#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:13:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178941 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/70/4117053.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_4117053
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_structural     'Co3(dpa)4BF4Cl, 2(CH2Cl2)'
_chemical_formula_sum            'C42 H36 B Cl5 Co3 F4 N12'
_chemical_formula_weight         1149.68
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.777(7)
_cell_length_b                   16.538(2)
_cell_length_c                   15.455(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      17.7
_cell_measurement_theta_min      9.0
_cell_volume                     4518(3)
_computing_cell_refinement       'CAD4 V5.0'
_computing_data_collection       'CAD4 V5.0'
_computing_data_reduction        XCAD4
_computing_molecular_graphics    'SHELXTL (Siemens, 1990)'
_computing_publication_material  'SHELXTL (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3078
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.142
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_obs          0.0422
_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)+(0.0527P)²+3.5482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1135
_refine_ls_wR_factor_obs         0.0954
_reflns_number_observed          1915
_reflns_number_total             2947
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971997h_3.cif
_cod_data_source_block           cmpd_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+3.5482P] 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^)+(0.0527P)^2^+3.5482P] 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        4517.6(25)
_cod_database_code               4117053
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.5000 0.62551(7) 0.2500 0.0288(3) Uani 1 d S .
Co2 Co 0.5000 0.77692(6) 0.2500 0.0206(3) Uani 1 d S .
Co3 Co 0.5000 0.91458(6) 0.2500 0.0221(3) Uani 1 d S .
Cl1 Cl 0.5000 0.48214(12) 0.2500 0.0383(6) Uani 1 d S .
F1 F 0.5000 1.0490(3) 0.2500 0.0387(13) Uani 1 d SD .
B1 B 0.5095(12) 1.1352(9) 0.2561(16) 0.039(5) Uani 0.50 d PD -1
F2 F 0.5772(7) 1.1523(6) 0.3152(17) 0.103(5) Uani 0.50 d PD -1
F3 F 0.4536(11) 1.1647(9) 0.2817(20) 0.101(9) Uani 0.50 d PD -1
F4 F 0.5028(20) 1.1600(9) 0.1722(14) 0.126(10) Uani 0.50 d PD -1
N1 N 0.5454(2) 0.6446(3) 0.3964(3) 0.0228(11) Uani 1 d . .
N2 N 0.5666(2) 0.7799(3) 0.3747(3) 0.0225(11) Uani 1 d . .
N3 N 0.5980(2) 0.9093(3) 0.3468(3) 0.0217(11) Uani 1 d . .
N4 N 0.6103(2) 0.6434(3) 0.2491(3) 0.0243(11) Uani 1 d . .
N5 N 0.5846(2) 0.7774(3) 0.2080(3) 0.0226(11) Uani 1 d . .
N6 N 0.5542(2) 0.9097(3) 0.1626(3) 0.0232(11) Uani 1 d . .
C1 C 0.5502(4) 0.5820(4) 0.4545(5) 0.031(2) Uani 1 d . .
H1 H 0.5340(32) 0.5424(35) 0.4255(39) 0.031 Uiso 1 d . .
C2 C 0.5733(4) 0.5885(4) 0.5474(5) 0.035(2) Uani 1 d . .
H2 H 0.5798(35) 0.5498(36) 0.5795(41) 0.035 Uiso 1 d . .
C3 C 0.5893(3) 0.6641(4) 0.5853(5) 0.036(2) Uani 1 d . .
H3 H 0.5997(32) 0.6721(35) 0.6453(40) 0.036 Uiso 1 d . .
C4 C 0.5851(3) 0.7294(4) 0.5298(4) 0.0281(15) Uani 1 d . .
H4 H 0.5973(30) 0.7836(33) 0.5488(35) 0.028 Uiso 1 d . .
C5 C 0.5666(3) 0.7190(3) 0.4348(4) 0.0226(13) Uani 1 d . .
C6 C 0.6495(3) 0.9687(4) 0.3568(4) 0.0292(15) Uani 1 d . .
H6 H 0.6350(31) 1.0101(33) 0.3147(35) 0.029 Uiso 1 d . .
C7 C 0.7207(3) 0.9653(4) 0.4205(4) 0.030(2) Uani 1 d . .
H7 H 0.7488(32) 1.0033(34) 0.4251(37) 0.030 Uiso 1 d . .
C8 C 0.7401(3) 0.8989(4) 0.4774(4) 0.029(2) Uani 1 d . .
H8 H 0.7861(32) 0.8973(32) 0.5202(37) 0.029 Uiso 1 d . .
C9 C 0.6890(3) 0.8381(4) 0.4683(4) 0.0273(15) Uani 1 d . .
H9 H 0.7019(31) 0.7967(32) 0.5029(37) 0.027 Uiso 1 d . .
C10 C 0.6171(3) 0.8411(3) 0.3994(4) 0.0214(13) Uani 1 d . .
C11 C 0.6601(4) 0.5812(4) 0.2719(4) 0.032(2) Uani 1 d . .
H11 H 0.6407(32) 0.5365(33) 0.2830(38) 0.032 Uiso 1 d . .
