#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/06/7000640.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_7000640
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            'C33.8 H31.18 Cu2 N2 O8'
_chemical_formula_weight         720.44
_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                 99.259(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.563(3)
_cell_length_b                   9.7095(13)
_cell_length_c                   19.354(3)
_cell_measurement_temperature    298
_cell_volume                     3442.9(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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0977
_diffrn_reflns_av_sigmaI/netI    0.1255
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12380
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.286
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.5381
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4229
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0568
_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)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                1858
_reflns_number_total             4229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b813178c.txt
_cod_data_source_block           311131
_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        3442.8(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C33.80 H31.18 Cu2 N2 O8'
_cod_database_code               7000640
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 0.1237(2) 0.7310(4) 0.2116(2) 0.0442(11) Uani 1 1 d . . .
C2 C 0.1982(2) 0.7309(4) 0.1917(2) 0.0476(12) Uani 1 1 d . . .
C3 C 0.2278(3) 0.8512(5) 0.1701(3) 0.0710(17) Uani 1 1 d . . .
H3 H 0.2011 0.9349 0.1694 0.085 Uiso 1 1 calc R . .
C4 C 0.2950(3) 0.8509(6) 0.1500(4) 0.088(2) Uani 1 1 d . . .
H4 H 0.3151 0.9341 0.1357 0.105 Uiso 1 1 calc R . .
C5 C 0.3333(3) 0.7301(7) 0.1506(3) 0.0865(19) Uani 1 1 d . . .
H5 H 0.3793 0.7289 0.1350 0.104 Uiso 1 1 calc R . .
C6 C 0.3055(3) 0.6119(6) 0.1735(4) 0.081(2) Uani 1 1 d . . .
H6 H 0.3330 0.5291 0.1759 0.097 Uiso 1 1 calc R . .
C7 C 0.2382(3) 0.6123(5) 0.1931(3) 0.0631(16) Uani 1 1 d . . .
H7 H 0.2187 0.5289 0.2080 0.076 Uiso 1 1 calc R . .
C8 C 0.0647(2) 0.7225(5) 0.3757(3) 0.0488(12) Uani 1 1 d . . .
C9 C 0.1043(3) 0.7190(5) 0.4486(3) 0.0537(12) Uani 1 1 d . . .
C10 C 0.1391(3) 0.8334(6) 0.4778(4) 0.0833(19) Uani 1 1 d . . .
H10 H 0.1376 0.9169 0.4520 0.100 Uiso 1 1 calc R . .
C11 C 0.1770(4) 0.8266(7) 0.5457(4) 0.103(2) Uani 1 1 d . . .
H11 H 0.2022 0.9060 0.5655 0.123 Uiso 1 1 calc R . .
C12 C 0.1790(4) 0.7114(8) 0.5840(4) 0.105(2) Uani 1 1 d . . .
H12 H 0.2046 0.7095 0.6307 0.126 Uiso 1 1 calc R . .
C13 C 0.1439(4) 0.5975(7) 0.5552(4) 0.105(2) Uani 1 1 d . . .
H13 H 0.1445 0.5155 0.5821 0.126 Uiso 1 1 calc R . .
C14 C 0.1077(3) 0.6000(5) 0.4877(3) 0.0810(19) Uani 1 1 d . . .
H14 H 0.0847 0.5187 0.4677 0.097 Uiso 1 1 calc R . .
C15 C 0.0300(2) 1.1560(4) 0.2044(3) 0.0455(12) Uani 1 1 d . . .
H15 H 0.0524 1.1081 0.1706 0.055 Uiso 1 1 calc R . .
C16 C 0.0301(2) 0.2981(4) 0.2037(2) 0.0438(11) Uani 1 1 d . . .
H16 H 0.0520 0.3456 0.1695 0.053 Uiso 1 1 calc R . .
Cu1 Cu 0.0000 0.85956(6) 0.2500 0.0424(3) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.59307(6) 0.2500 0.0441(3) Uani 1 2 d S . .
N1 N 0.0000 1.0842(4) 0.2500 0.0375(13) Uani 1 2 d S . .
N2 N 0.0000 0.3691(4) 0.2500 0.0384(13) Uani 1 2 d S . .
O1 O 0.09217(16) 0.8444(3) 0.21407(18) 0.0536(9) Uani 1 1 d . . .
