'Paul T. Wood'
'Dominic Wright'
_publ_section_title
;
 Transition metal complexes of the pentacyanocyclopentadienide anion
;
_journal_name_full               Chem.Commun.
_journal_page_first              10007
_journal_paper_doi               10.1039/c1cc13021h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C28 H20 Co N10 O4, C4 H8 O, 2(H2 O)'
_chemical_formula_sum            'C32 H32 Co N10 O7'
_chemical_formula_weight         727.61
_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                107.933(2)
_cell_angle_beta                 98.454(2)
_cell_angle_gamma                101.237(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4871(3)
_cell_length_b                   10.6177(4)
_cell_length_c                   10.7684(4)
_cell_measurement_reflns_used    7449
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      1.00
_cell_volume                     882.97(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8990
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             377
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0388
_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)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                2544
_reflns_number_total             3784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13021h.txt
_cod_data_source_block           dw1061
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106810
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 1.0000 0.03130(16) Uani 1 2 d S . .
O2W O -0.1354(2) 0.12365(16) 0.95208(15) 0.0432(4) Uani 1 1 d . . .
H21W H -0.159(4) 0.131(3) 0.882(3) 0.065 Uiso 1 1 d . . .
H22W H -0.161(4) 0.182(3) 1.001(3) 0.065 Uiso 1 1 d . . .
N1 N -0.1250(2) -0.16287(16) 0.81941(16) 0.0351(4) Uani 1 1 d . . .
N2 N -0.4977(3) -0.5280(2) 0.8156(2) 0.0566(6) Uani 1 1 d . . .
N3 N -0.5411(3) -0.86339(19) 0.4364(2) 0.0560(6) Uani 1 1 d . . .
N4 N -0.2407(3) -0.70958(19) 0.1972(2) 0.0588(6) Uani 1 1 d . . .
N5 N 0.0090(3) -0.26153(19) 0.43127(18) 0.0498(5) Uani 1 1 d . . .
C11 C -0.2344(3) -0.39403(19) 0.62832(19) 0.0319(5) Uani 1 1 d . . .
C12 C -0.3444(3) -0.51148(19) 0.63016(19) 0.0329(5) Uani 1 1 d . . .
C13 C -0.3615(3) -0.61707(19) 0.5087(2) 0.0346(5) Uani 1 1 d . . .
C14 C -0.2667(3) -0.56648(19) 0.43091(19) 0.0351(5) Uani 1 1 d . . .
C15 C -0.1864(3) -0.42775(19) 0.50461(19) 0.0325(5) Uani 1 1 d . . .
C21 C -0.1754(3) -0.2657(2) 0.7339(2) 0.0312(5) Uani 1 1 d . . .
C22 C -0.4272(3) -0.5207(2) 0.7347(2) 0.0390(6) Uani 1 1 d . . .
C23 C -0.4616(3) -0.7536(2) 0.4700(2) 0.0404(6) Uani 1 1 d . . .
C24 C -0.2513(3) -0.6443(2) 0.3003(2) 0.0418(6) Uani 1 1 d . . .
C25 C -0.0773(3) -0.3360(2) 0.46297(19) 0.0362(5) Uani 1 1 d . . .
O1 O 0.17856(18) 0.06582(14) 0.90330(13) 0.0414(4) Uani 1 1 d D . .
C31 C 0.1613(3) 0.0295(3) 0.7596(2) 0.0532(7) Uani 1 1 d D . .
H31A H 0.0596 0.0476 0.7188 0.064 Uiso 1 1 calc R . .
H31B H 0.1565 -0.0687 0.7176 0.064 Uiso 1 1 calc R . .
C32 C 0.3100(3) 0.1172(3) 0.7409(2) 0.0569(7) Uani 1 1 d D . .
H32A H 0.2905 0.2056 0.7390 0.068 Uiso 1 1 calc R . .
H32B H 0.3414 0.0703 0.6570 0.068 Uiso 1 1 calc R . .
C33 C 0.4400(3) 0.1380(3) 0.8612(3) 0.0648(8) Uani 1 1 d D . .
H33A H 0.4949 0.0621 0.8447 0.078 Uiso 1 1 calc R . .
