#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:18:11 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179684 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/06/7000639.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_7000639
loop_
_publ_author_name
'Takamizawa, Satoshi'
'Nakata, Ei-ichi'
'Miyake, Ryosuke'
_publ_section_title
;
 Structural susceptibility of gas inclusion crystal to external gas
 pressure and temperature: force guide role of channel
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1752
_journal_page_last               1760
_journal_paper_doi               10.1039/b813178c
_journal_year                    2009
_chemical_formula_sum            'C33.22 H28.86 Cu2 N2 O8'
_chemical_formula_weight         711.14
_chemical_name_systematic
; 
 ? 
;
_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                 98.811(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.468(3)
_cell_length_b                   9.7026(14)
_cell_length_c                   19.307(3)
_cell_measurement_temperature    298
_cell_volume                     3418.7(9)
_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      298
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12330
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.8602
_exptl_absorpt_correction_T_min  0.5107
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1457
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0554
_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)+(0.0527P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                1888
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813178c.txt
_cod_data_source_block           311251
_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_original_cell_volume        3418.7(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7000639
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
C1 C 0.1250(3) 0.7305(4) 0.2116(2) 0.0476(11) Uani 1 1 d . . .
C2 C 0.1993(2) 0.7311(4) 0.1907(2) 0.0498(11) Uani 1 1 d . . .
C3 C 0.2286(3) 0.8508(5) 0.1684(3) 0.0817(17) Uani 1 1 d . . .
H3 H 0.2025 0.9328 0.1681 0.098 Uiso 1 1 calc R . .
C4 C 0.2953(4) 0.8501(6) 0.1466(3) 0.101(2) Uani 1 1 d . . .
H4 H 0.3146 0.9314 0.1317 0.122 Uiso 1 1 calc R . .
C5 C 0.3341(3) 0.7289(7) 0.1467(3) 0.0983(19) Uani 1 1 d . . .
H5 H 0.3788 0.7274 0.1302 0.118 Uiso 1 1 calc R . .
C6 C 0.3069(3) 0.6126(6) 0.1707(3) 0.0861(19) Uani 1 1 d . . .
H6 H 0.3340 0.5315 0.1723 0.103 Uiso 1 1 calc R . .
C7 C 0.2398(3) 0.6125(4) 0.1929(3) 0.0663(15) Uani 1 1 d . . .
H7 H 0.2218 0.5315 0.2096 0.080 Uiso 1 1 calc R . .
C8 C 0.0634(2) 0.7214(5) 0.3766(2) 0.0536(11) Uani 1 1 d . . .
C9 C 0.1025(3) 0.7190(5) 0.4491(2) 0.0613(12) Uani 1 1 d . . .
C10 C 0.1374(3) 0.8322(6) 0.4787(3) 0.0895(19) Uani 1 1 d . . .
H10 H 0.1360 0.9140 0.4534 0.107 Uiso 1 1 calc R . .
C11 C 0.1751(4) 0.8269(7) 0.5462(4) 0.117(2) Uani 1 1 d . . .
H11 H 0.1989 0.9052 0.5658 0.140 Uiso 1 1 calc R . .
C12 C 0.1777(4) 0.7098(9) 0.5840(3) 0.114(2) Uani 1 1 d . . .
H12 H 0.2033 0.7066 0.6294 0.137 Uiso 1 1 calc R . .
C13 C 0.1425(4) 0.5966(7) 0.5546(3) 0.113(2) Uani 1 1 d . . .
H13 H 0.1430 0.5158 0.5806 0.135 Uiso 1 1 calc R . .
C14 C 0.1062(3) 0.5996(5) 0.4877(3) 0.0883(19) Uani 1 1 d . . .
H14 H 0.0838 0.5201 0.4679 0.106 Uiso 1 1 calc R . .
C15 C 0.0307(2) 1.1562(3) 0.2041(2) 0.0512(12) Uani 1 1 d . . .
H15 H 0.0530 1.1096 0.1709 0.061 Uiso 1 1 calc R . .
C16 C 0.0306(2) 0.2982(3) 0.2039(2) 0.0508(12) Uani 1 1 d . . .
H16 H 0.0527 0.3451 0.1706 0.061 Uiso 1 1 calc R . .
Cu1 Cu 0.0000 0.85933(6) 0.2500 0.0485(3) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.59262(6) 0.2500 0.0492(3) Uani 1 2 d S . .
N1 N 0.0000 1.0842(4) 0.2500 0.0436(14) Uani 1 2 d S . .
