#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:51:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180017 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/11/7031165.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_7031165
loop_
_publ_author_name
'Park, Gyungse'
'Przyborowska, Ann M.'
'Ye, Neng'
'Tsoupas, Nicole M.'
'Bauer, Cary B.'
'Broker, Grant A.'
'Rogers, Robin D.'
'Brechbiel, Martin W.'
'Planalp, Roy P.'
_publ_section_title
;
 Steric effects caused by N-alkylation of the tripodal chelator
 N,N′,N″-tris(2-pyridylmethyl)-cis,cis-1,3,5-triaminocyclohexane
 (tachpyr): structural and electronic properties of the Mn(ii), Co(ii),
 Ni(ii), Cu(ii) and Zn(ii) complexes
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              318
_journal_paper_doi               10.1039/b209228j
_journal_year                    2003
_chemical_formula_structural     RP22
_chemical_formula_sum            'C27 H36 Cl2 N6 O8 Zn'
_chemical_formula_weight         708.89
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.2593(2)
_cell_length_b                   11.2593(2)
_cell_length_c                   13.5750(4)
_cell_measurement_reflns_used    4785
_cell_measurement_temperature    173(2)
_cell_volume                     1490.37(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       '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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9116
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.038(11)
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.985
_refine_ls_goodness_of_fit_obs   1.013
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.985
_refine_ls_restrained_S_obs      1.013
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_obs          0.0275
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0290P)²+ 0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0570
_refine_ls_wR_factor_obs         0.0542
_reflns_number_observed          1986
_reflns_number_total             2300
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b209228j.txt
_cod_data_source_block           rp22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+ 0.0000P] 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^)+(0.0290P)^2^+ 0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P31c
_cod_database_code               7031165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
Zn Zn 0.6667 0.3333 0.10697(3) 0.01782(12) Uani 1 d S
Cl1 Cl 1.0000 1.0000 0.02729(9) 0.0234(2) Uani 1 d S
Cl2 Cl 0.3333 0.6667 0.07874(6) 0.0227(2) Uani 1 d S
O1 O 1.0000 1.0000 0.1322(2) 0.0455(10) Uani 1 d S
O2 O 0.9820(2) 0.8717(2) -0.00770(15) 0.0407(5) Uani 1 d .
O3 O 0.3333 0.6667 -0.0253(3) 0.0611(11) Uani 1 d S
O4 O 0.2809(2) 0.7509(2) 0.1145(2) 0.0482(5) Uani 1 d .
N1 N 0.5949(2) 0.4487(2) 0.01450(13) 0.0207(4) Uani 1 d .
N2 N 0.7337(2) 0.5193(2) 0.19137(14) 0.0214(4) Uani 1 d .
C1 C 0.6108(3) 0.4293(2) -0.0938(2) 0.0249(5) Uani 1 d .
H1A H 0.5786 0.4846 -0.1310 0.030 Uiso 1 calc R
C2 C 0.7587(2) 0.4789(3) -0.1259(2) 0.0268(6) Uani 1 d .
H2A H 0.8178 0.5724 -0.0994 0.032 Uiso 1 calc R
H2B H 0.7630 0.4857 -0.1987 0.032 Uiso 1 calc R
C3 C 0.6727(2) 0.5960(2) 0.0421(2) 0.0237(5) Uani 1 d .
H3A H 0.6149 0.6379 0.0298 0.028 Uiso 1 calc R
H3B H 0.7553 0.6436 0.0000 0.028 Uiso 1 calc R
C4 C 0.7155(2) 0.6161(2) 0.1483(2) 0.0205(5) Uani 1 d .
C5 C 0.7447(2) 0.7367(2) 0.1976(2) 0.0269(5) Uani 1 d .
H5A H 0.7280 0.8027 0.1668 0.032 Uiso 1 calc R
C6 C 0.7978(2) 0.7585(3) 0.2913(2) 0.0312(6) Uani 1 d .
H6A H 0.8203 0.8410 0.3253 0.037 Uiso 1 calc R
C7 C 0.8182(2) 0.6603(2) 0.3357(2) 0.0290(5) Uani 1 d .
H7A H 0.8547 0.6737 0.4005 0.035 Uiso 1 calc R
C8 C 0.7845(2) 0.5418(2) 0.2842(2) 0.0249(5) Uani 1 d .
H8A H 0.7974 0.4734 0.3151 0.030 Uiso 1 calc R
C9 C 0.4496(2) 0.4058(2) 0.0375(2) 0.0251(5) Uani 1 d .
H9A H 0.4171 0.4509 -0.0080 0.030 Uiso 1 calc R
H9B H 0.4432 0.4321 0.1053 0.030 Uiso 1 calc R
H9C H 0.3927 0.3061 0.0305 0.030 Uiso 1 calc R
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N2 Zn N2 94.57(7) 3_665 2_655
N2 Zn N2 94.57(7) 3_665 .