H33B H 0.5241 0.2256 0.8853 0.078 Uiso 1 1 calc R . .
C34 C 0.3468(3) 0.1400(3) 0.9682(2) 0.0581(7) Uani 1 1 d D . .
H34A H 0.3943 0.0960 1.0281 0.070 Uiso 1 1 calc R . .
H34B H 0.3521 0.2354 1.0223 0.070 Uiso 1 1 calc R . .
O1W O -0.2297(2) 0.12733(18) 0.70499(16) 0.0559(5) Uani 1 1 d . . .
H11W H -0.166(4) 0.171(3) 0.658(3) 0.084 Uiso 1 1 d . . .
H12W H -0.287(4) 0.055(3) 0.656(3) 0.084 Uiso 1 1 d . . .
O51 O -0.0680(4) 0.5994(3) 0.9414(3) 0.0476(8) Uiso 0.50 1 d PD A -1
C52 C -0.0850(7) 0.5855(6) 1.0658(6) 0.0511(15) Uiso 0.50 1 d PD A -1
H52A H -0.1901 0.5194 1.0555 0.061 Uiso 0.50 1 calc PR A -1
H52B H -0.0823 0.6747 1.1324 0.061 Uiso 0.50 1 calc PR A -1
C53 C 0.0614(9) 0.5334(7) 1.1093(7) 0.059(2) Uiso 0.50 1 d PD A -1
H53A H 0.0306 0.4686 1.1563 0.071 Uiso 0.50 1 calc PR A -1
H53B H 0.1547 0.6101 1.1690 0.071 Uiso 0.50 1 calc PR A -1
C54 C 0.1052(8) 0.4613(6) 0.9771(5) 0.0557(17) Uiso 0.50 1 d PD A -1
H54A H 0.2187 0.5046 0.9750 0.067 Uiso 0.50 1 calc PR A -1
H54B H 0.0946 0.3630 0.9623 0.067 Uiso 0.50 1 calc PR A -1
C55 C -0.0186(9) 0.4802(6) 0.8757(6) 0.0523(18) Uiso 0.50 1 d PD A -1
H55A H 0.0304 0.4918 0.8007 0.063 Uiso 0.50 1 calc PR A -1
H55B H -0.1147 0.3995 0.8395 0.063 Uiso 0.50 1 calc PR A -1
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'
Co Co 0.3494 0.9721 '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'
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
_geom_angle_publ_flag
O2W Co1 O2W 180.000(1) 2_557 . ?
O2W Co1 O1 89.36(7) 2_557 . ?
O2W Co1 O1 90.64(7) . . ?
O2W Co1 O1 90.64(7) 2_557 2_557 ?
O2W Co1 O1 89.36(7) . 2_557 ?
O1 Co1 O1 180.0 . 2_557 ?
O2W Co1 N1 89.19(7) 2_557 . ?
O2W Co1 N1 90.81(7) . . ?
O1 Co1 N1 90.02(6) . . ?
O1 Co1 N1 89.98(6) 2_557 . ?
O2W Co1 N1 90.81(7) 2_557 2_557 ?
O2W Co1 N1 89.19(7) . 2_557 ?
O1 Co1 N1 89.98(6) . 2_557 ?
O1 Co1 N1 90.02(6) 2_557 2_557 ?
N1 Co1 N1 180.0 . 2_557 ?
Co1 O2W H21W 128(2) . . ?
Co1 O2W H22W 127(2) . . ?
H21W O2W H22W 104(3) . . ?
C21 N1 Co1 165.93(17) . . ?
C15 C11 C12 108.11(16) . . ?
C15 C11 C21 125.31(17) . . ?
C12 C11 C21 126.52(18) . . ?
C13 C12 C11 107.47(17) . . ?
C13 C12 C22 126.01(18) . . ?
C11 C12 C22 126.50(17) . . ?
C14 C13 C12 108.84(16) . . ?
C14 C13 C23 125.55(17) . . ?
C12 C13 C23 125.61(18) . . ?
C13 C14 C15 108.09(16) . . ?
C13 C14 C24 125.33(17) . . ?
C15 C14 C24 126.56(19) . . ?
C11 C15 C14 107.49(17) . . ?