N2 N 0.0000 0.3692(4) 0.2500 0.0428(13) Uani 1 2 d S . .
O1 O 0.09240(16) 0.8440(2) 0.21409(15) 0.0572(9) Uani 1 1 d . . .
O2 O 0.09871(17) 0.6151(2) 0.22572(16) 0.0608(9) Uani 1 1 d . . .
O3 O 0.05380(17) 0.8363(3) 0.34576(15) 0.0608(9) Uani 1 1 d . . .
O4 O 0.04067(18) 0.6086(3) 0.34877(15) 0.0618(9) Uani 1 1 d . . .
C1S C 0.0738(7) 0.8110(13) 0.0135(6) 0.187(9) Uani 0.608(13) 1 d PD . .
H1S H 0.124(2) 0.811(14) 0.006(6) 0.281 Uiso 0.608(13) 1 d PD . .
H2S H 0.059(7) 0.719(5) 0.024(6) 0.281 Uiso 0.608(13) 1 d PD . .
H3S H 0.043(5) 0.844(13) -0.028(4) 0.281 Uiso 0.608(13) 1 d PD . .
H4S H 0.069(7) 0.871(10) 0.052(4) 0.281 Uiso 0.608(13) 1 d PD . .
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'
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 C1 O2 124.3(4) . . ?
O1 C1 C2 118.2(4) . . ?
O2 C1 C2 117.5(4) . . ?
C7 C2 C3 118.6(4) . . ?
C7 C2 C1 120.7(4) . . ?
C3 C2 C1 120.7(4) . . ?
C4 C3 C2 120.7(5) . . ?
C3 C4 C5 119.9(5) . . ?
C6 C5 C4 119.7(5) . . ?
C5 C6 C7 120.7(5) . . ?
C2 C7 C6 120.3(5) . . ?
O4 C8 O3 123.4(4) . . ?
O4 C8 C9 118.2(4) . . ?
O3 C8 C9 118.3(4) . . ?
C10 C9 C14 118.3(5) . . ?
C10 C9 C8 121.3(5) . . ?
C14 C9 C8 120.4(5) . . ?
C9 C10 C11 120.4(6) . . ?
C12 C11 C10 121.0(6) . . ?
C11 C12 C13 118.7(6) . . ?
C12 C13 C14 121.0(6) . . ?
C13 C14 C9 120.6(5) . . ?
N1 C15 C16 122.0(4) . 1_565 ?
N2 C16 C15 121.4(4) . 1_545 ?
O1 Cu1 O1 171.22(14) 2 . ?
O1 Cu1 O3 90.04(13) 2 . ?
O1 Cu1 O3 88.97(13) . . ?
O1 Cu1 O3 88.97(13) 2 2 ?
O1 Cu1 O3 90.04(13) . 2 ?
O3 Cu1 O3 167.00(16) . 2 ?
O1 Cu1 N1 94.39(7) 2 . ?
O1 Cu1 N1 94.39(7) . . ?
O3 Cu1 N1 96.50(8) . . ?
O3 Cu1 N1 96.50(8) 2 . ?
O1 Cu1 Cu2 85.61(7) 2 . ?
O1 Cu1 Cu2 85.61(7) . . ?
O3 Cu1 Cu2 83.50(8) . . ?
O3 Cu1 Cu2 83.50(8) 2 . ?
N1 Cu1 Cu2 180.000(1) . . ?
O4 Cu2 O4 170.87(15) . 2 ?
O4 Cu2 O2 89.45(13) . 2 ?
O4 Cu2 O2 89.54(13) 2 2 ?
O4 Cu2 O2 89.54(13) . . ?
O4 Cu2 O2 89.45(13) 2 . ?
O2 Cu2 O2 167.23(14) 2 . ?
O4 Cu2 N2 94.57(7) . . ?
O4 Cu2 N2 94.57(7) 2 . ?
O2 Cu2 N2 96.38(7) 2 . ?
O2 Cu2 N2 96.38(7) . . ?
O4 Cu2 Cu1 85.43(7) . . ?
O4 Cu2 Cu1 85.43(7) 2 . ?
O2 Cu2 Cu1 83.62(7) 2 . ?
O2 Cu2 Cu1 83.62(7) . . ?
N2 Cu2 Cu1 180.0 . . ?
C15 N1 C15 116.2(4) 2 . ?
C15 N1 Cu1 121.9(2) 2 . ?
C15 N1 Cu1 121.9(2) . . ?
C16 N2 C16 117.1(4) 2 . ?
C16 N2 Cu2 121.5(2) 2 . ?