N2 Zn N2 94.57(7) 2_655 .
N2 Zn N1 77.71(7) 3_665 3_665
N2 Zn N1 165.75(6) 2_655 3_665
N2 Zn N1 97.95(7) . 3_665
N2 Zn N1 97.95(7) 3_665 2_655
N2 Zn N1 77.71(7) 2_655 2_655
N2 Zn N1 165.75(6) . 2_655
N1 Zn N1 91.37(7) 3_665 2_655
N2 Zn N1 165.75(7) 3_665 .
N2 Zn N1 97.95(7) 2_655 .
N2 Zn N1 77.71(7) . .
N1 Zn N1 91.37(7) 3_665 .
N1 Zn N1 91.37(7) 2_655 .
O1 Cl1 O2 109.32(9) . 3_675
O1 Cl1 O2 109.32(9) . .
O2 Cl1 O2 109.62(9) 3_675 .
O1 Cl1 O2 109.32(9) . 2_765
O2 Cl1 O2 109.62(9) 3_675 2_765
O2 Cl1 O2 109.62(9) . 2_765
O3 Cl2 O4 109.85(11) . .
O3 Cl2 O4 109.85(11) . 2_665
O4 Cl2 O4 109.09(11) . 2_665
O3 Cl2 O4 109.85(11) . 3_565
O4 Cl2 O4 109.09(11) . 3_565
O4 Cl2 O4 109.09(11) 2_665 3_565
C3 N1 C9 104.4(2) . .
C3 N1 C1 111.2(2) . .
C9 N1 C1 110.3(2) . .
C3 N1 Zn 109.03(13) . .
C9 N1 Zn 110.63(14) . .
C1 N1 Zn 111.14(13) . .
C4 N2 C8 118.4(2) . .
C4 N2 Zn 115.74(15) . .
C8 N2 Zn 125.74(15) . .
N1 C1 C2 114.2(2) . .
N1 C1 C2 112.1(2) . 2_655
C2 C1 C2 108.6(2) . 2_655
C1 C2 C1 115.8(2) . 3_665
N1 C3 C4 112.1(2) . .
N2 C4 C5 121.6(2) . .
N2 C4 C3 117.7(2) . .
C5 C4 C3 120.5(2) . .
C6 C5 C4 119.2(2) . .
C7 C6 C5 119.6(2) . .
C6 C7 C8 118.6(2) . .
N2 C8 C7 122.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn N2 2.165(2) 3_665
Zn N2 2.165(2) 2_655
Zn N2 2.165(2) .
Zn N1 2.228(2) 3_665
Zn N1 2.228(2) 2_655
Zn N1 2.228(2) .
Cl1 O1 1.425(4) .
Cl1 O2 1.435(2) 3_675
Cl1 O2 1.435(2) .
Cl1 O2 1.435(2) 2_765
Cl2 O3 1.412(3) .
Cl2 O4 1.430(2) .
Cl2 O4 1.430(2) 2_665
Cl2 O4 1.430(2) 3_565
N1 C3 1.485(3) .
N1 C9 1.490(3) .
N1 C1 1.510(3) .
N2 C4 1.340(3) .
N2 C8 1.354(3) .
C1 C2 1.532(3) .
C1 C2 1.531(3) 2_655
C2 C1 1.531(3) 3_665
C3 C4 1.501(3) .
C4 C5 1.399(3) .
C5 C6 1.374(4) .
C6 C7 1.376(4) .
C7 C8 1.381(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C1 C2 C1 C2 52.7(3) . . 3_665 3_665
C2 C1 C2 C1 -52.7(3) . 3_665 3_665 2_655
C1 C2 C1 C2 52.7(3) 3_665 3_665 2_655 2_655
C2 C1 C2 C1 -52.7(3) 3_665 2_655 2_655 .
C1 C2 C1 C2 52.7(3) 2_655 2_655 . .
C2 C1 C2 C1 -52.7(3) 2_655 . . 3_665
N1 X1 X2 N2 -43.19(8) . . . .
N1 X1 X2 N2 -163.19(8) . . . 3_665
N1 X1 X2 N2 76.81(8) . . . 2_655
N1 X1 X2 N2 76.81(8) 3_665 . . .
N1 X1 X2 N2 -43.19(8) 3_665 . . 3_665
N1 X1 X2 N2 -163.19(8) 3_665 . . 2_655
N1 X1 X2 N2 -163.19(8) 2_655 . . .
N1 X1 X2 N2 76.81(8) 2_655 . . 3_665
N1 X1 X2 N2 -43.19(8) 2_655 . . 2_655
