#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:34:44 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179668 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/21/4512113.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_4512113
loop_
_publ_author_name
'Li, Zhuo'
'Wang, Yu-Fang'
'Liu, Bin'
'Zheng, Tian-Yu'
'Zhang, Shi-Chao'
'Zhao, Jian-She'
_publ_section_title
;
 Pressure-Dependent Pseudo-Polymorphism of Polymeric
 {[Cu2(TBA)]·2H2O}nand Dinuclear [Cu2(TBA)(H2O)2]·2H2O
 Complexes Based on in Situ Tetramerization of DMBA
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5640
_journal_paper_doi               10.1021/cg500935a
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C26 H26 Cu2 N8 O14'
_chemical_formula_weight         801.63
_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                 120.542(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.291(7)
_cell_length_b                   10.161(3)
_cell_length_c                   15.215(6)
_cell_measurement_temperature    296(2)
_cell_volume                     2834.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'w 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  0.1528
_diffrn_reflns_av_sigmaI/netI    0.2997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8500
_diffrn_reflns_theta_full        29.76
_diffrn_reflns_theta_max         29.76
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.593
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.382
_refine_ls_extinction_coef       0.0090(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.2655
_refine_ls_R_factor_gt           0.0857
_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)+(0.1088P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.2655
_reflns_number_gt                1137
_reflns_number_total             3635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500935a_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512112--4512113.cif.'
_cod_original_cell_volume        2834.8(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4512113
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
Cu1 Cu 0.68344(7) 0.56409(11) 0.02155(9) 0.0432(5) Uani 1 1 d .
C1 C 0.6549(5) 0.3752(9) 0.1586(8) 0.037(2) Uani 1 1 d .
C2 C 0.6645(5) 0.4128(8) 0.3227(7) 0.037(2) Uani 1 1 d .
C3 C 0.7137(5) 0.3129(9) 0.3628(7) 0.038(2) Uani 1 1 d .
C4 C 0.7301(5) 0.2336(10) 0.3021(8) 0.042(2) Uani 1 1 d .
C5 C 0.7195(6) 0.1884(10) 0.1376(8) 0.054(3) Uani 1 1 d .
H5A H 0.7520 0.1190 0.1780 0.081 Uiso 1 1 calc R
H5B H 0.7427 0.2423 0.1105 0.081 Uiso 1 1 calc R
H5C H 0.6757 0.1510 0.0824 0.081 Uiso 1 1 calc R
C6 C 0.5790(6) 0.5458(10) 0.1696(8) 0.056(3) Uani 1 1 d .
H6A H 0.5653 0.5520 0.0991 0.084 Uiso 1 1 calc R
H6B H 0.5983 0.6288 0.2026 0.084 Uiso 1 1 calc R
H6C H 0.5369 0.5240 0.1742 0.084 Uiso 1 1 calc R
C7 C 0.7589(8) 0.2892(11) 0.4777(11) 0.072(4) Uani 1 1 d .
C8 C 0.8327(6) 0.3637(9) 0.5381(8) 0.045(3) Uani 1 1 d .
C9 C 0.8294(6) 0.4924(10) 0.5678(8) 0.045(3) Uani 1 1 d .
C10 C 0.9569(7) 0.5170(11) 0.6133(10) 0.061(3) Uani 1 1 d .
C11 C 0.8950(6) 0.3084(10) 0.5483(8) 0.042(2) Uani 1 1 d .
C12 C 1.0229(6) 0.3320(12) 0.6026(11) 0.090(5) Uani 1 1 d .
H12A H 1.0154 0.2418 0.5809 0.134 Uiso 1 1 calc R
H12B H 1.0590 0.3365 0.6739 0.134 Uiso 1 1 calc R
H12C H 1.0394 0.3809 0.5642 0.134 Uiso 1 1 calc R
C13 C 0.8930(6) 0.7040(10) 0.6330(9) 0.060(3) Uani 1 1 d .
H13A H 0.8460 0.7270 0.6228 0.090 Uiso 1 1 calc R
H13B H 0.9040 0.7596 0.5916 0.090 Uiso 1 1 calc R
H13C H 0.9293 0.7158 0.7036 0.090 Uiso 1 1 calc R
N1 N 0.6350(4) 0.4423(7) 0.2202(6) 0.0362(18) Uani 1 1 d .
N2 N 0.7012(4) 0.2688(7) 0.2012(6) 0.040(2) Uani 1 1 d .
N3 N 0.9547(4) 0.3878(8) 0.5859(7) 0.051(2) Uani 1 1 d .
N4 N 0.8923(5) 0.5662(8) 0.6042(7) 0.052(2) Uani 1 1 d .
O1 O 0.6311(4) 0.4090(6) 0.0685(5) 0.0420(17) Uani 1 1 d .
O2 O 0.7718(4) 0.1314(6) 0.3332(5) 0.0482(18) Uani 1 1 d .
O3 O 0.6454(4) 0.4838(6) 0.3750(5) 0.0443(18) Uani 1 1 d .
