#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:25:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180338 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/07/7200732.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_7200732
loop_
_publ_author_name
'Abuhmaiera, Ramadan'
'Lan, Yanhua'
'Ako, Ayuk M.'
'Kostakis, George E.'
'Mavrandonakis, Andreas'
'Klopper, Wim'
'Clérac, Rodolphe'
'Anson, Christopher E.'
'Powell, Annie K.'
_publ_section_title
;
 One-dimensional Cu(II) coordination polymers: tuning the structure by
 modulating the “carboxylate arm” lengths of
 polycarboxylate ligands
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1089
_journal_paper_doi               10.1039/b820834d
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C26 H40 Cu N2 O18'
_chemical_formula_weight         732.14
_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                 102.636(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.3062(13)
_cell_length_b                   7.3389(7)
_cell_length_c                   14.9630(14)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      1.46
_cell_volume                     1532.9(3)
_computing_cell_refinement       'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_data_collection       'WinXpose 1.05 (Stoe & Cie GmbH, 2000)'
_computing_data_reduction        'X-Area 1.09 (Stoe & Cie GmbH, 2000)'
_computing_molecular_graphics    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9101
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0409
_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)+(0.0902P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                2830
_reflns_number_total             3234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820834d.txt
_cod_data_source_block           ram4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7200732
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 0.0000 0.0000 0.0000 0.01621(13) Uani 1 2 d S . .
N1 N 0.22030(11) 0.4414(2) -0.11000(10) 0.0167(3) Uani 1 1 d . . .
H1 H 0.1799(18) 0.436(3) -0.0719(17) 0.020 Uiso 1 1 d . . .
C1 C 0.24466(14) 0.2499(2) -0.13353(13) 0.0197(4) Uani 1 1 d . . .
H1A H 0.2953 0.2543 -0.1693 0.024 Uiso 1 1 calc R . .
H1B H 0.1873 0.1925 -0.1723 0.024 Uiso 1 1 calc R . .
C2 C 0.27909(13) 0.1346(3) -0.04851(13) 0.0210(4) Uani 1 1 d . . .
H2A H 0.3287 0.2044 -0.0055 0.025 Uiso 1 1 calc R . .
H2B H 0.3103 0.0243 -0.0665 0.025 Uiso 1 1 calc R . .
C3 C 0.20314(13) 0.0742(2) 0.00287(13) 0.0181(4) Uani 1 1 d . . .
O1 O 0.11645(9) 0.07315(18) -0.04208(9) 0.0190(3) Uani 1 1 d . . .
O2 O 0.23159(10) 0.0220(2) 0.08364(10) 0.0241(3) Uani 1 1 d . . .
O3 O -0.03517(10) 0.7085(2) -0.10227(10) 0.0243(3) Uani 1 1 d . . .
H3 H -0.079(2) 0.640(4) -0.0855(19) 0.037 Uiso 1 1 d . . .
C4 C 0.16840(13) 0.5453(3) -0.19373(12) 0.0184(4) Uani 1 1 d . . .
H4A H 0.1303 0.4596 -0.2384 0.022 Uiso 1 1 calc R . .
H4B H 0.2156 0.6056 -0.2234 0.022 Uiso 1 1 calc R . .
C5 C 0.10277(13) 0.6875(2) -0.16640(13) 0.0187(4) Uani 1 1 d . . .
H5A H 0.1392 0.7614 -0.1151 0.022 Uiso 1 1 calc R . .
H5B H 0.0789 0.7701 -0.2188 0.022 Uiso 1 1 calc R . .
C6 C 0.01916(13) 0.5980(2) -0.13774(12) 0.0166(3) Uani 1 1 d . . .
O4 O 0.00477(10) 0.43493(19) -0.14787(10) 0.0225(3) Uani 1 1 d . . .
O5 O 0.24607(10) 0.5808(2) 0.16788(10) 0.0264(3) Uani 1 1 d . . .
C7 C 0.30376(13) 0.5458(3) -0.05829(12) 0.0174(4) Uani 1 1 d . . .
C8 C 0.37566(13) 0.5945(3) -0.10297(13) 0.0207(4) Uani 1 1 d . . .
H8 H 0.3725 0.5561 -0.1642 0.025 Uiso 1 1 calc R . .
C9 C 0.45216(14) 0.6997(3) -0.05749(14) 0.0225(4) Uani 1 1 d . . .
H9 H 0.5013 0.7339 -0.0878 0.027 Uiso 1 1 calc R . .
C10 C 0.45708(14) 0.7552(3) 0.03222(14) 0.0226(4) Uani 1 1 d . . .
H10 H 0.5088 0.8290 0.0629 0.027 Uiso 1 1 calc R . .
C11 C 0.38593(13) 0.7023(3) 0.07666(13) 0.0201(4) Uani 1 1 d . . .
H11 H 0.3904 0.7383 0.1384 0.024 Uiso 1 1 calc R . .
C12 C 0.30790(13) 0.5972(2) 0.03274(13) 0.0180(4) Uani 1 1 d . . .
C13 C 0.23253(13) 0.5454(3) 0.08565(13) 0.0183(4) Uani 1 1 d . . .
O6 O 0.15771(10) 0.4655(2) 0.03866(10) 0.0225(3) Uani 1 1 d . . .
O7 O -0.07285(10) 0.1284(2) -0.10470(10) 0.0217(3) Uani 1 1 d . . .
H71 H -0.135(2) 0.107(4) -0.1082(19) 0.033 Uiso 1 1 d . . .
