#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:50:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179080 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/42/4304281.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_4304281
loop_
_publ_author_name
'Shane G. Telfer'
'Nyree D. Parker'
'Reiko Kuroda'
'Takunori Harada'
'Julie Lefebvre'
'Daniel B. Leznoff'
_publ_section_title
;
Helicates, Boxes, and Polymers from Simple Pyridine-Alcohol Ligands: the
Impact of the Identity of the Transition Metal Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              209
_journal_page_last               218
_journal_paper_doi               10.1021/ic701757e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C28 H34 Cl2 Cu2 N4 O12'
_chemical_formula_weight         816.57
_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                 105.2620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0579(6)
_cell_length_b                   11.7112(7)
_cell_length_c                   13.7986(8)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.10
_cell_volume                     1568.02(16)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9572
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.7405
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+3.1071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                3149
_reflns_number_total             3603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701757e-file012_3.cif
_cod_data_source_block           '[Cu2(1)2(1-H)2](ClO4)2'
_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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304281
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.89211(3) 0.07560(3) 0.43344(2) 0.01246(11) Uani 1 1 d . . .
Cl1 Cl 0.72445(7) 0.60369(6) 0.35753(5) 0.01511(16) Uani 1 1 d . . .
N1 N 0.7192(2) 0.11968(19) 0.47397(17) 0.0119(4) Uani 1 1 d . . .
C2 C 0.6168(3) 0.1938(2) 0.4306(2) 0.0139(5) Uani 1 1 d . . .
C3 C 0.5098(3) 0.2156(3) 0.4744(2) 0.0173(6) Uani 1 1 d . . .
H3 H 0.4403 0.2665 0.4441 0.021 Uiso 1 1 calc R . .
C4 C 0.5063(3) 0.1616(3) 0.5631(2) 0.0198(6) Uani 1 1 d . . .
H4 H 0.4345 0.1756 0.5924 0.024 Uiso 1 1 calc R . .
C5 C 0.6106(3) 0.0869(2) 0.6073(2) 0.0160(6) Uani 1 1 d . . .
H5 H 0.6105 0.0497 0.6668 0.019 Uiso 1 1 calc R . .
C6 C 0.7158(3) 0.0683(2) 0.5613(2) 0.0129(5) Uani 1 1 d . . .
C7 C 0.8344(3) -0.0101(2) 0.6071(2) 0.0148(6) Uani 1 1 d . . .
H7A H 0.8622 -0.0001 0.6794 0.018 Uiso 1 1 calc R . .
H7B H 0.8065 -0.0889 0.5928 0.018 Uiso 1 1 calc R . .
O8 O 0.9452(2) 0.01565(18) 0.56643(15) 0.0163(4) Uani 1 1 d . . .
C9 C 0.6235(3) 0.2536(3) 0.3359(2) 0.0174(6) Uani 1 1 d . . .
H9A H 0.7139 0.2852 0.3443 0.026 Uiso 1 1 calc R . .
H9B H 0.5564 0.3138 0.3214 0.026 Uiso 1 1 calc R . .
H9C H 0.6044 0.2000 0.2813 0.026 Uiso 1 1 calc R . .
N11 N 0.8579(2) 0.10772(19) 0.28786(17) 0.0112(4) Uani 1 1 d . . .
C12 C 0.7843(3) 0.0329(2) 0.2204(2) 0.0159(6) Uani 1 1 d . . .
C13 C 0.7749(3) 0.0428(3) 0.1194(2) 0.0200(6) Uani 1 1 d . . .
H13 H 0.7222 -0.0086 0.0737 0.024 Uiso 1 1 calc R . .
C14 C 0.8451(3) 0.1302(3) 0.0870(2) 0.0202(6) Uani 1 1 d . . .
H14 H 0.8418 0.1370 0.0193 0.024 Uiso 1 1 calc R . .
C15 C 0.9198(3) 0.2073(3) 0.1555(2) 0.0189(6) Uani 1 1 d . . .
H15 H 0.9663 0.2671 0.1344 0.023 Uiso 1 1 calc R . .
C16 C 0.9248(3) 0.1942(2) 0.2565(2) 0.0133(5) Uani 1 1 d . . .
C17 C 1.0064(3) 0.2769(2) 0.3330(2) 0.0170(6) Uani 1 1 d . . .
H17A H 1.1027 0.2739 0.3327 0.020 Uiso 1 1 calc R . .
H17B H 0.9732 0.3539 0.3154 0.020 Uiso 1 1 calc R . .
O18 O 0.9937(3) 0.2498(2) 0.42942(17) 0.0254(5) Uani 1 1 d . . .
C19 C 0.7116(3) -0.0602(3) 0.2628(2) 0.0219(6) Uani 1 1 d . . .
H19A H 0.7723 -0.0896 0.3234 0.033 Uiso 1 1 calc R . .
