#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:13:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178941 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/70/4117052.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_4117052
loop_
_publ_author_name
'F. Albert Cotton'
'Lee M. Daniels'
'Glenn T. Jordan'
'Carlos A. Murillo'
_publ_section_title
;
 Symmetrical and Unsymmetrical Compounds Having a Linear Co36+ Chain
 Ligated by a Spiral Set of Dipyridyl Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10377
_journal_page_last               10381
_journal_paper_doi               10.1021/ja971997h
_journal_volume                  119
_journal_year                    1997
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C20 H16 Co N6'
_chemical_formula_sum            'C60 H48 Cl2 Co4 N18'
_chemical_formula_weight         1327.8
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.803(8)
_cell_length_b                   13.803(2)
_cell_length_c                   14.9460(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      41.6
_cell_measurement_theta_min      18.1
_cell_volume                     2847.6(17)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'SHELXTL V5 (Siemens, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'area detector'
_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  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16847
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green-brown'
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       'large sphere'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.112
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_obs          0.0393
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+4.2324P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_obs         0.0908
_reflns_number_observed          2111
_reflns_number_total             2532
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971997h_2.cif
_cod_data_source_block           cmpd_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.2324P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+4.2324P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2848(2)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4117052
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.2500 0.2500 0.98413(5) 0.0267(2) Uani 1 d S
Co2 Co 0.2500 0.2500 0.81961(5) 0.0180(2) Uani 1 d S
Co3 Co 0.2500 0.2500 0.66673(5) 0.0192(2) Uani 1 d S
Cl1 Cl 0.2500 0.2500 1.14159(9) 0.0324(4) Uani 1 d S
Cl2 Cl 0.2500 0.2500 0.50706(9) 0.0279(3) Uani 1 d S
N1 N 0.2758(2) 0.1003(2) 0.9610(2) 0.0273(6) Uani 1 d .
N2 N 0.2150(2) 0.1163(2) 0.81849(15) 0.0223(5) Uani 1 d .
N3 N 0.1569(2) 0.1428(2) 0.67616(15) 0.0229(5) Uani 1 d .
C1 C 0.3209(3) 0.0472(3) 1.0245(2) 0.0362(8) Uani 1 d .
H1 H 0.3361(26) 0.0810(25) 1.0774(23) 0.038(10) Uiso 1 d .
C2 C 0.3399(3) -0.0498(3) 1.0154(2) 0.0439(9) Uani 1 d .
H2 H 0.3712(27) -0.0850(28) 1.0605(25) 0.048(11) Uiso 1 d .
C3 C 0.3139(3) -0.0953(3) 0.9366(2) 0.0383(8) Uani 1 d .
H3 H 0.3318(25) -0.1613(27) 0.9276(22) 0.039(10) Uiso 1 d .
C4 C 0.2702(2) -0.0433(2) 0.8698(2) 0.0301(7) Uani 1 d .
H4 H 0.2575(23) -0.0714(24) 0.8148(21) 0.029(9) Uiso 1 d .
C5 C 0.2510(2) 0.0563(2) 0.8829(2) 0.0235(6) Uani 1 d .
C6 C 0.1553(2) 0.0865(2) 0.7510(2) 0.0236(6) Uani 1 d .
C7 C 0.0889(3) 0.0091(2) 0.7564(2) 0.0359(8) Uani 1 d .
H7 H 0.0894(25) -0.0261(26) 0.8073(23) 0.038(10) Uiso 1 d .
C8 C 0.0238(3) -0.0070(3) 0.6895(3) 0.0410(9) Uani 1 d .
H8 H -0.0192(31) -0.0566(31) 0.6990(27) 0.059(12) Uiso 1 d .
C9 C 0.0233(2) 0.0532(3) 0.6157(2) 0.0369(8) Uani 1 d .
H9 H -0.0201(26) 0.0450(25) 0.5710(23) 0.039(10) Uiso 1 d .
C10 C 0.0899(2) 0.1261(2) 0.6115(2) 0.0297(7) Uani 1 d .
H10 H 0.0938(23) 0.1680(24) 0.5631(22) 0.029(8) Uiso 1 d .
Co4 Co 0.7500 0.2500 0.5000 0.0325(2) Uani 1 d S
N4 N 0.6457(2) 0.2425(2) 0.4100(2) 0.0315(6) Uani 1 d .
N5 N 0.7500 0.2500 0.2802(3) 0.0342(9) Uani 1 d S
C11 C 0.5525(3) 0.2358(3) 0.4391(2) 0.0395(8) Uani 1 d .
