#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:46:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179204 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/38/4313868.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_4313868
loop_
_publ_author_name
'John F. Berry'
'F. Albert Cotton'
'Tongbu Lu'
'Carlos A. Murillo'
_publ_section_title
;
 Increasing Solubility and Stability of Linear Tricobalt(II) Chains with
 depa (Diethyldipyridylamide) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4425
_journal_page_last               4430
_journal_paper_doi               10.1021/ic034149y
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'Co3C58H64N14, 4(CH2Cl2), 2(H2O)'
_chemical_formula_sum            'C62 H76 Cl8 Co3 N14 O2'
_chemical_formula_weight         1509.76
_chemical_melting_point          ?
_chemical_name_common            'Co3(depa)4(CN)2, 4CH2Cl2, 2H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           120
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_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            4
_cell_length_a                   17.9117(7)
_cell_length_b                   17.9117(7)
_cell_length_c                   21.9213(17)
_cell_measurement_reflns_used    5224
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.968
_cell_measurement_theta_min      2.457
_cell_volume                     7033.0(7)
_computing_cell_refinement       'SAINT V.6.22'
_computing_data_collection       'SMART V.5.618'
_computing_data_reduction        'SAINT V.6.22'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Brucker SMART 1000'
_diffrn_measurement_method       'omega sacns'
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17825
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.8750
_exptl_absorpt_correction_T_min  0.5607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0985P)²+14.9179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                2777
_reflns_number_total             3087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034149ysi20030212_102325_1.cif
_cod_data_source_block           Co3(depa)4(CN)2.4Dichloromethane.2Water
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_database_code               4313868
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'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'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
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
Co2 Co 0.5000 1.0000 0.5000 0.0317(3) Uani 1 4 d S . .
Co1 Co 0.59221(3) 0.90779(3) 0.5000 0.0360(2) Uani 1 2 d S . .
N4 N 0.5000 1.0000 0.4134(2) 0.0350(9) Uani 1 2 d S . .
N1 N 0.5140(2) 0.8435(2) 0.46337(18) 0.0394(8) Uani 1 1 d . . .
N2 N 0.42443(18) 0.92443(18) 0.5000 0.0363(9) Uani 1 2 d S . .
N3 N 0.6176(2) 0.9465(2) 0.41773(18) 0.0400(8) Uani 1 1 d . . .
N5 N 0.7178(2) 0.7822(2) 0.5000 0.076(2) Uani 1 2 d S . .
C15 C 0.6730(2) 0.8270(2) 0.5000 0.0484(14) Uani 1 2 d S . .
C11 C 0.5865(3) 1.0159(3) 0.3272(2) 0.0433(11) Uani 1 1 d . . .
H11A H 0.5507 1.0424 0.3044 0.052 Uiso 1 1 calc R . .
C3 C 0.4061(4) 0.7504(3) 0.4100(3) 0.0591(15) Uani 1 1 d . D .
C8 C 0.6866(3) 0.9388(3) 0.3948(3) 0.0480(11) Uani 1 1 d . . .
H8A H 0.7223 0.9131 0.4182 0.058 Uiso 1 1 calc R . .
C12 C 0.5665(3) 0.9867(3) 0.3841(2) 0.0367(9) Uani 1 1 d . . .
C5 C 0.4391(3) 0.8600(3) 0.4699(2) 0.0435(10) Uani 1 1 d . . .
C10 C 0.6561(3) 1.0069(3) 0.3039(2) 0.0516(13) Uani 1 1 d . C .
C2 C 0.4808(4) 0.7356(3) 0.4034(3) 0.0604(16) Uani 1 1 d . . .
H2A H 0.4965 0.6933 0.3815 0.073 Uiso 1 1 calc R . .
C9 C 0.7082(3) 0.9667(3) 0.3387(2) 0.0531(13) Uani 1 1 d . . .
H9A H 0.7569 0.9589 0.3240 0.064 Uiso 1 1 calc R . .
C4 C 0.3857(3) 0.8131(3) 0.4432(3) 0.0523(13) Uani 1 1 d . . .
H4A H 0.3348 0.8245 0.4478 0.063 Uiso 1 1 calc R . .
C13 C 0.6772(4) 1.0387(4) 0.2422(3) 0.0711(18) Uani 1 1 d D . .
H13A H 0.7182 1.0088 0.2253 0.085 Uiso 1 1 calc R A 1
H13B H 0.6344 1.0335 0.2147 0.085 Uiso 1 1 calc R A 1
C6 C 0.3485(4) 0.6999(4) 0.3809(4) 0.084(2) Uani 1 1 d D . .
