#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/20/7102094.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_7102094
loop_
_publ_author_name
'Ni, Wen-Xiu'
'Li, Mian'
'Zhou, Xiao-Ping'
'Li, Zhen'
'Huang, Xiao-Chun'
'Li, Dan'
_publ_section_title
;
 pH-Induced formation of metalloligand: increasing structure
 dimensionality by tuning number of ligand functional sites.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3479
_journal_page_last               3481
_journal_paper_doi               10.1039/b705603f
_journal_year                    2007
_chemical_formula_sum            'C27 H23 Cu4 N11 O4.5'
_chemical_formula_weight         827.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9969(15)
_cell_length_b                   7.3578(5)
_cell_length_c                   20.3447(14)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.00
_cell_volume                     3292.8(4)
_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      293(2)
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20812
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         4066
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0475
_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)+(0.0713P)²+2.0231P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                3016
_reflns_number_total             4066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b705603f.txt
_cod_data_source_block           Complex2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_sg_symbol_H-M      Pcca
_cod_original_formula_sum        'C27 H23 Cu4 N11 O4.50'
_cod_database_code               7102094
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, 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
O1 O 0.48745(12) 0.2958(3) 0.44312(12) 0.0474(6) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.5000 0.5000 0.03892(17) Uani 1 2 d S . .
Cu2 Cu 0.2500 0.0000 0.82000(3) 0.04666(19) Uani 1 2 d S . .
Cu3 Cu 0.41262(2) -0.42888(7) 0.82581(3) 0.05188(17) Uani 1 1 d . . .
N1 N 0.41700(13) -0.3163(4) 0.36789(16) 0.0440(7) Uani 1 1 d . . .
N2 N 0.42211(13) 0.2056(4) 0.52535(14) 0.0399(6) Uani 1 1 d . . .
N3 N 0.43935(13) 0.3705(4) 0.55296(14) 0.0411(6) Uani 1 1 d . . .
N4 N 0.30568(13) 0.1387(4) 0.74660(14) 0.0442(7) Uani 1 1 d . . .
N5 N 0.34329(17) -0.2885(5) 0.84681(19) 0.0622(9) Uani 1 1 d . . .
N6 N 0.47978(16) -0.4039(4) 0.76815(18) 0.0507(8) Uani 0.50 1 d P . 1
C14 C 0.47978(16) -0.4039(4) 0.76815(18) 0.0507(8) Uani 0.50 1 d P . 2
C1 C 0.45081(18) -0.1849(5) 0.34194(19) 0.0489(9) Uani 1 1 d . . .
H1 H 0.4682 -0.2049 0.3009 0.059 Uiso 1 1 calc R . .
C2 C 0.46150(16) -0.0205(4) 0.37245(19) 0.0441(8) Uani 1 1 d . . .
H2 H 0.4848 0.0682 0.3519 0.053 Uiso 1 1 calc R . .
C3 C 0.43718(15) 0.0105(4) 0.43367(16) 0.0358(7) Uani 1 1 d . . .
C4 C 0.40125(17) -0.1249(5) 0.4608(2) 0.0486(9) Uani 1 1 d . . .
H4 H 0.3833 -0.1082 0.5017 0.058 Uiso 1 1 calc R . .
C5 C 0.39241(17) -0.2836(5) 0.4268(2) 0.0499(9) Uani 1 1 d . . .
H5 H 0.3681 -0.3729 0.4456 0.060 Uiso 1 1 calc R . .
C6 C 0.44967(15) 0.1845(4) 0.46908(16) 0.0376(7) Uani 1 1 d . . .
C7 C 0.41884(17) 0.4154(5) 0.60893(18) 0.0452(8) Uani 1 1 d . . .
H7 H 0.4310 0.5291 0.6240 0.054 Uiso 1 1 calc R . .
C8 C 0.37831(16) 0.3129(5) 0.65392(17) 0.0403(7) Uani 1 1 d . . .
C9 C 0.34599(18) 0.4086(5) 0.70046(19) 0.0466(8) Uani 1 1 d . . .
H9 H 0.3485 0.5347 0.7019 0.056 Uiso 1 1 calc R . .
C10 C 0.31041(17) 0.3184(5) 0.74434(18) 0.0466(8) Uani 1 1 d . . .
H10 H 0.2882 0.3864 0.7744 0.056 Uiso 1 1 calc R . .
C11 C 0.3376(2) 0.0456(5) 0.7034(2) 0.0583(11) Uani 1 1 d . . .
H11 H 0.3357 -0.0806 0.7052 0.070 Uiso 1 1 calc R . .
C12 C 0.3740(2) 0.1246(5) 0.6553(2) 0.0573(11) Uani 1 1 d . . .
H12 H 0.3948 0.0535 0.6250 0.069 Uiso 1 1 calc R . .