C12 C 0.7335(4) 0.5868(4) 0.2796(5) 0.038(2) Uani 1 d . .
H12 H 0.7628(33) 0.5443(36) 0.2905(38) 0.038 Uiso 1 d . .
C13 C 0.7619(4) 0.6620(4) 0.2694(4) 0.035(2) Uani 1 d . .
H13 H 0.8098(34) 0.6710(34) 0.2777(38) 0.035 Uiso 1 d . .
C14 C 0.7140(3) 0.7268(4) 0.2478(4) 0.0299(15) Uani 1 d . .
H14 H 0.7333(31) 0.7725(33) 0.2398(38) 0.030 Uiso 1 d . .
C15 C 0.6371(3) 0.7164(3) 0.2332(3) 0.0221(14) Uani 1 d . .
C16 C 0.5588(3) 0.9744(4) 0.1117(4) 0.029(2) Uani 1 d . .
H16 H 0.5372(30) 1.0188(33) 0.1193(36) 0.029 Uiso 1 d . .
C17 C 0.5998(3) 0.9752(4) 0.0540(4) 0.034(2) Uani 1 d . .
H17 H 0.6038(30) 1.0229(36) 0.0258(36) 0.034 Uiso 1 d . .
C18 C 0.6375(4) 0.9067(4) 0.0457(4) 0.032(2) Uani 1 d . .
H18 H 0.6624(33) 0.9070(36) 0.0098(38) 0.032 Uiso 1 d . .
C19 C 0.6330(3) 0.8399(4) 0.0944(4) 0.030(2) Uani 1 d . .
H19 H 0.6483(31) 0.7940(34) 0.0765(37) 0.030 Uiso 1 d . .
C20 C 0.5923(3) 0.8417(3) 0.1561(4) 0.0230(13) Uani 1 d . .
C21 C 0.5979(4) 0.6742(4) -0.0930(4) 0.048(2) Uani 1 d D .
Cl2 Cl 0.62487(10) 0.63067(10) 0.01801(12) 0.0499(5) Uani 1 d D .
Cl3A Cl 0.6738(3) 0.6539(7) -0.1368(3) 0.071(3) Uani 0.60(2) d PD 1
Cl3B Cl 0.6769(6) 0.7169(21) -0.1128(16) 0.154(11) Uani 0.40(2) d PD 2
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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_3
_geom_angle_publ_flag
Co3 Co2 Co1 180.0 . y
Cl1 Co1 Co2 180.0 . y
Co2 Co3 F1 180.0 . y
Co3 F1 B1 173.2(8) . y
N1 Co1 N1 163.2(2) 2_655 y
N4 Co1 N4 163.8(3) 2_655 y
N4 Co1 N1 86.8(2) . y
N4 Co1 N1 90.8(2) 2_655 y
N4 Co1 Cl1 98.10(13) . y
N1 Co1 Cl1 98.42(12) . y
N4 Co1 Co2 81.90(12) . y
N1 Co1 Co2 81.58(12) . y
N5 Co2 N5 179.6(3) 2_655 y
N5 Co2 N2 90.4(2) . y
N5 Co2 N2 89.6(2) 2_655 y
N2 Co2 N2 177.0(3) 2_655 y
N5 Co2 Co3 89.78(13) . y
N2 Co2 Co3 88.52(13) . y
N5 Co2 Co1 90.22(13) . y
N2 Co2 Co1 91.48(13) . y
N3 Co3 N3 174.9(3) 2_655 y
N3 Co3 N6 87.2(2) . y
N3 Co3 N6 92.6(2) 2_655 y
N6 Co3 N6 175.3(3) 2_655 y
N3 Co3 F1 92.57(13) . y
N6 Co3 F1 92.37(14) . y
N3 Co3 Co2 87.43(13) . y
N6 Co3 Co2 87.63(14) . y
F2 B1 F4 111.2(16) . y
F2 B1 F3 112.8(16) . y
F4 B1 F3 110.6(15) . y
F2 B1 F1 109.1(13) . y
F4 B1 F1 106.0(14) . y
F3 B1 F1 106.9(15) . y
C1 N1 C5 117.1(5) . ?
C1 N1 Co1 119.9(4) . ?
C5 N1 Co1 122.8(4) . ?
C10 N2 C5 121.3(4) . ?
C10 N2 Co2 117.5(4) . ?
C5 N2 Co2 121.0(3) . ?
C6 N3 C10 119.9(5) . ?
C6 N3 Co3 120.8(4) . ?
C10 N3 Co3 119.0(4) . ?
C11 N4 C15 117.1(5) . ?
C11 N4 Co1 119.2(4) . ?
C15 N4 Co1 123.5(4) . ?
C20 N5 C15 121.9(4) . ?
C20 N5 Co2 117.9(3) . ?
C15 N5 Co2 120.1(3) . ?
C16 N6 C20 118.4(5) . ?
C16 N6 Co3 121.5(4) . ?
C20 N6 Co3 119.9(4) . ?
N1 C1 C2 124.6(6) . ?
N1 C1 H1 109.2(44) . ?
C2 C1 H1 125.9(44) . ?
C1 C2 C3 118.0(6) . ?