C16 N2 Cu2 121.5(2) . . ?
C1 O1 Cu1 122.1(3) . . ?
C1 O2 Cu2 123.4(3) . . ?
C8 O3 Cu1 123.7(3) . . ?
C8 O4 Cu2 122.7(3) . . ?
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
C1 O1 1.259(4) . ?
C1 O2 1.267(4) . ?
C1 C2 1.488(6) . ?
C2 C7 1.370(5) . ?
C2 C3 1.378(6) . ?
C3 C4 1.360(7) . ?
C4 C5 1.377(7) . ?
C5 C6 1.345(7) . ?
C6 C7 1.371(6) . ?
C8 O4 1.262(5) . ?
C8 O3 1.264(5) . ?
C8 C9 1.473(6) . ?
C9 C10 1.356(6) . ?
C9 C14 1.373(6) . ?
C10 C11 1.380(7) . ?
C11 C12 1.348(9) . ?
C12 C13 1.356(8) . ?
C13 C14 1.362(7) . ?
C15 N1 1.323(4) . ?
C15 C16 1.378(4) 1_565 ?
C16 N2 1.319(4) . ?
C16 C15 1.378(4) 1_545 ?
Cu1 O1 1.943(3) 2 ?
Cu1 O1 1.943(3) . ?
Cu1 O3 1.973(3) . ?
Cu1 O3 1.973(3) 2 ?
Cu1 N1 2.182(4) . ?
Cu1 Cu2 2.5878(8) . ?
Cu2 O4 1.946(3) . ?
Cu2 O4 1.946(3) 2 ?
Cu2 O2 1.963(3) 2 ?
Cu2 O2 1.963(3) . ?
Cu2 N2 2.168(4) . ?
N1 C15 1.323(4) 2 ?
N2 C16 1.319(4) 2 ?
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
_geom_torsion_publ_flag
O1 C1 C2 C7 174.3(4) . . . . ?
O2 C1 C2 C7 -5.7(6) . . . . ?
O1 C1 C2 C3 -6.0(6) . . . . ?
O2 C1 C2 C3 174.0(4) . . . . ?
C7 C2 C3 C4 2.3(8) . . . . ?
C1 C2 C3 C4 -177.4(5) . . . . ?
C2 C3 C4 C5 0.1(10) . . . . ?
C3 C4 C5 C6 -2.5(10) . . . . ?
C4 C5 C6 C7 2.3(10) . . . . ?
C3 C2 C7 C6 -2.5(7) . . . . ?
C1 C2 C7 C6 177.2(4) . . . . ?
C5 C6 C7 C2 0.2(9) . . . . ?
O4 C8 C9 C10 170.4(5) . . . . ?
O3 C8 C9 C10 -10.1(7) . . . . ?
O4 C8 C9 C14 -7.7(7) . . . . ?
O3 C8 C9 C14 171.8(5) . . . . ?
C14 C9 C10 C11 -0.5(9) . . . . ?
C8 C9 C10 C11 -178.6(5) . . . . ?
C9 C10 C11 C12 -0.3(10) . . . . ?
C10 C11 C12 C13 -0.2(12) . . . . ?
C11 C12 C13 C14 1.4(12) . . . . ?
C12 C13 C14 C9 -2.2(10) . . . . ?
C10 C9 C14 C13 1.7(9) . . . . ?
C8 C9 C14 C13 179.8(5) . . . . ?
O1 Cu1 Cu2 O4 -82.99(13) 2 . . . ?
O1 Cu1 Cu2 O4 97.01(13) . . . . ?
O3 Cu1 Cu2 O4 7.56(13) . . . . ?
O3 Cu1 Cu2 O4 -172.44(13) 2 . . . ?
N1 Cu1 Cu2 O4 76(100) . . . . ?
O1 Cu1 Cu2 O4 97.01(13) 2 . . 2 ?
O1 Cu1 Cu2 O4 -82.99(13) . . . 2 ?
O3 Cu1 Cu2 O4 -172.44(13) . . . 2 ?
O3 Cu1 Cu2 O4 7.56(13) 2 . . 2 ?
N1 Cu1 Cu2 O4 -104(100) . . . 2 ?
O1 Cu1 Cu2 O2 6.97(13) 2 . . 2 ?
O1 Cu1 Cu2 O2 -173.03(13) . . . 2 ?
O3 Cu1 Cu2 O2 97.51(13) . . . 2 ?
O3 Cu1 Cu2 O2 -82.49(13) 2 . . 2 ?
N1 Cu1 Cu2 O2 166(100) . . . 2 ?