C11 C15 C25 125.46(17) . . ?
C14 C15 C25 127.05(18) . . ?
N1 C21 C11 178.7(2) . . ?
N2 C22 C12 177.8(3) . . ?
N3 C23 C13 178.5(2) . . ?
N4 C24 C14 178.0(2) . . ?
N5 C25 C15 179.0(2) . . ?
C34 O1 C31 108.56(16) . . ?
C34 O1 Co1 124.93(12) . . ?
C31 O1 Co1 126.04(13) . . ?
O1 C31 C32 105.81(18) . . ?
O1 C31 H31A 110.6 . . ?
C32 C31 H31A 110.6 . . ?
O1 C31 H31B 110.6 . . ?
C32 C31 H31B 110.6 . . ?
H31A C31 H31B 108.7 . . ?
C31 C32 C33 103.37(19) . . ?
C31 C32 H32A 111.1 . . ?
C33 C32 H32A 111.1 . . ?
C31 C32 H32B 111.1 . . ?
C33 C32 H32B 111.1 . . ?
H32A C32 H32B 109.1 . . ?
C34 C33 C32 103.7(2) . . ?
C34 C33 H33A 111.0 . . ?
C32 C33 H33A 111.0 . . ?
C34 C33 H33B 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
O1 C34 C33 107.28(19) . . ?
O1 C34 H34A 110.3 . . ?
C33 C34 H34A 110.3 . . ?
O1 C34 H34B 110.3 . . ?
C33 C34 H34B 110.3 . . ?
H34A C34 H34B 108.5 . . ?
H11W O1W H12W 111(3) . . ?
C52 O51 C55 103.0(4) . . ?
O51 C52 C53 105.2(4) . . ?
O51 C52 H52A 110.7 . . ?
C53 C52 H52A 110.7 . . ?
O51 C52 H52B 110.7 . . ?
C53 C52 H52B 110.7 . . ?
H52A C52 H52B 108.8 . . ?
C52 C53 C54 103.5(5) . . ?
C52 C53 H53A 111.1 . . ?
C54 C53 H53A 111.1 . . ?
C52 C53 H53B 111.1 . . ?
C54 C53 H53B 111.1 . . ?
H53A C53 H53B 109.0 . . ?
C55 C54 C53 102.9(5) . . ?
C55 C54 H54A 111.2 . . ?
C53 C54 H54A 111.2 . . ?
C55 C54 H54B 111.2 . . ?
C53 C54 H54B 111.2 . . ?
H54A C54 H54B 109.1 . . ?
O51 C55 C54 107.1(5) . . ?
O51 C55 H55A 110.3 . . ?
C54 C55 H55A 110.3 . . ?
O51 C55 H55B 110.3 . . ?
C54 C55 H55B 110.3 . . ?
H55A C55 H55B 108.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2W 2.0352(17) 2_557 ?
Co1 O2W 2.0352(17) . ?
Co1 O1 2.0901(13) . ?
Co1 O1 2.0901(13) 2_557 ?
Co1 N1 2.1226(16) . ?
Co1 N1 2.1226(17) 2_557 ?
O2W H21W 0.79(3) . ?
O2W H22W 0.77(3) . ?
N1 C21 1.143(2) . ?
N2 C22 1.140(3) . ?
N3 C23 1.143(2) . ?
N4 C24 1.140(3) . ?
N5 C25 1.136(3) . ?
C11 C15 1.411(3) . ?
C11 C12 1.412(3) . ?
C11 C21 1.419(3) . ?
C12 C13 1.402(3) . ?
C12 C22 1.430(3) . ?
C13 C14 1.394(3) . ?
C13 C23 1.429(3) . ?
C14 C15 1.412(3) . ?
C14 C24 1.435(3) . ?
C15 C25 1.431(3) . ?
O1 C34 1.441(3) . ?
O1 C31 1.452(2) . ?
C31 C32 1.493(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.501(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.488(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
O1W H11W 0.95(3) . ?
O1W H12W 0.80(3) . ?
O51 C52 1.417(6) . ?
O51 C55 1.421(7) . ?
C52 C53 1.525(8) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.532(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.488(8) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