H19B H 0.6858 -0.1207 0.2145 0.033 Uiso 1 1 calc R . .
H19C H 0.6306 -0.0293 0.2773 0.033 Uiso 1 1 calc R . .
O1 O 0.8239(2) 0.51338(19) 0.36917(17) 0.0257(5) Uani 1 1 d . . .
O2 O 0.7123(3) 0.6611(2) 0.26373(17) 0.0319(6) Uani 1 1 d . . .
O3 O 0.7688(2) 0.6855(2) 0.43877(17) 0.0285(5) Uani 1 1 d . . .
O4 O 0.5932(3) 0.5592(2) 0.3603(2) 0.0353(6) Uani 1 1 d . . .
H18 H 1.082(6) 0.288(5) 0.484(4) 0.073(17) 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'
Cu Cu 0.3201 1.2651 '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
O8 Cu1 O8 77.02(9) . 3_756 ?
O8 Cu1 N11 167.34(9) . . ?
O8 Cu1 N11 91.53(9) 3_756 . ?
O8 Cu1 N1 82.61(9) . . ?
O8 Cu1 N1 156.54(9) 3_756 . ?
N11 Cu1 N1 107.35(9) . . ?
O8 Cu1 O18 109.76(9) . . ?
O8 Cu1 O18 96.22(9) 3_756 . ?
N11 Cu1 O18 76.46(9) . . ?
N1 Cu1 O18 101.56(9) . . ?
O8 Cu1 Cu1 39.09(6) . 3_756 ?
O8 Cu1 Cu1 37.93(6) 3_756 3_756 ?
N11 Cu1 Cu1 129.26(7) . 3_756 ?
N1 Cu1 Cu1 120.83(7) . 3_756 ?
O18 Cu1 Cu1 106.46(6) . 3_756 ?
O4 Cl1 O2 109.57(17) . . ?
O4 Cl1 O1 110.47(15) . . ?
O2 Cl1 O1 109.75(14) . . ?
O4 Cl1 O3 108.53(16) . . ?
O2 Cl1 O3 108.85(15) . . ?
O1 Cl1 O3 109.63(14) . . ?
C6 N1 C2 118.7(2) . . ?
C6 N1 Cu1 110.87(18) . . ?
C2 N1 Cu1 130.29(19) . . ?
N1 C2 C3 120.7(3) . . ?
N1 C2 C9 118.6(2) . . ?
C3 C2 C9 120.7(2) . . ?
C4 C3 C2 120.2(3) . . ?
C5 C4 C3 119.1(3) . . ?
C4 C5 C6 118.7(3) . . ?
N1 C6 C5 122.5(3) . . ?
N1 C6 C7 116.2(2) . . ?
C5 C6 C7 121.3(2) . . ?
O8 C7 C6 109.0(2) . . ?
C7 O8 Cu1 114.37(16) . . ?
C7 O8 Cu1 129.36(17) . 3_756 ?
Cu1 O8 Cu1 102.98(9) . 3_756 ?
C16 N11 C12 119.7(2) . . ?
C16 N11 Cu1 119.95(19) . . ?
C12 N11 Cu1 119.55(19) . . ?
N11 C12 C13 121.5(3) . . ?
N11 C12 C19 115.7(3) . . ?
C13 C12 C19 122.7(3) . . ?
C12 C13 C14 119.0(3) . . ?
C15 C14 C13 119.8(3) . . ?
C14 C15 C16 119.0(3) . . ?
N11 C16 C15 121.0(3) . . ?
N11 C16 C17 118.9(2) . . ?
C15 C16 C17 120.0(3) . . ?
O18 C17 C16 110.5(2) . . ?
C17 O18 Cu1 112.10(18) . . ?
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
Cu1 O8 1.9051(19) . ?
Cu1 O8 1.9542(19) 3_756 ?
Cu1 N11 1.983(2) . ?
Cu1 N1 2.029(2) . ?
Cu1 O18 2.289(2) . ?
Cu1 Cu1 3.0200(7) 3_756 ?
Cl1 O4 1.430(3) . ?
Cl1 O2 1.435(2) . ?
Cl1 O1 1.435(2) . ?
Cl1 O3 1.452(2) . ?
N1 C6 1.356(3) . ?
N1 C2 1.360(4) . ?
C2 C3 1.389(4) . ?
C2 C9 1.500(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.380(4) . ?
C5 C6 1.386(4) . ?
C6 C7 1.505(4) . ?
C7 O8 1.406(3) . ?
O8 Cu1 1.9542(19) 3_756 ?
N11 C16 1.349(4) . ?
N11 C12 1.349(4) . ?
C12 C13 1.376(4) . ?
C12 C19 1.513(4) . ?
C13 C14 1.383(5) . ?
C14 C15 1.378(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.506(4) . ?
C17 O18 1.407(4) . ?