O2 O 0.09795(16) 0.6156(3) 0.22529(18) 0.0542(9) Uani 1 1 d . . .
O3 O 0.05510(16) 0.8373(3) 0.34556(16) 0.0533(9) Uani 1 1 d . . .
O4 O 0.04223(18) 0.6085(3) 0.34889(17) 0.0573(10) Uani 1 1 d . . .
C1S C 0.0733(5) 0.8059(9) 0.0129(5) 0.175(6) Uani 0.898(17) 1 d PD . .
H1S H 0.052(4) 0.847(8) -0.031(2) 0.263 Uiso 0.898(17) 1 d PD . .
H2S H 0.1251(9) 0.799(9) 0.014(5) 0.263 Uiso 0.898(17) 1 d PD . .
H3S H 0.063(5) 0.862(8) 0.051(3) 0.263 Uiso 0.898(17) 1 d PD . .
H4S H 0.053(4) 0.715(4) 0.017(5) 0.263 Uiso 0.898(17) 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 125.3(4) . . ?
O1 C1 C2 117.9(4) . . ?
O2 C1 C2 116.8(4) . . ?
C7 C2 C3 118.5(5) . . ?
C7 C2 C1 121.1(4) . . ?
C3 C2 C1 120.4(4) . . ?
C4 C3 C2 120.6(5) . . ?
C3 C4 C5 119.8(5) . . ?
C6 C5 C4 120.0(6) . . ?
C5 C6 C7 120.1(5) . . ?
C6 C7 C2 121.0(5) . . ?
O3 C8 O4 124.9(4) . . ?
O3 C8 C9 118.3(4) . . ?
O4 C8 C9 116.8(4) . . ?
C10 C9 C14 118.6(5) . . ?
C10 C9 C8 120.4(5) . . ?
C14 C9 C8 121.0(5) . . ?
C9 C10 C11 119.3(6) . . ?
C12 C11 C10 121.9(6) . . ?
C11 C12 C13 118.9(6) . . ?
C12 C13 C14 120.5(6) . . ?
C13 C14 C9 120.8(6) . . ?
N1 C15 C16 122.5(4) . 1_565 ?
N2 C16 C15 120.9(4) . 1_545 ?
O1 Cu1 O1 171.34(15) . 2 ?
O1 Cu1 O3 90.55(14) . 2 ?
O1 Cu1 O3 88.50(14) 2 2 ?
O1 Cu1 O3 88.50(14) . . ?
O1 Cu1 O3 90.55(14) 2 . ?
O3 Cu1 O3 167.45(16) 2 . ?
O1 Cu1 N1 94.33(7) . . ?
O1 Cu1 N1 94.33(7) 2 . ?
O3 Cu1 N1 96.28(8) 2 . ?
O3 Cu1 N1 96.28(8) . . ?
O1 Cu1 Cu2 85.67(7) . . ?
O1 Cu1 Cu2 85.67(7) 2 . ?
O3 Cu1 Cu2 83.72(8) 2 . ?
O3 Cu1 Cu2 83.72(8) . . ?
N1 Cu1 Cu2 180.000(1) . . ?
O4 Cu2 O4 171.20(16) 2 . ?
O4 Cu2 O2 89.67(14) 2 . ?
O4 Cu2 O2 89.36(14) . . ?
O4 Cu2 O2 89.36(14) 2 2 ?
O4 Cu2 O2 89.67(14) . 2 ?
O2 Cu2 O2 167.23(15) . 2 ?
O4 Cu2 N2 94.40(8) 2 . ?
O4 Cu2 N2 94.40(8) . . ?
O2 Cu2 N2 96.39(8) . . ?
O2 Cu2 N2 96.39(8) 2 . ?
O4 Cu2 Cu1 85.60(8) 2 . ?
O4 Cu2 Cu1 85.60(8) . . ?
O2 Cu2 Cu1 83.61(8) . . ?
O2 Cu2 Cu1 83.61(8) 2 . ?
N2 Cu2 Cu1 180.0 . . ?
C15 N1 C15 116.0(5) . 2 ?
C15 N1 Cu1 122.0(2) . . ?
C15 N1 Cu1 122.0(2) 2 . ?
C16 N2 C16 117.2(5) . 2 ?
C16 N2 Cu2 121.4(2) . . ?
C16 N2 Cu2 121.4(2) 2 . ?