C13 C 0.30365(15) -0.1871(5) 0.84710(17) 0.0395(7) Uani 1 1 d . . .
O1W O 0.3043(5) 0.7048(15) 0.5843(5) 0.122(3) Uani 0.50 1 d PU A 1
H1WA H 0.3133 0.8117 0.5968 0.147 Uiso 0.50 1 d PR A 1
H1WB H 0.2659 0.6998 0.5794 0.147 Uiso 0.50 1 d PR A 1
O2W O 0.2264(6) 0.806(2) 0.5003(6) 0.189(5) Uani 0.50 1 d PU B 2
H2WA H 0.2116 0.9021 0.5169 0.227 Uiso 0.50 1 d PR B 2
H2WB H 0.2213 0.7185 0.5271 0.227 Uiso 0.50 1 d PR B 2
O3W O 0.2755(11) 0.716(4) 0.5470(11) 0.134(8) Uani 0.25 1 d PU C 3
H3WA H 0.2545 0.8044 0.5616 0.160 Uiso 0.25 1 d PR C 3
H3WB H 0.2534 0.6510 0.5222 0.160 Uiso 0.25 1 d PR C 3
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
C6 O1 Cu1 110.2(2) . .
O1 Cu1 O1 180.0 5_666 .
O1 Cu1 N3 81.54(11) 5_666 5_666
O1 Cu1 N3 98.46(11) . 5_666
O1 Cu1 N3 98.46(11) 5_666 .
O1 Cu1 N3 81.54(11) . .
N3 Cu1 N3 180.00(12) 5_666 .
C13 Cu2 C13 146.2(2) . 2
C13 Cu2 N4 102.04(13) . 2
C13 Cu2 N4 100.90(14) 2 2
C13 Cu2 N4 100.90(14) . .
C13 Cu2 N4 102.04(13) 2 .
N4 Cu2 N4 93.74(16) 2 .
N5 Cu3 N6 135.67(16) . .
N5 Cu3 N1 116.13(14) . 7_546
N6 Cu3 N1 107.98(13) . 7_546
C1 N1 C5 116.8(3) . .
C1 N1 Cu3 121.5(2) . 7_545
C5 N1 Cu3 121.1(2) . 7_545
C6 N2 N3 109.4(3) . .
C7 N3 N2 119.5(3) . .
C7 N3 Cu1 127.5(2) . .
N2 N3 Cu1 112.8(2) . .
C11 N4 C10 117.0(3) . .
C11 N4 Cu2 120.8(2) . .
C10 N4 Cu2 122.2(2) . .
C13 N5 Cu3 165.7(4) . .
N6 N6 Cu3 174.29(15) 3_656 .
N1 C1 C2 123.7(3) . .
C3 C2 C1 119.1(3) . .
C2 C3 C4 117.6(3) . .
C2 C3 C6 120.5(3) . .
C4 C3 C6 121.9(3) . .
C5 C4 C3 119.5(3) . .
N1 C5 C4 123.3(3) . .
O1 C6 N2 126.0(3) . .
O1 C6 C3 117.9(3) . .
N2 C6 C3 116.1(3) . .
N3 C7 C8 129.4(3) . .
C9 C8 C12 117.4(3) . .
C9 C8 C7 118.3(3) . .
C12 C8 C7 124.1(3) . .
C10 C9 C8 119.9(3) . .
N4 C10 C9 123.6(3) . .
N4 C11 C12 123.9(4) . .
C8 C12 C11 118.0(4) . .
N5 C13 Cu2 160.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C6 1.281(4) .
O1 Cu1 1.916(2) .
Cu1 O1 1.916(2) 5_666
Cu1 N3 1.962(3) 5_666
Cu1 N3 1.962(3) .
Cu2 C13 1.895(3) .
Cu2 C13 1.895(3) 2
Cu2 N4 2.185(3) 2
Cu2 N4 2.184(3) .
Cu3 N5 1.891(4) .
Cu3 N6 1.895(3) .
Cu3 N1 2.063(3) 7_546
N1 C1 1.329(4) .
N1 C5 1.336(5) .
N1 Cu3 2.063(3) 7_545
N2 C6 1.305(4) .
N2 N3 1.390(4) .
N3 C7 1.269(4) .
N4 C11 1.316(5) .
N4 C10 1.327(5) .
N5 C13 1.147(5) .
N6 N6 1.156(7) 3_656
C1 C2 1.380(5) .
C2 C3 1.375(5) .
C3 C4 1.386(5) .
C3 C6 1.495(5) .
C4 C5 1.371(5) .
C7 C8 1.484(5) .
C8 C9 1.377(5) .
C8 C12 1.389(5) .
C9 C10 1.360(5) .
C11 C12 1.393(5) .