O4 O 0.8998(4) 0.1884(6) 0.5254(5) 0.0463(18) Uani 1 1 d .
O5 O 1.0098(5) 0.5876(8) 0.6431(8) 0.094(3) Uani 1 1 d .
O6 O 0.7743(4) 0.5462(6) 0.5635(5) 0.0488(18) Uani 1 1 d .
O7 O 1.1549(13) 0.575(3) 0.6847(18) 0.319(13) Uani 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'
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
O4 Cu1 O3 88.4(3) 4_655 6_565
O4 Cu1 O2 91.0(3) 4_655 4_655
O3 Cu1 O2 172.9(3) 6_565 4_655
O4 Cu1 O6 172.9(3) 4_655 6_565
O3 Cu1 O6 89.8(3) 6_565 6_565
O2 Cu1 O6 89.9(3) 4_655 6_565
O4 Cu1 O1 93.7(2) 4_655 .
O3 Cu1 O1 101.4(2) 6_565 .
O2 Cu1 O1 85.7(3) 4_655 .
O6 Cu1 O1 93.5(2) 6_565 .
O4 Cu1 C7 95.8(4) 4_655 6_565
O3 Cu1 C7 78.5(3) 6_565 6_565
O2 Cu1 C7 94.5(3) 4_655 6_565
O6 Cu1 C7 77.1(4) 6_565 6_565
O1 Cu1 C7 170.5(4) . 6_565
O1 C1 N2 121.7(9) . .
O1 C1 N1 121.0(9) . .
N2 C1 N1 117.2(9) . .
O3 C2 C3 123.7(9) . .
O3 C2 N1 118.1(8) . .
C3 C2 N1 118.2(9) . .
C2 C3 C4 121.9(9) . .
C2 C3 C7 121.7(9) . .
C4 C3 C7 116.2(9) . .
O2 C4 N2 116.9(9) . .
O2 C4 C3 125.4(9) . .
N2 C4 C3 117.7(9) . .
C7 C7 C3 123.1(19) 7_656 .
C7 C7 C8 119.6(18) 7_656 .
C3 C7 C8 117.3(9) . .
C7 C7 Cu1 79.6(9) 7_656 6_566
C3 C7 Cu1 95.4(7) . 6_566
C8 C7 Cu1 98.3(7) . 6_566
C11 C8 C9 123.4(10) . .
C11 C8 C7 119.7(9) . .
C9 C8 C7 116.3(10) . .
O6 C9 N4 118.1(9) . .
O6 C9 C8 125.9(10) . .
N4 C9 C8 116.0(10) . .
O5 C10 N3 124.1(11) . .
O5 C10 N4 120.3(10) . .
N3 C10 N4 115.5(10) . .
O4 C11 N3 119.4(9) . .
O4 C11 C8 124.1(10) . .
N3 C11 C8 116.5(9) . .
C1 N1 C2 122.3(8) . .
C1 N1 C6 116.1(8) . .
C2 N1 C6 121.6(8) . .
C4 N2 C1 122.2(8) . .
C4 N2 C5 118.2(8) . .
C1 N2 C5 119.5(8) . .
C11 N3 C10 125.2(9) . .
C11 N3 C12 118.5(9) . .
C10 N3 C12 116.3(9) . .
C9 N4 C10 123.3(9) . .
C9 N4 C13 119.9(9) . .
C10 N4 C13 116.8(9) . .
C1 O1 Cu1 123.6(6) . .
C4 O2 Cu1 121.8(6) . 4_645
C2 O3 Cu1 118.5(6) . 6_566
C11 O4 Cu1 121.4(6) . 4_645
C9 O6 Cu1 119.1(6) . 6_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.990(7) 4_655
Cu1 O3 2.008(6) 6_565
Cu1 O2 2.029(6) 4_655
Cu1 O6 2.037(6) 6_565
Cu1 O1 2.247(6) .
Cu1 C7 2.517(10) 6_565
C1 O1 1.244(10) .
C1 N2 1.383(11) .
C1 N1 1.388(11) .
C2 O3 1.283(10) .
C2 C3 1.360(12) .
C2 N1 1.386(12) .
C3 C4 1.398(13) .
C3 C7 1.526(15) .
C4 O2 1.289(11) .
C4 N2 1.380(11) .
C5 N2 1.463(11) .
C6 N1 1.479(11) .
C7 C7 1.22(2) 7_656
C7 C8 1.557(17) .
C7 Cu1 2.517(10) 6_566
C8 C11 1.375(13) .
C8 C9 1.397(13) .
C9 O6 1.264(11) .
C9 N4 1.383(12) .
C10 O5 1.213(13) .
C10 N3 1.371(13) .
C10 N4 1.401(13) .
C11 O4 1.286(11) .
C11 N3 1.360(12) .
C12 N3 1.457(12) .
C13 N4 1.466(12) .
O2 Cu1 2.029(6) 4_645
O3 Cu1 2.008(6) 6_566
O4 Cu1 1.990(7) 4_645
O6 Cu1 2.037(6) 6_566