H6A H 0.3738 0.6671 0.3518 0.101 Uiso 1 1 calc R B 1
H6B H 0.3266 0.6683 0.4127 0.101 Uiso 1 1 calc R B 1
C1 C 0.5332(3) 0.7834(3) 0.4291(3) 0.0535(13) Uani 1 1 d . . .
H1A H 0.5841 0.7737 0.4225 0.064 Uiso 1 1 calc R . .
C14 C 0.7009(15) 1.1194(6) 0.2429(11) 0.087(3) Uiso 0.346(15) 1 d PD C 1
H14A H 0.7134 1.1351 0.2018 0.130 Uiso 0.346(15) 1 calc PR C 1
H14B H 0.7442 1.1252 0.2691 0.130 Uiso 0.346(15) 1 calc PR C 1
H14C H 0.6603 1.1499 0.2583 0.130 Uiso 0.346(15) 1 calc PR C 1
C14' C 0.7455(6) 1.0876(7) 0.2407(6) 0.087(3) Uiso 0.654(15) 1 d PD C 2
H14D H 0.7540 1.1049 0.1993 0.130 Uiso 0.654(15) 1 calc PR C 2
H14E H 0.7884 1.0593 0.2545 0.130 Uiso 0.654(15) 1 calc PR C 2
H14F H 0.7380 1.1303 0.2673 0.130 Uiso 0.654(15) 1 calc PR C 2
C7 C 0.2864(15) 0.7401(17) 0.3483(15) 0.137(6) Uiso 0.375(16) 1 d PD D 1
H7A H 0.2524 0.7039 0.3307 0.206 Uiso 0.375(16) 1 calc PR D 1
H7B H 0.3073 0.7709 0.3161 0.206 Uiso 0.375(16) 1 calc PR D 1
H7C H 0.2597 0.7715 0.3770 0.206 Uiso 0.375(16) 1 calc PR D 1
C7' C 0.3418(13) 0.7186(13) 0.3143(5) 0.137(6) Uiso 0.625(16) 1 d PD D 2
H7'A H 0.3045 0.6867 0.2956 0.206 Uiso 0.625(16) 1 calc PR D 2
H7'B H 0.3895 0.7109 0.2944 0.206 Uiso 0.625(16) 1 calc PR D 2
H7'C H 0.3269 0.7704 0.3098 0.206 Uiso 0.625(16) 1 calc PR D 2
Cl2A Cl 0.6555(5) 0.6261(4) 0.3746(3) 0.167(2) Uiso 0.697(7) 1 d PD E 1
C1A C 0.6660(10) 0.5965(8) 0.4423(6) 0.121(5) Uiso 0.697(7) 1 d PD E 1
H1AA H 0.6514 0.6355 0.4713 0.146 Uiso 0.697(7) 1 calc PR E 1
H1AB H 0.7187 0.5844 0.4494 0.146 Uiso 0.697(7) 1 calc PR E 1
Cl1A Cl 0.6160(6) 0.5239(5) 0.4527(4) 0.220(3) Uiso 0.697(7) 1 d PD E 1
Cl2B Cl 0.6826(11) 0.6479(10) 0.3835(8) 0.167(2) Uiso 0.303(7) 1 d PD E 2
C1B C 0.6620(19) 0.625(3) 0.4510(11) 0.121(5) Uiso 0.303(7) 1 d PD E 2
H1BA H 0.6848 0.6658 0.4741 0.146 Uiso 0.303(7) 1 calc PR E 2
H1BB H 0.6957 0.5825 0.4574 0.146 Uiso 0.303(7) 1 calc PR E 2
Cl1B Cl 0.5947(11) 0.6031(12) 0.4943(13) 0.220(3) Uiso 0.303(7) 1 d PD E 2
OW1 O 0.4465(10) 0.5535(10) 0.2500 0.318(16) Uani 1 2 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'
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'
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
N4 Co2 N4 180.000(1) . 15_455 ?
N4 Co2 N2 90.000(1) . 2_675 ?
N4 Co2 N2 90.000(1) 15_455 2_675 ?
N4 Co2 N2 90.000(1) . . ?
N4 Co2 N2 90.000(1) 15_455 . ?
N2 Co2 N2 180.000(1) 2_675 . ?
N4 Co2 Co1 90.0 . 2_675 ?
N4 Co2 Co1 90.0 15_455 2_675 ?
N2 Co2 Co1 90.000(1) 2_675 2_675 ?
N2 Co2 Co1 90.0 . 2_675 ?
N4 Co2 Co1 90.0 . . ?
N4 Co2 Co1 90.0 15_455 . ?
N2 Co2 Co1 90.0 2_675 . ?
N2 Co2 Co1 90.000(1) . . ?
