#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:36:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179927 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/22/7022272.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_7022272
loop_
_publ_author_name
'Cubanski, John R.'
'Cameron, Scott A.'
'Crowley, James D.'
'Blackman, Allan G.'
_publ_section_title
;
 Low symmetry pyrazole-based tripodal tetraamine ligands: metal complexes
 and ligand decomposition reactions.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2174
_journal_page_last               2185
_journal_paper_doi               10.1039/c2dt32200e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C28 H50 Cl4 Co2 N14 O6'
_chemical_formula_weight         938.48
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.746(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9001(19)
_cell_length_b                   27.533(6)
_cell_length_c                   9.309(2)
_cell_measurement_reflns_used    6662
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.54
_cell_volume                     2054.7(8)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29703
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.9204
_exptl_absorpt_correction_T_min  0.7663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.238
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4201
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0803
_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)+(0.1017P)²+13.2527P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2174
_reflns_number_gt                3430
_reflns_number_total             4201
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt32200e.txt
_cod_data_source_block           CobepzCl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2054.6(8)
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7022272
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.58319(8) 0.93872(3) 0.07546(8) 0.0200(2) Uani 1 1 d .
Cl1 Cl 0.66543(15) 1.02350(4) 0.15460(15) 0.0238(3) Uani 1 1 d .
N3 N 0.4261(6) 0.93243(18) 0.1846(6) 0.0297(11) Uani 1 1 d .
N2 N 0.3211(6) 0.8926(2) 0.1330(8) 0.0452(15) Uani 1 1 d .
N1 N 0.5000(7) 0.86066(18) 0.0124(6) 0.0341(11) Uani 1 1 d .
N6 N 0.8503(6) 0.86907(17) 0.3071(6) 0.0303(11) Uani 1 1 d .
N7 N 0.7946(5) 0.91535(16) 0.2824(5) 0.0231(9) Uani 1 1 d .
N4 N 0.6531(6) 0.90352(17) -0.1988(5) 0.0267(10) Uani 1 1 d .
N5 N 0.7059(5) 0.93230(16) -0.0666(5) 0.0229(9) Uani 1 1 d .
C4 C 0.3926(10) 0.9540(3) 0.2945(8) 0.051(2) Uani 1 1 d .
H4 H 0.4426 0.9827 0.3519 0.061 Uiso 1 1 calc R
C3 C 0.2649(10) 0.9251(4) 0.3096(10) 0.060(3) Uani 1 1 d U
H3 H 0.2170 0.9311 0.3815 0.072 Uiso 1 1 calc R
C2 C 0.2253(10) 0.8883(3) 0.2045(11) 0.059(2) Uani 1 1 d .
H2 H 0.1433 0.8640 0.1863 0.071 Uiso 1 1 calc R
C1 C 0.3210(8) 0.8632(2) -0.0045(8) 0.0419(16) Uani 1 1 d .
H1A H 0.2474 0.8787 -0.1071 0.050 Uiso 1 1 calc R
H1B H 0.2787 0.8300 -0.0029 0.050 Uiso 1 1 calc R
C14 C 0.8921(7) 0.9395(2) 0.4144(6) 0.0264(12) Uani 1 1 d .
H14 H 0.8816 0.9732 0.4306 0.032 Uiso 1 1 calc R
C13 C 1.0101(7) 0.9095(3) 0.5243(7) 0.0358(14) Uani 1 1 d .
H13 H 1.0931 0.9180 0.6270 0.043 Uiso 1 1 calc R
C12 C 0.9822(8) 0.8651(2) 0.4545(8) 0.0375(15) Uani 1 1 d .
H12 H 1.0434 0.8363 0.4999 0.045 Uiso 1 1 calc R
C11 C 0.7740(8) 0.8308(2) 0.1954(9) 0.0451(17) Uani 1 1 d .
H11A H 0.8282 0.7996 0.2432 0.054 Uiso 1 1 calc R
H11B H 0.7923 0.8365 0.0992 0.054 Uiso 1 1 calc R
C10 C 0.5896(9) 0.8269(2) 0.1469(8) 0.0423(16) Uani 1 1 d .
H10A H 0.5517 0.7931 0.1139 0.051 Uiso 1 1 calc R
H10B H 0.5655 0.8353 0.2382 0.051 Uiso 1 1 calc R
C9 C 0.8521(7) 0.9509(2) -0.0481(7) 0.0287(12) Uani 1 1 d .
H9 H 0.9186 0.9723 0.0352 0.034 Uiso 1 1 calc R
C8 C 0.8936(8) 0.9342(2) -0.1685(8) 0.0357(14) Uani 1 1 d .
H8 H 0.9900 0.9419 -0.1833 0.043 Uiso 1 1 calc R
C7 C 0.7626(8) 0.9040(2) -0.2610(8) 0.0384(15) Uani 1 1 d .
H7 H 0.7526 0.8867 -0.3530 0.046 Uiso 1 1 calc R
C6 C 0.4951(7) 0.8773(2) -0.2556(7) 0.0295(12) Uani 1 1 d .