H72 H -0.059(2) 0.242(4) -0.1077(19) 0.033 Uiso 1 1 d . . .
O11 O 0.41262(12) 0.4387(2) 0.27847(11) 0.0300(3) Uani 1 1 d . . .
H111 H 0.461(3) 0.499(4) 0.278(2) 0.045 Uiso 1 1 d . . .
H112 H 0.371(3) 0.509(4) 0.245(3) 0.045 Uiso 1 1 d . . .
O12 O 0.40790(11) 0.0978(2) 0.20044(11) 0.0292(3) Uani 1 1 d . . .
H121 H 0.357(3) 0.078(5) 0.163(2) 0.044 Uiso 1 1 d . . .
H122 H 0.405(2) 0.204(5) 0.218(2) 0.044 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'
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
O7 Cu1 O7 180.00(13) 3 . ?
O7 Cu1 O1 92.76(6) 3 . ?
O7 Cu1 O1 87.24(6) . . ?
O7 Cu1 O1 87.24(6) 3 3 ?
O7 Cu1 O1 92.76(6) . 3 ?
O1 Cu1 O1 180.00(7) . 3 ?
O7 Cu1 O3 94.37(6) 3 1_545 ?
O7 Cu1 O3 85.63(6) . 1_545 ?
O1 Cu1 O3 95.93(5) . 1_545 ?
O1 Cu1 O3 84.07(5) 3 1_545 ?
O7 Cu1 O3 85.63(6) 3 3_565 ?
O7 Cu1 O3 94.37(6) . 3_565 ?
O1 Cu1 O3 84.07(5) . 3_565 ?
O1 Cu1 O3 95.93(5) 3 3_565 ?
O3 Cu1 O3 180.00(7) 1_545 3_565 ?
C7 N1 C1 113.67(14) . . ?
C7 N1 C4 111.35(14) . . ?
C1 N1 C4 111.87(14) . . ?
C7 N1 H1 104.3(16) . . ?
C1 N1 H1 108.8(16) . . ?
C4 N1 H1 106.2(16) . . ?
N1 C1 C2 111.91(15) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 116.60(15) . . ?
C1 C2 H2A 108.1 . . ?
C3 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
C3 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
O2 C3 O1 125.63(17) . . ?
O2 C3 C2 117.34(16) . . ?
O1 C3 C2 116.94(16) . . ?
C3 O1 Cu1 128.53(12) . . ?
C6 O3 Cu1 133.38(12) . 1_565 ?
C6 O3 H3 106.6(19) . . ?
Cu1 O3 H3 110.9(19) 1_565 . ?
N1 C4 C5 110.07(14) . . ?
N1 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 C4 110.68(15) . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 O3 123.92(17) . . ?
O4 C6 C5 121.07(16) . . ?
O3 C6 C5 115.00(16) . . ?
C8 C7 C12 121.29(17) . . ?
C8 C7 N1 118.49(16) . . ?
C12 C7 N1 120.21(16) . . ?
C9 C8 C7 119.57(18) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.26(18) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.55(18) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 121.58(17) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C7 117.72(17) . . ?
C11 C12 C13 118.57(16) . . ?
C7 C12 C13 123.71(17) . . ?
O5 C13 O6 124.96(18) . . ?
O5 C13 C12 119.59(17) . . ?
O6 C13 C12 115.46(16) . . ?
Cu1 O7 H71 108.3(18) . . ?
Cu1 O7 H72 115.3(19) . . ?
H71 O7 H72 114(3) . . ?
H111 O11 H112 99(3) . . ?
H121 O12 H122 106(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
Cu1 O7 1.9274(14) 3 ?
Cu1 O7 1.9274(14) . ?
Cu1 O1 1.9797(13) . ?
Cu1 O1 1.9797(13) 3 ?
Cu1 O3 2.6144(15) 1_545 ?
Cu1 O3 2.6144(15) 3_565 ?
N1 C7 1.485(2) . ?
N1 C1 1.508(2) . ?
N1 C4 1.515(2) . ?
N1 H1 0.90(3) . ?
C1 C2 1.518(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.528(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O2 1.248(2) . ?
C3 O1 1.275(2) . ?
O3 C6 1.313(2) . ?
O3 Cu1 2.6144(15) 1_565 ?
O3 H3 0.88(3) . ?
C4 C5 1.518(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.507(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.218(2) . ?
O5 C13 1.231(2) . ?
C7 C8 1.391(3) . ?
C7 C12 1.402(3) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.519(2) . ?
C13 O6 1.286(2) . ?
O7 H71 0.89(3) . ?
O7 H72 0.86(3) . ?
O11 H111 0.82(4) . ?
O11 H112 0.86(4) . ?
O12 H121 0.83(4) . ?
O12 H122 0.83(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O6 0.90(3) 1.77(3) 2.579(2) 150(2) .
O3 H3 O6 0.88(3) 1.65(3) 2.518(2) 170(3) 3_565
O7 H71 O2 0.89(3) 1.78(3) 2.606(2) 153(3) 3
O7 H72 O4 0.86(3) 1.85(3) 2.650(2) 153(3) .
O11 H111 O12 0.82(4) 1.97(4) 2.775(2) 165(3) 2_655
O11 H112 O5 0.86(4) 1.98(4) 2.789(2) 157(3) .
O12 H121 O2 0.83(4) 1.96(4) 2.792(2) 174(3) .
O12 H122 O11 0.83(4) 1.94(4) 2.756(2) 169(3) .