H11 H 0.5489(23) 0.2344(23) 0.5008(23) 0.029(9) Uiso 1 d .
C12 C 0.4737(3) 0.2311(3) 0.3849(3) 0.0449(9) Uani 1 d .
H12 H 0.4148(31) 0.2240(28) 0.4074(24) 0.047(11) Uiso 1 d .
C13 C 0.4895(3) 0.2327(3) 0.2930(3) 0.0414(8) Uani 1 d .
H13 H 0.4376(28) 0.2260(26) 0.2541(23) 0.040(10) Uiso 1 d .
C14 C 0.5813(3) 0.2389(3) 0.2617(2) 0.0373(8) Uani 1 d .
H14 H 0.5950(26) 0.2421(26) 0.2024(26) 0.044(10) Uiso 1 d .
C15 C 0.6629(2) 0.2441(2) 0.3204(2) 0.0301(7) Uani 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Co1 N1 88.48(2) . 3 y
N1 Co1 N1 161.27(13) . 2 y
N1 Co1 Cl1 99.36(7) . . y
N1 Co1 Co2 80.64(7) . . y
Cl1 Co1 Co2 180.0 . . ?
N2 Co2 N2 89.996(12) 3 . y
N2 Co2 N2 179.00(14) 2 . y
N2 Co2 Co3 89.50(7) . . y
N2 Co2 Co1 90.50(7) . . y
Co3 Co2 Co1 180.0 . . y
N3 Co3 N3 89.70(3) 3 . y
N3 Co3 N3 171.77(13) 2 . y
N3 Co3 Co2 85.89(7) . . y
N3 Co3 Cl2 94.11(7) . . y
Co2 Co3 Cl2 180.0 . . ?
C1 N1 C5 118.5(3) . . ?
C1 N1 Co1 119.4(2) . . ?
C5 N1 Co1 122.1(2) . . ?
C5 N2 C6 123.9(2) . . ?
C5 N2 Co2 119.3(2) . . ?
C6 N2 Co2 116.8(2) . . ?
C10 N3 C6 118.4(3) . . ?
C10 N3 Co3 121.5(2) . . ?
C6 N3 Co3 120.0(2) . . ?
N1 C1 C2 123.3(3) . . ?
C1 C2 C3 118.6(3) . . ?
C4 C3 C2 119.8(3) . . ?
C3 C4 C5 119.5(3) . . ?
N1 C5 N2 115.2(3) . . ?
N1 C5 C4 120.3(3) . . ?
N2 C5 C4 124.2(3) . . ?
N3 C6 N2 115.1(3) . . ?
N3 C6 C7 119.4(3) . . ?
N2 C6 C7 125.3(3) . . ?
C8 C7 C6 120.7(3) . . ?
C7 C8 C9 119.5(3) . . ?
C10 C9 C8 118.4(3) . . ?
N3 C10 C9 123.5(3) . . ?
N4 Co4 N4 94.04(15) 2_655 . y
N4 Co4 N4 117.69(8) . 7_666 y
C15 N4 C11 118.7(3) . . ?
C15 N4 Co4 122.9(2) . . ?
C11 N4 Co4 118.4(2) . . ?
C15 N5 C15 127.0(4) 2_655 . ?
C12 C11 N4 124.7(3) . . ?
C11 C12 C13 117.6(3) . . ?
C14 C13 C12 119.2(3) . . ?
C13 C14 C15 122.0(3) . . ?
N5 C15 N4 126.6(3) . . ?
N5 C15 C14 115.7(3) . . ?
N4 C15 C14 117.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 Co2 2.459(1) y
Co2 Co3 2.285(1) y
Co1 Cl1 2.353(2) y
Co3 Cl2 2.386(2) y
Co1 N1 2.125(3) y
Co2 N2 1.907(3) y
Co3 N3 1.965(3) y
N1 C1 1.350(4) ?
N1 C5 1.361(4) ?
N2 C5 1.364(4) ?
N2 C6 1.366(4) ?
N3 C10 1.357(4) ?
N3 C6 1.362(4) ?
C1 C2 1.371(5) ?
C2 C3 1.383(5) ?
C3 C4 1.369(5) ?
C4 C5 1.414(4) ?
C6 C7 1.410(4) ?
C7 C8 1.362(5) ?
C8 C9 1.381(5) ?
C9 C10 1.364(5) ?
Co4 N4 1.973(3) y
N4 C15 1.361(4) ?
N4 C11 1.361(4) ?
N5 C15 1.346(4) ?
C11 C12 1.357(5) ?
C12 C13 1.391(6) ?
C13 C14 1.353(5) ?
C14 C15 1.430(4) ?