O1 Cu1 Cu2 O2 -173.03(13) 2 . . . ?
O1 Cu1 Cu2 O2 6.97(13) . . . . ?
O3 Cu1 Cu2 O2 -82.49(13) . . . . ?
O3 Cu1 Cu2 O2 97.51(13) 2 . . . ?
N1 Cu1 Cu2 O2 -14(100) . . . . ?
O1 Cu1 Cu2 N2 21(100) 2 . . . ?
O1 Cu1 Cu2 N2 -159(100) . . . . ?
O3 Cu1 Cu2 N2 111(100) . . . . ?
O3 Cu1 Cu2 N2 -69(100) 2 . . . ?
N1 Cu1 Cu2 N2 0(42) . . . . ?
C16 C15 N1 C15 -0.1(3) 1_565 . . 2 ?
C16 C15 N1 Cu1 179.9(3) 1_565 . . . ?
O1 Cu1 N1 C15 30.6(2) 2 . . 2 ?
O1 Cu1 N1 C15 -149.4(2) . . . 2 ?
O3 Cu1 N1 C15 -60.0(2) . . . 2 ?
O3 Cu1 N1 C15 120.0(2) 2 . . 2 ?
Cu2 Cu1 N1 C15 -129(100) . . . 2 ?
O1 Cu1 N1 C15 -149.4(2) 2 . . . ?
O1 Cu1 N1 C15 30.6(2) . . . . ?
O3 Cu1 N1 C15 120.0(2) . . . . ?
O3 Cu1 N1 C15 -60.0(2) 2 . . . ?
Cu2 Cu1 N1 C15 51(100) . . . . ?
C15 C16 N2 C16 -0.1(3) 1_545 . . 2 ?
C15 C16 N2 Cu2 179.9(3) 1_545 . . . ?
O4 Cu2 N2 C16 52.3(2) . . . 2 ?
O4 Cu2 N2 C16 -127.7(2) 2 . . 2 ?
O2 Cu2 N2 C16 -37.6(2) 2 . . 2 ?
O2 Cu2 N2 C16 142.4(2) . . . 2 ?
Cu1 Cu2 N2 C16 -51(100) . . . 2 ?
O4 Cu2 N2 C16 -127.7(2) . . . . ?
O4 Cu2 N2 C16 52.3(2) 2 . . . ?
O2 Cu2 N2 C16 142.4(2) 2 . . . ?
O2 Cu2 N2 C16 -37.6(2) . . . . ?
Cu1 Cu2 N2 C16 129(100) . . . . ?
O2 C1 O1 Cu1 6.7(6) . . . . ?
C2 C1 O1 Cu1 -173.4(3) . . . . ?
O1 Cu1 O1 C1 -9.2(3) 2 . . . ?
O3 Cu1 O1 C1 74.3(3) . . . . ?
O3 Cu1 O1 C1 -92.7(3) 2 . . . ?
N1 Cu1 O1 C1 170.8(3) . . . . ?
Cu2 Cu1 O1 C1 -9.2(3) . . . . ?
O1 C1 O2 Cu2 2.9(6) . . . . ?
C2 C1 O2 Cu2 -177.1(3) . . . . ?
O4 Cu2 O2 C1 -92.9(3) . . . . ?
O4 Cu2 O2 C1 78.1(3) 2 . . . ?
O2 Cu2 O2 C1 -7.4(3) 2 . . . ?
N2 Cu2 O2 C1 172.6(3) . . . . ?
Cu1 Cu2 O2 C1 -7.4(3) . . . . ?
O4 C8 O3 Cu1 1.5(6) . . . . ?
C9 C8 O3 Cu1 -178.0(3) . . . . ?
O1 Cu1 O3 C8 78.3(3) 2 . . . ?
O1 Cu1 O3 C8 -93.0(3) . . . . ?
O3 Cu1 O3 C8 -7.3(3) 2 . . . ?
N1 Cu1 O3 C8 172.7(3) . . . . ?
Cu2 Cu1 O3 C8 -7.3(3) . . . . ?
O3 C8 O4 Cu2 8.9(6) . . . . ?
C9 C8 O4 Cu2 -171.6(3) . . . . ?
O4 Cu2 O4 C8 -10.9(3) 2 . . . ?
O2 Cu2 O4 C8 -94.6(4) 2 . . . ?
O2 Cu2 O4 C8 72.7(3) . . . . ?
N2 Cu2 O4 C8 169.1(3) . . . . ?
Cu1 Cu2 O4 C8 -10.9(3) . . . . ?
