#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:43:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179489 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/86/4338697.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_4338697
loop_
_publ_author_name
'Santillan, Guillermo A.'
'Carrano, Carl J.'
_publ_section_title
;
 Cobalt, zinc, and nickel complexes of a diatopic heteroscorpionate
 ligand: building blocks for coordination polymers.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              930
_journal_page_last               939
_journal_paper_doi               10.1021/ic701718b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C50 H46 Co2 N8 O16'
_chemical_formula_weight         1132.81
_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                90.45(5)
_cell_angle_beta                 107.79(5)
_cell_angle_gamma                112.76(4)
_cell_formula_units_Z            1
_cell_length_a                   10.331(10)
_cell_length_b                   11.426(11)
_cell_length_c                   14.246(14)
_cell_measurement_reflns_used    638
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      17.74
_cell_measurement_theta_min      2.31
_cell_volume                     1461(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.851
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.2634
_diffrn_reflns_av_sigmaI/netI    1.1428
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13038
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.409
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       0.34(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.4608
_refine_ls_R_factor_gt           0.1459
_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)+(0.1600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3301
_refine_ls_wR_factor_ref         0.4739
_reflns_number_gt                1257
_reflns_number_total             5915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701718b-complex_6.cif
_cod_data_source_block           gs38b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1461(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338697
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
Co1 Co 0.5043(3) 0.6614(3) 0.7449(2) 0.0577(14) Uani 1 1 d .
N1 N 0.7140(15) 0.7072(14) 0.7384(12) 0.065(5) Uani 1 1 d .
N2 N 0.7629(16) 0.6182(16) 0.7267(12) 0.061(5) Uani 1 1 d .
N3 N 0.4321(17) 0.4984(14) 0.6537(12) 0.060(5) Uani 1 1 d .
N4 N 0.5312(19) 0.4489(15) 0.6477(13) 0.058(5) Uani 1 1 d .
O1 O 0.2935(16) 0.5444(15) 0.8092(11) 0.071(5) Uani 1 1 d .
O2 O 0.5250(15) 0.6716(12) 0.8831(10) 0.074(4) Uani 1 1 d .
O3 O 0.4803(17) 0.9095(15) 0.7860(14) 0.092(5) Uani 1 1 d .
O4 O 0.3981(13) 0.7512(13) 0.6598(9) 0.061(4) Uani 1 1 d .
C1 C 0.995(2) 0.590(2) 0.7245(19) 0.109(9) Uani 1 1 d .
H1A H 0.9308 0.5001 0.7171 0.163 Uiso 1 1 calc R
H1B H 1.0820 0.6124 0.7836 0.163 Uiso 1 1 calc R
H1C H 1.0258 0.6076 0.6664 0.163 Uiso 1 1 calc R
C2 C 0.908(3) 0.672(2) 0.7345(19) 0.095(8) Uani 1 1 d .
C3 C 0.955(3) 0.802(2) 0.747(2) 0.119(11) Uani 1 1 d .
H3A H 1.0503 0.8640 0.7540 0.143 Uiso 1 1 calc R
C4 C 0.833(2) 0.8230(19) 0.7479(16) 0.072(7) Uani 1 1 d .
C5 C 0.823(3) 0.947(2) 0.761(2) 0.115(10) Uani 1 1 d .
H5A H 0.9175 1.0161 0.7661 0.173 Uiso 1 1 calc R
H5B H 0.7997 0.9546 0.8207 0.173 Uiso 1 1 calc R
H5C H 0.7453 0.9511 0.7036 0.173 Uiso 1 1 calc R
C6 C 0.525(2) 0.2603(19) 0.5542(16) 0.082(7) Uani 1 1 d .
H6A H 0.6268 0.2912 0.5987 0.123 Uiso 1 1 calc R
H6B H 0.5228 0.2586 0.4857 0.123 Uiso 1 1 calc R
H6C H 0.4684 0.1744 0.5652 0.123 Uiso 1 1 calc R
C7 C 0.458(3) 0.345(2) 0.5737(18) 0.068(6) Uani 1 1 d .