C1 O1 Cu1 121.5(3) . . ?
C1 O2 Cu2 123.1(3) . . ?
C8 O3 Cu1 123.0(3) . . ?
C8 O4 Cu2 121.5(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 1.251(5) . ?
C1 O2 1.263(4) . ?
C1 C2 1.494(6) . ?
C2 C7 1.368(5) . ?
C2 C3 1.383(6) . ?
C3 C4 1.365(7) . ?
C4 C5 1.370(7) . ?
C5 C6 1.362(7) . ?
C6 C7 1.363(7) . ?
C8 O3 1.257(5) . ?
C8 O4 1.265(5) . ?
C8 C9 1.482(6) . ?
C9 C10 1.362(6) . ?
C9 C14 1.377(6) . ?
C10 C11 1.388(8) . ?
C11 C12 1.340(8) . ?
C12 C13 1.357(8) . ?
C13 C14 1.370(8) . ?
C15 N1 1.317(4) . ?
C15 C16 1.380(5) 1_565 ?
C16 N2 1.323(4) . ?
C16 C15 1.380(5) 1_545 ?
Cu1 O1 1.953(3) . ?
Cu1 O1 1.953(3) 2 ?
Cu1 O3 1.976(3) 2 ?
Cu1 O3 1.976(3) . ?
Cu1 N1 2.181(4) . ?
Cu1 Cu2 2.5875(8) . ?
Cu2 O4 1.954(3) 2 ?
Cu2 O4 1.954(3) . ?
Cu2 O2 1.965(3) . ?
Cu2 O2 1.965(3) 2 ?
Cu2 N2 2.175(4) . ?
N1 C15 1.317(4) 2 ?
N2 C16 1.323(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 174.8(4) . . . . ?
O2 C1 C2 C7 -4.4(7) . . . . ?
O1 C1 C2 C3 -6.2(7) . . . . ?
O2 C1 C2 C3 174.5(4) . . . . ?
C7 C2 C3 C4 0.8(9) . . . . ?
C1 C2 C3 C4 -178.1(5) . . . . ?
C2 C3 C4 C5 0.5(10) . . . . ?
C3 C4 C5 C6 -2.3(10) . . . . ?
C4 C5 C6 C7 2.8(10) . . . . ?
C5 C6 C7 C2 -1.4(9) . . . . ?
C3 C2 C7 C6 -0.4(8) . . . . ?
C1 C2 C7 C6 178.6(5) . . . . ?
O3 C8 C9 C10 -10.4(7) . . . . ?
O4 C8 C9 C10 170.7(5) . . . . ?
O3 C8 C9 C14 170.8(5) . . . . ?
O4 C8 C9 C14 -8.1(7) . . . . ?
C14 C9 C10 C11 0.1(9) . . . . ?
C8 C9 C10 C11 -178.7(6) . . . . ?
C9 C10 C11 C12 -1.5(12) . . . . ?
C10 C11 C12 C13 1.1(12) . . . . ?
C11 C12 C13 C14 0.7(12) . . . . ?
C12 C13 C14 C9 -2.1(11) . . . . ?
C10 C9 C14 C13 1.6(10) . . . . ?
C8 C9 C14 C13 -179.6(6) . . . . ?
O1 Cu1 Cu2 O4 -83.51(14) . . . 2 ?
O1 Cu1 Cu2 O4 96.49(14) 2 . . 2 ?
O3 Cu1 Cu2 O4 7.52(14) 2 . . 2 ?
O3 Cu1 Cu2 O4 -172.48(14) . . . 2 ?
N1 Cu1 Cu2 O4 -104(42) . . . 2 ?
O1 Cu1 Cu2 O4 96.49(14) . . . . ?
O1 Cu1 Cu2 O4 -83.51(14) 2 . . . ?
O3 Cu1 Cu2 O4 -172.48(14) 2 . . . ?
O3 Cu1 Cu2 O4 7.52(14) . . . . ?
N1 Cu1 Cu2 O4 76(44) . . . . ?
O1 Cu1 Cu2 O2 6.65(14) . . . . ?
O1 Cu1 Cu2 O2 -173.35(14) 2 . . . ?
O3 Cu1 Cu2 O2 97.68(14) 2 . . . ?
O3 Cu1 Cu2 O2 -82.32(14) . . . . ?
N1 Cu1 Cu2 O2 -14(42) . . . . ?