C1 C2 H2 121.6(47) . ?
C3 C2 H2 120.3(47) . ?
C4 C3 C2 119.7(6) . ?
C4 C3 H3 118.9(39) . ?
C2 C3 H3 121.3(39) . ?
C3 C4 C5 120.2(6) . ?
C3 C4 H4 126.6(33) . ?
C5 C4 H4 113.0(32) . ?
N1 C5 N2 115.7(5) . ?
N1 C5 C4 120.0(5) . ?
N2 C5 C4 124.3(5) . ?
N3 C6 C7 122.8(6) . ?
N3 C6 H6 115.5(36) . ?
C7 C6 H6 121.5(36) . ?
C6 C7 C8 118.4(6) . ?
C6 C7 H7 118.8(42) . ?
C8 C7 H7 122.7(42) . ?
C9 C8 C7 119.8(5) . ?
C9 C8 H8 121.6(36) . ?
C7 C8 H8 118.6(36) . ?
C8 C9 C10 120.9(6) . ?
C8 C9 H9 119.1(38) . ?
C10 C9 H9 119.9(38) . ?
N2 C10 N3 115.6(5) . ?
N2 C10 C9 126.1(5) . ?
N3 C10 C9 118.1(5) . ?
C12 C11 N4 124.5(6) . ?
C12 C11 H11 121.9(39) . ?
N4 C11 H11 113.6(39) . ?
C11 C12 C13 118.3(6) . ?
C11 C12 H12 121.3(41) . ?
C13 C12 H12 120.4(41) . ?
C14 C13 C12 119.1(6) . ?
C14 C13 H13 117.4(39) . ?
C12 C13 H13 123.4(39) . ?
C13 C14 C15 120.2(6) . ?
C13 C14 H14 116.6(38) . ?
C15 C14 H14 123.0(38) . ?
N4 C15 N5 115.4(5) . ?
N4 C15 C14 120.3(5) . ?
N5 C15 C14 124.2(5) . ?
N6 C16 C17 123.5(6) . ?
N6 C16 H16 117.9(37) . ?
C17 C16 H16 118.4(37) . ?
C16 C17 C18 118.7(6) . ?
C16 C17 H17 118.4(36) . ?
C18 C17 H17 122.8(36) . ?
C19 C18 C17 119.5(6) . ?
C19 C18 H18 121.7(42) . ?
C17 C18 H18 118.8(42) . ?
C18 C19 C20 120.6(6) . ?
C18 C19 H19 115.9(37) . ?
C20 C19 H19 122.3(37) . ?
N6 C20 N5 116.0(5) . ?
N6 C20 C19 119.2(5) . ?
N5 C20 C19 124.7(5) . ?
Cl3B C21 Cl2 110.4(6) . ?
Cl2 C21 Cl3A 106.5(4) . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 Co2 2.504(2) y
Co2 Co3 2.277(2) y
Co1 Cl1 2.371(2) y
Co1 N4 2.097(4) y
Co1 N1 2.155(4) y
Co2 N5 1.908(4) y
Co2 N2 1.912(4) y
Co3 N3 1.943(4) y
Co3 N6 1.948(4) y
Co3 F1 2.223(5) y
B1 F1 1.44(2) y
B1 F2 1.32(2) y
B1 F3 1.33(2) y
B1 F4 1.32(2) y
N1 C1 1.353(7) ?
N1 C5 1.366(6) ?
N2 C10 1.351(7) ?
N2 C5 1.370(7) ?
N3 C6 1.349(7) ?
N3 C10 1.367(7) ?
N4 C11 1.354(7) ?
N4 C15 1.363(7) ?
N5 C20 1.369(7) ?
N5 C15 1.371(6) ?
N6 C16 1.348(7) ?
N6 C20 1.356(7) ?
C1 C2 1.358(9) ?
C1 H1 0.79(5) ?
C2 C3 1.371(9) ?
C2 H2 0.79(6) ?
C3 C4 1.365(8) ?
C3 H3 0.89(6) ?
C4 C5 1.400(8) ?
C4 H4 0.95(5) ?
C6 C7 1.369(8) ?
C6 H6 0.92(5) ?
C7 C8 1.377(8) ?
C7 H7 0.81(6) ?
C8 C9 1.365(8) ?
C8 H8 0.89(5) ?
C9 C10 1.409(7) ?
C9 H9 0.85(5) ?
C11 C12 1.347(9) ?
C11 H11 0.86(5) ?
C12 C13 1.383(9) ?
C12 H12 0.87(6) ?
C13 C14 1.365(8) ?
C13 H13 0.88(6) ?
C14 C15 1.395(8) ?
C14 H14 0.87(5) ?
C16 C17 1.361(8) ?
C16 H16 0.87(5) ?
C17 C18 1.365(9) ?
C17 H17 0.92(6) ?
C18 C19 1.356(8) ?
C18 H18 0.84(6) ?
C19 C20 1.408(8) ?
C19 H19 0.89(6) ?
C21 Cl3B 1.761(13) ?
C21 Cl2 1.770(6) ?
C21 Cl3A 1.805(8) ?