H6A H 0.4744 0.8606 -0.3566 0.035 Uiso 1 1 calc R
H6B H 0.4037 0.9010 -0.2784 0.035 Uiso 1 1 calc R
C5 C 0.4922(8) 0.8405(2) -0.1373(7) 0.0294(12) Uani 1 1 d .
H5A H 0.3888 0.8211 -0.1891 0.035 Uiso 1 1 calc R
H5B H 0.5877 0.8181 -0.1108 0.035 Uiso 1 1 calc R
Cl2 Cl 0.8841(4) 0.78665(13) 0.8988(3) 0.0993(11) Uani 1 1 d .
O1 O 0.7119(7) 0.79095(17) 0.5376(5) 0.0447(12) Uani 1 1 d .
H1X H 0.7707 0.7880 0.6385 0.054 Uiso 1 1 d .
H1Y H 0.7719 0.7804 0.4923 0.054 Uiso 1 1 d .
O2 O 0.2022(7) 0.7468(2) 0.1057(6) 0.0526(14) Uani 1 1 d .
H2X H 0.1398 0.7684 0.1161 0.063 Uiso 1 1 d .
H2Y H 0.2778 0.7385 0.1956 0.063 Uiso 1 1 d .
O3 O 0.3667(8) 0.78832(18) 0.4203(7) 0.0604(15) Uani 1 1 d .
H3X H 0.4714 0.7862 0.4769 0.072 Uiso 1 1 d .
H3Y H 0.3185 0.7777 0.4768 0.072 Uiso 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'
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_3
N5 Co1 N3 166.67(19) .
N5 Co1 N7 92.77(17) .
N3 Co1 N7 92.92(18) .
N5 Co1 N1 87.53(18) .
N3 Co1 N1 80.4(2) .
N7 Co1 N1 90.50(18) .
N5 Co1 Cl1 95.85(13) .
N3 Co1 Cl1 96.28(15) .
N7 Co1 Cl1 89.12(13) .
N1 Co1 Cl1 176.62(14) .
N5 Co1 Cl1 90.26(13) 3_675
N3 Co1 Cl1 85.46(14) 3_675
N7 Co1 Cl1 173.01(13) 3_675
N1 Co1 Cl1 95.92(14) 3_675
Cl1 Co1 Cl1 84.31(5) 3_675
Co1 Cl1 Co1 95.69(5) 3_675
C4 N3 N2 106.2(6) .
C4 N3 Co1 140.5(5) .
N2 N3 Co1 113.3(4) .
C2 N2 N3 112.9(7) .
C2 N2 C1 128.8(7) .
N3 N2 C1 118.0(5) .
C5 N1 C10 110.5(5) .
C5 N1 C1 107.5(5) .
C10 N1 C1 105.6(5) .
C5 N1 Co1 118.6(4) .
C10 N1 Co1 112.4(4) .
C1 N1 Co1 101.0(4) .
N7 N6 C12 109.7(5) .
N7 N6 C11 123.3(5) .
C12 N6 C11 126.9(5) .
C14 N7 N6 105.7(5) .
C14 N7 Co1 130.5(4) .
N6 N7 Co1 123.7(3) .
C7 N4 N5 110.8(5) .
C7 N4 C6 128.3(5) .
N5 N4 C6 120.9(4) .
C9 N5 N4 105.8(4) .
C9 N5 Co1 130.0(4) .
N4 N5 Co1 124.0(3) .
N3 C4 C3 106.2(8) .
C2 C3 C4 108.2(7) .
N2 C2 C3 106.4(8) .
N2 C1 N1 108.6(5) .
N7 C14 C13 111.4(5) .
C12 C13 C14 105.3(5) .
C13 C12 N6 107.9(5) .
N6 C11 C10 112.5(6) .
N1 C10 C11 108.9(6) .
N5 C9 C8 110.6(5) .
C7 C8 C9 104.5(5) .
N4 C7 C8 108.3(5) .
N4 C6 C5 112.8(5) .
N1 C5 C6 115.4(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N5 2.056(4) .
Co1 N3 2.062(5) .
Co1 N7 2.125(5) .
Co1 N1 2.266(5) .
Co1 Cl1 2.4615(15) .
Co1 Cl1 2.5392(15) 3_675
Cl1 Co1 2.5392(14) 3_675
N3 C4 1.324(9) .
N3 N2 1.384(8) .
N2 C2 1.295(10) .
N2 C1 1.514(10) .
N1 C5 1.473(7) .
N1 C10 1.484(8) .
N1 C1 1.533(9) .
N6 N7 1.350(6) .
N6 C12 1.369(8) .
N6 C11 1.429(8) .
N7 C14 1.333(7) .
N4 C7 1.333(8) .
N4 N5 1.365(6) .
N4 C6 1.460(7) .
N5 C9 1.338(7) .
C4 C3 1.443(12) .
C3 C2 1.345(13) .
C14 C13 1.379(8) .
C13 C12 1.355(10) .
C11 C10 1.505(10) .
C9 C8 1.401(8) .
C8 C7 1.385(9) .
C6 C5 1.506(8) .