O1 Cu1 Cu2 O2 -173.35(14) . . . 2 ?
O1 Cu1 Cu2 O2 6.65(14) 2 . . 2 ?
O3 Cu1 Cu2 O2 -82.32(14) 2 . . 2 ?
O3 Cu1 Cu2 O2 97.68(14) . . . 2 ?
N1 Cu1 Cu2 O2 166(44) . . . 2 ?
O1 Cu1 Cu2 N2 -159(100) . . . . ?
O1 Cu1 Cu2 N2 21(100) 2 . . . ?
O3 Cu1 Cu2 N2 -68(100) 2 . . . ?
O3 Cu1 Cu2 N2 112(100) . . . . ?
N1 Cu1 Cu2 N2 0(43) . . . . ?
C16 C15 N1 C15 -0.2(3) 1_565 . . 2 ?
C16 C15 N1 Cu1 179.8(3) 1_565 . . . ?
O1 Cu1 N1 C15 30.7(2) . . . . ?
O1 Cu1 N1 C15 -149.3(2) 2 . . . ?
O3 Cu1 N1 C15 -60.4(2) 2 . . . ?
O3 Cu1 N1 C15 119.6(2) . . . . ?
Cu2 Cu1 N1 C15 51(41) . . . . ?
O1 Cu1 N1 C15 -149.3(2) . . . 2 ?
O1 Cu1 N1 C15 30.7(2) 2 . . 2 ?
O3 Cu1 N1 C15 119.6(2) 2 . . 2 ?
O3 Cu1 N1 C15 -60.4(2) . . . 2 ?
Cu2 Cu1 N1 C15 -129(44) . . . 2 ?
C15 C16 N2 C16 -0.2(3) 1_545 . . 2 ?
C15 C16 N2 Cu2 179.8(3) 1_545 . . . ?
O4 Cu2 N2 C16 52.6(2) 2 . . . ?
O4 Cu2 N2 C16 -127.4(2) . . . . ?
O2 Cu2 N2 C16 -37.6(2) . . . . ?
O2 Cu2 N2 C16 142.4(2) 2 . . . ?
Cu1 Cu2 N2 C16 128(100) . . . . ?
O4 Cu2 N2 C16 -127.4(2) 2 . . 2 ?
O4 Cu2 N2 C16 52.6(2) . . . 2 ?
O2 Cu2 N2 C16 142.4(2) . . . 2 ?
O2 Cu2 N2 C16 -37.6(2) 2 . . 2 ?
Cu1 Cu2 N2 C16 -52(100) . . . 2 ?
O2 C1 O1 Cu1 6.5(6) . . . . ?
C2 C1 O1 Cu1 -172.7(3) . . . . ?
O1 Cu1 O1 C1 -8.8(3) 2 . . . ?
O3 Cu1 O1 C1 -92.5(3) 2 . . . ?
O3 Cu1 O1 C1 75.0(3) . . . . ?
N1 Cu1 O1 C1 171.2(3) . . . . ?
Cu2 Cu1 O1 C1 -8.8(3) . . . . ?
O1 C1 O2 Cu2 2.5(6) . . . . ?
C2 C1 O2 Cu2 -178.3(3) . . . . ?
O4 Cu2 O2 C1 78.6(3) 2 . . . ?
O4 Cu2 O2 C1 -92.6(3) . . . . ?
O2 Cu2 O2 C1 -7.0(3) 2 . . . ?
N2 Cu2 O2 C1 173.0(3) . . . . ?
Cu1 Cu2 O2 C1 -7.0(3) . . . . ?
O4 C8 O3 Cu1 1.4(7) . . . . ?
C9 C8 O3 Cu1 -177.4(3) . . . . ?
O1 Cu1 O3 C8 -93.1(4) . . . . ?
O1 Cu1 O3 C8 78.3(4) 2 . . . ?
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 8.8(6) . . . . ?
C9 C8 O4 Cu2 -172.4(3) . . . . ?
O4 Cu2 O4 C8 -10.7(3) 2 . . . ?
O2 Cu2 O4 C8 73.0(4) . . . . ?
O2 Cu2 O4 C8 -94.3(4) 2 . . . ?
N2 Cu2 O4 C8 169.3(3) . . . . ?
Cu1 Cu2 O4 C8 -10.7(3) . . . . ?