C8 C 0.310(2) 0.3330(18) 0.5243(14) 0.059(5) Uani 1 1 d .
H8A H 0.2354 0.2718 0.4706 0.071 Uiso 1 1 calc R
C9 C 0.302(2) 0.4335(19) 0.5749(17) 0.062(6) Uani 1 1 d .
C10 C 0.167(2) 0.460(2) 0.5568(15) 0.076(6) Uani 1 1 d .
H10A H 0.1904 0.5351 0.6021 0.113 Uiso 1 1 calc R
H10B H 0.0881 0.3870 0.5678 0.113 Uiso 1 1 calc R
H10C H 0.1340 0.4764 0.4886 0.113 Uiso 1 1 calc R
C11 C 0.670(2) 0.4828(17) 0.7262(14) 0.049(5) Uani 1 1 d .
H11A H 0.7200 0.4301 0.7111 0.059 Uiso 1 1 calc R
C12 C 0.650(2) 0.4586(18) 0.8249(15) 0.046(5) Uani 1 1 d .
C13 C 0.770(2) 0.5211(18) 0.9151(18) 0.056(6) Uani 1 1 d .
H13A H 0.8611 0.5781 0.9105 0.068 Uiso 1 1 calc R
C14 C 0.761(2) 0.5038(19) 1.0060(17) 0.069(6) Uani 1 1 d .
H14A H 0.8427 0.5462 1.0640 0.083 Uiso 1 1 calc R
C15 C 0.618(2) 0.4166(19) 1.0104(15) 0.053(5) Uani 1 1 d .
C16 C 0.504(2) 0.3497(17) 0.9221(18) 0.058(6) Uani 1 1 d .
H16A H 0.4132 0.2895 0.9251 0.070 Uiso 1 1 calc R
C17 C 0.5206(19) 0.3684(17) 0.8326(14) 0.051(5) Uani 1 1 d .
H17A H 0.4426 0.3191 0.7747 0.061 Uiso 1 1 calc R
C18 C 0.391(2) 0.5952(19) 0.8832(18) 0.055(6) Uani 1 1 d .
C19 C 0.399(2) 0.851(3) 0.697(2) 0.072(7) Uani 1 1 d .
C20 C 0.291(2) 0.9050(19) 0.6378(19) 0.064(6) Uani 1 1 d .
C21 C 0.199(2) 0.8456(19) 0.5436(16) 0.063(6) Uani 1 1 d .
H21A H 0.2135 0.7803 0.5135 0.076 Uiso 1 1 calc R
C22 C 0.080(2) 0.8812(19) 0.4897(17) 0.079(7) Uani 1 1 d .
H22A H 0.0143 0.8362 0.4265 0.094 Uiso 1 1 calc R
C23 C 0.062(2) 0.9829(18) 0.5313(17) 0.055(5) Uani 1 1 d .
C25 C 0.270(2) 1.0089(18) 0.6761(15) 0.060(5) Uani 1 1 d .
H25A H 0.3343 1.0537 0.7395 0.072 Uiso 1 1 calc R
C24 C 0.164(2) 1.0463(18) 0.6273(16) 0.049(5) Uani 1 1 d .
H24A H 0.1561 1.1160 0.6570 0.058 Uiso 1 1 calc R
O5 O 0.8278(16) 0.8222(15) 1.0276(11) 0.108(5) Uani 1 1 d .
O6 O 0.1178(15) 0.2763(14) 0.7744(11) 0.090(5) Uani 1 1 d .
O8 O -0.1699(17) 0.2878(16) 0.7474(16) 0.146(8) Uani 1 1 d .
O7 O 0.673(2) 1.1485(18) 0.8701(19) 0.170(9) 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 0.0033 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'
O O 0.0106 0.0060 '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
O2 Co1 O4 119.0(5) .
O2 Co1 N3 124.8(6) .
O4 Co1 N3 100.8(6) .
O2 Co1 N1 106.4(6) .
