#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/25/8102558.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_8102558
loop_
_publ_author_name
'Wei-Jie Gong'
'Dao-Cheng Xia'
'Jian-Fang Ma'
_publ_section_title
;
 Crystal structure of
 [m-12,25-dimethyl-3,8,16,21-tetraaza-tricyclo[21.3.110,14]tetracosa-1(27),10,12,14(28),23,25-hexaene-27,28-diolato-
 k4N3,N8,O27,O28: k4N16,N21,O27,O28]zinc(II) dichloride,
 Zn2(C26H38N4O2)Cl2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              687
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C26 H38 Cl2 N4 O2 Zn2'
_chemical_formula_sum            'C26 H38 Cl2 N4 O2 Zn2'
_chemical_formula_weight         640.24
_chemical_melting_point          ?
_chemical_name_common
;
[μ-12,25-Dimethyl-3,8,16,21-tetraaza-
tricyclo[21.3.1^10,14^]tetracosa-1(27),10,12,14(28),23,25-
hexaene-27,28-diolato-κ⁴N³,N⁸,O²⁷,O²⁸:
κ⁴N¹⁶,N²¹,O²⁷,O²⁸]- bischloride zinc(II)
;
_chemical_name_systematic
;
[μ-12,25-Dimethyl-3,8,16,21-tetraaza-
tricyclo[21.3.1^10,14^]tetracosa-1(27),10,12,14(28),23,25-
hexaene-27,28-diolato-κ⁴N³,N⁸,O²⁷,O²⁸:
κ⁴N¹⁶,N²¹,O²⁷,O²⁸]- bischloride zinc(II)
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.366(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9863(4)
_cell_length_b                   11.5880(3)
_cell_length_c                   21.2059(7)
_cell_measurement_reflns_used    2182
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.230
_cell_measurement_theta_min      3.03
_cell_volume                     2840.15(16)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis [5]'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 [6]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8177
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                2182
_reflns_number_total             3321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2772.cff
_cod_data_source_block           c2c
_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 2.4.1 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_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               8102558
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_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
Zn1 Zn 0.86116(2) 0.17559(2) 0.506200(14) 0.03261(10) Uani 1 1 d . . .
C1 C 0.6823(3) -0.0045(4) 0.78662(16) 0.0882(12) Uani 1 1 d . . .
H1A H 0.7465 -0.0551 0.8039 0.132 Uiso 1 1 calc R . .
H1B H 0.6123 -0.0488 0.7739 0.132 Uiso 1 1 calc R . .
H1C H 0.6765 0.0506 0.8195 0.132 Uiso 1 1 calc R . .
C2 C 0.7007(2) 0.0585(3) 0.72766(13) 0.0501(7) Uani 1 1 d . . .
C3 C 0.6230(2) 0.1377(2) 0.69247(12) 0.0460(7) Uani 1 1 d . . .
H3 H 0.5582 0.1553 0.7069 0.055 Uiso 1 1 calc R . .
C4 C 0.63567(19) 0.1926(2) 0.63685(12) 0.0366(6) Uani 1 1 d . . .
C5 C 0.73281(19) 0.1664(2) 0.61301(11) 0.0334(5) Uani 1 1 d . . .
C6 C 0.81522(19) 0.0899(2) 0.64980(11) 0.0347(6) Uani 1 1 d . . .
C7 C 0.7971(2) 0.0380(2) 0.70516(12) 0.0469(7) Uani 1 1 d . . .
H7 H 0.8527 -0.0132 0.7284 0.056 Uiso 1 1 calc R . .
C8 C 0.9234(2) 0.0531(2) 0.63074(13) 0.0484(7) Uani 1 1 d . . .
H8A H 0.9807 0.0282 0.6698 0.058 Uiso 1 1 calc R . .
H8B H 0.9045 -0.0129 0.6017 0.058 Uiso 1 1 calc R . .
C9 C 1.0166(2) 0.2454(3) 0.63943(15) 0.0681(9) Uani 1 1 d . . .
H9A H 1.0910 0.2281 0.6695 0.082 Uiso 1 1 calc R . .
H9B H 0.9626 0.2629 0.6650 0.082 Uiso 1 1 calc R . .
C10 C 1.0291(3) 0.3542(3) 0.59696(18) 0.0759(10) Uani 1 1 d . . .
H10A H 0.9536 0.3716 0.5680 0.091 Uiso 1 1 calc R . .
H10B H 1.0518 0.4196 0.6261 0.091 Uiso 1 1 calc R . .
C11 C 1.1126(3) 0.3434(3) 0.55686(18) 0.0760(10) Uani 1 1 d . . .
H11A H 1.1596 0.2752 0.5709 0.091 Uiso 1 1 calc R . .
H11B H 1.1637 0.4098 0.5651 0.091 Uiso 1 1 calc R . .
C12 C 1.0585(2) 0.3350(3) 0.48535(17) 0.0637(8) Uani 1 1 d . . .