Co1 Co2 Co1 180.0 2_675 . ?
N1 Co1 N1 169.8(2) 16_665 . ?
N1 Co1 N3 89.28(16) 16_665 . ?
N1 Co1 N3 89.85(16) . . ?
N1 Co1 N3 89.85(16) 16_665 16_665 ?
N1 Co1 N3 89.28(16) . 16_665 ?
N3 Co1 N3 170.3(2) . 16_665 ?
N1 Co1 C15 95.10(11) 16_665 . ?
N1 Co1 C15 95.10(11) . . ?
N3 Co1 C15 94.87(11) . . ?
N3 Co1 C15 94.87(11) 16_665 . ?
N1 Co1 Co2 84.90(11) 16_665 . ?
N1 Co1 Co2 84.90(11) . . ?
N3 Co1 Co2 85.13(11) . . ?
N3 Co1 Co2 85.13(11) 16_665 . ?
C15 Co1 Co2 180.00(4) . . ?
C12 N4 C12 124.3(5) 2_675 . ?
C12 N4 Co2 117.8(2) 2_675 . ?
C12 N4 Co2 117.8(2) . . ?
C1 N1 C5 118.2(4) . . ?
C1 N1 Co1 120.4(4) . . ?
C5 N1 Co1 121.3(3) . . ?
C5 N2 C5 124.5(5) . 15_455 ?
C5 N2 Co2 117.8(3) . . ?
C5 N2 Co2 117.8(3) 15_455 . ?
C8 N3 C12 117.8(4) . . ?
C8 N3 Co1 121.0(4) . . ?
C12 N3 Co1 121.1(3) . . ?
N5 C15 Co1 180.0(5) . . ?
C10 C11 C12 121.7(5) . . ?
C2 C3 C4 118.0(5) . . ?
C2 C3 C6 120.3(5) . . ?
C4 C3 C6 121.7(6) . . ?
N3 C8 C9 123.5(5) . . ?
N4 C12 N3 114.6(4) . . ?
N4 C12 C11 125.0(4) . . ?
N3 C12 C11 120.2(4) . . ?
N2 C5 N1 114.9(4) . . ?
N2 C5 C4 125.6(5) . . ?
N1 C5 C4 119.4(4) . . ?
C11 C10 C9 117.9(5) . . ?
C11 C10 C13 121.4(5) . . ?
C9 C10 C13 120.7(5) . . ?
C3 C2 C1 119.8(5) . . ?
C8 C9 C10 118.9(5) . . ?
C3 C4 C5 121.7(5) . . ?
C14' C13 C14 38.1(10) . . ?
C14' C13 C10 116.2(7) . . ?
C14 C13 C10 114.9(11) . . ?
C7' C6 C7 51.1(15) . . ?
C7' C6 C3 109.4(10) . . ?
C7 C6 C3 114.7(15) . . ?
N1 C1 C2 122.8(5) . . ?
Cl2A C1A Cl1A 109.8(9) . . ?
Cl2B C1B Cl1B 143(3) . . ?
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
Co2 N4 1.899(5) . ?
Co2 N4 1.899(5) 15_455 ?
Co2 N2 1.914(5) 2_675 ?
Co2 N2 1.914(5) . ?
Co2 Co1 2.3357(7) 2_675 ?
Co2 Co1 2.3357(7) . ?
Co1 N1 1.984(4) 16_665 ?
Co1 N1 1.984(4) . ?
Co1 N3 1.985(4) . ?
Co1 N3 1.985(4) 16_665 ?
Co1 C15 2.047(6) . ?
N4 C12 1.374(5) 2_675 ?
N4 C12 1.374(5) . ?
N1 C1 1.356(6) . ?
N1 C5 1.382(6) . ?
N2 C5 1.355(5) . ?
N2 C5 1.355(5) 15_455 ?
N3 C8 1.341(6) . ?
N3 C12 1.379(6) . ?
N5 C15 1.136(9) . ?
C11 C10 1.356(7) . ?
C11 C12 1.399(7) . ?
C3 C2 1.371(9) . ?
C3 C4 1.387(8) . ?
C3 C6 1.513(9) . ?
C8 C9 1.384(7) . ?
C5 C4 1.401(7) . ?
C10 C9 1.403(8) . ?
C10 C13 1.516(7) . ?
C2 C1 1.390(9) . ?
C13 C14' 1.504(5) . ?
C13 C14 1.506(5) . ?
C6 C7' 1.504(5) . ?
C6 C7 1.506(5) . ?
Cl2A C1A 1.586(9) . ?
C1A Cl1A 1.597(9) . ?
Cl2B C1B 1.580(10) . ?
C1B Cl1B 1.583(10) . ?