O4 Co1 N1 113.3(6) .
N3 Co1 N1 88.9(6) .
N2 N1 C4 104.9(13) .
N2 N1 Co1 122.2(11) .
C4 N1 Co1 132.9(12) .
N1 N2 C2 111.0(16) .
N1 N2 C11 119.6(13) .
C2 N2 C11 128.3(15) .
N4 N3 C9 106.8(15) .
N4 N3 Co1 119.6(13) .
C9 N3 Co1 131.9(12) .
N3 N4 C7 108.4(16) .
N3 N4 C11 121.0(16) .
C7 N4 C11 128.3(16) .
C18 O2 Co1 103.4(13) .
C19 O4 Co1 119.2(14) .
N2 C2 C3 108.5(16) .
N2 C2 C1 122(2) .
C3 C2 C1 129(2) .
C2 C3 C4 105.4(19) .
C3 C4 N1 110.2(17) .
C3 C4 C5 128(2) .
N1 C4 C5 121.8(16) .
N4 C7 C8 109.7(17) .
N4 C7 C6 123(2) .
C8 C7 C6 127(2) .
C9 C8 C7 103.3(19) .
N3 C9 C8 111.3(16) .
N3 C9 C10 122.7(17) .
C8 C9 C10 126(2) .
N4 C11 N2 107.6(14) .
N4 C11 C12 112.0(15) .
N2 C11 C12 111.9(15) .
C17 C12 C13 117.2(16) .
C17 C12 C11 121.9(18) .
C13 C12 C11 120.6(16) .
C14 C13 C12 124.2(17) .
C13 C14 C15 116.5(19) .
C16 C15 C14 118.8(17) .
C16 C15 C18 126.1(19) 2_667
C14 C15 C18 115.1(18) 2_667
C17 C16 C15 122.1(17) .
C16 C17 C12 120.8(18) .
O1 C18 O2 121.4(19) .
O1 C18 C15 125.7(19) 2_667
O2 C18 C15 113(2) 2_667
O4 C19 O3 124(2) .
O4 C19 C20 119(2) .
O3 C19 C20 116(2) .
C21 C20 C25 116.4(19) .
C21 C20 C19 119(2) .
C25 C20 C19 124(2) .
C20 C21 C22 121.3(19) .
C23 C22 C21 120(2) .
C22 C23 C24 117.2(17) .
C22 C23 C23 117(3) 2_576
C24 C23 C23 126(2) 2_576
C24 C25 C20 124(2) .
C25 C24 C23 121.3(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 1.912(13) .
Co1 O4 1.952(12) .
Co1 N3 2.001(16) .
Co1 N1 2.054(13) .
N1 N2 1.329(17) .
N1 C4 1.39(2) .
N2 C2 1.35(2) .
N2 C11 1.47(2) .
N3 N4 1.371(17) .
N3 C9 1.38(2) .
N4 C7 1.37(3) .
N4 C11 1.43(2) .
O1 C18 1.16(2) .
O2 C18 1.32(2) .
O3 C19 1.29(3) .
O4 C19 1.25(3) .
C1 C2 1.56(3) .
C2 C3 1.36(3) .
C3 C4 1.37(2) .
C4 C5 1.47(3) .
C6 C7 1.46(2) .
C7 C8 1.43(3) .
C8 C9 1.39(2) .
C9 C10 1.49(2) .
C11 C12 1.50(2) .
C12 C17 1.37(2) .
C12 C13 1.42(2) .
C13 C14 1.34(2) .
C14 C15 1.45(2) .
C15 C16 1.39(3) .
C15 C18 1.55(3) 2_667
C16 C17 1.34(2) .
C18 C15 1.55(3) 2_667
C19 C20 1.51(3) .
C20 C21 1.37(3) .
C20 C25 1.42(2) .
C21 C22 1.44(2) .
C22 C23 1.40(2) .
C23 C24 1.42(2) .
C23 C23 1.51(4) 2_576
C25 C24 1.33(2) .