H12A H 1.0049 0.3987 0.4720 0.076 Uiso 1 1 calc R . .
H12B H 1.1183 0.3428 0.4625 0.076 Uiso 1 1 calc R . .
C13 C 0.9510(2) 0.2167(2) 0.39364(13) 0.0458(7) Uani 1 1 d . . .
H13A H 0.9154 0.1414 0.3833 0.055 Uiso 1 1 calc R . .
H13B H 1.0155 0.2209 0.3741 0.055 Uiso 1 1 calc R . .
N1 N 0.97527(17) 0.1433(2) 0.59824(11) 0.0444(6) Uani 1 1 d . . .
H1N H 1.026(2) 0.120(3) 0.5889(15) 0.067 Uiso 1 1 d . . .
N2 N 0.99633(16) 0.22620(19) 0.46553(11) 0.0411(5) Uani 1 1 d . . .
O1 O 0.74383(13) 0.21470(14) 0.55753(8) 0.0394(4) Uani 1 1 d . . .
Cl1 Cl 0.81955(5) -0.00845(5) 0.46435(3) 0.04005(16) Uani 1 1 d . . .
H2N H 1.041(2) 0.174(2) 0.4765(15) 0.060 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
O1 Zn1 O1 79.81(7) 7_656 . ?
O1 Zn1 N1 150.06(8) 7_656 . ?
O1 Zn1 N1 85.14(7) . . ?
O1 Zn1 N2 87.79(7) 7_656 . ?
O1 Zn1 N2 150.11(8) . . ?
N1 Zn1 N2 92.74(8) . . ?
O1 Zn1 Cl1 106.82(5) 7_656 . ?
O1 Zn1 Cl1 107.45(5) . . ?
N1 Zn1 Cl1 102.33(7) . . ?
N2 Zn1 Cl1 102.14(6) . . ?
O1 Zn1 Zn1 40.06(4) 7_656 7_656 ?
O1 Zn1 Zn1 39.75(4) . 7_656 ?
N1 Zn1 Zn1 120.50(6) . 7_656 ?
N2 Zn1 Zn1 122.82(6) . 7_656 ?
Cl1 Zn1 Zn1 112.585(19) . 7_656 ?
C3 C2 C7 115.7(2) . . ?
C3 C2 C1 122.9(2) . . ?
C7 C2 C1 121.3(3) . . ?
C2 C3 C4 123.8(2) . . ?
C3 C4 C5 119.4(2) . . ?
C3 C4 C13 118.0(2) . 7_656 ?
C5 C4 C13 122.4(2) . 7_656 ?
O1 C5 C6 122.29(19) . . ?
O1 C5 C4 120.3(2) . . ?
C6 C5 C4 117.4(2) . . ?
C7 C6 C5 120.0(2) . . ?
C7 C6 C8 116.1(2) . . ?
C5 C6 C8 123.7(2) . . ?
C2 C7 C6 123.4(2) . . ?
N1 C8 C6 114.9(2) . . ?
N1 C9 C10 111.7(3) . . ?
C11 C10 C9 116.1(3) . . ?
C10 C11 C12 114.4(3) . . ?
N2 C12 C11 113.5(2) . . ?
N2 C13 C4 114.5(2) . 7_656 ?
C9 N1 C8 114.1(2) . . ?
C9 N1 Zn1 116.2(2) . . ?
C8 N1 Zn1 107.98(16) . . ?
C12 N2 C13 112.3(2) . . ?
C12 N2 Zn1 120.54(18) . . ?
C13 N2 Zn1 106.75(14) . . ?
C5 O1 Zn1 131.11(13) . 7_656 ?
C5 O1 Zn1 128.06(13) . . ?
Zn1 O1 Zn1 100.19(7) 7_656 . ?
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
Zn1 O1 2.0310(16) 7_656 ?
Zn1 O1 2.0443(14) . ?
Zn1 N1 2.099(2) . ?
Zn1 N2 2.1103(19) . ?
Zn1 Cl1 2.3129(6) . ?
Zn1 Zn1 3.1261(5) 7_656 ?
C1 C2 1.513(4) . ?
C2 C3 1.378(4) . ?
C2 C7 1.383(3) . ?
C3 C4 1.383(3) . ?
C4 C5 1.420(3) . ?
C4 C13 1.499(3) 7_656 ?
C5 O1 1.341(3) . ?
C5 C6 1.401(3) . ?
C6 C7 1.386(3) . ?
C6 C8 1.518(3) . ?
C8 N1 1.477(3) . ?
C9 N1 1.476(4) . ?
C9 C10 1.580(5) . ?
C10 C11 1.480(4) . ?
C11 C12 1.486(4) . ?
C12 N2 1.468(4) . ?
C13 N2 1.481(3) . ?
C13 C4 1.499(3) 7_656 ?
O1 Zn1 2.0310(16) 7_656 ?
