#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:47:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179764 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006003.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_7006003
loop_
_publ_author_name
'Cheng, Jian-Wen'
'Zheng, Shou-Tian'
'Yang, Guo-Yu'
_publ_section_title
;
 Diversity of crystal structure with different lanthanide ions
 involving in situ oxidation-hydrolysis reaction.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4059
_journal_page_last               4066
_journal_paper_doi               10.1039/b708165k
_journal_year                    2007
_chemical_formula_sum            'C14 H10 Cu N2 O9 Pr'
_chemical_formula_weight         554.69
_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                 106.375(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.113(6)
_cell_length_b                   9.306(2)
_cell_length_c                   17.348(5)
_cell_measurement_reflns_used    4402
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.2283
_cell_volume                     3270.2(15)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12194
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.300
_exptl_absorpt_correction_T_max  0.4801
_exptl_absorpt_correction_T_min  0.2781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.343
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+12.2199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                3404
_reflns_number_total             3728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708165k.txt
_cod_data_source_block           2
_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      C2/c
_cod_database_code               7006003
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
Pr Pr 0.013735(8) 0.683773(17) 0.073138(10) 0.01756(7) Uani 1 1 d . . .
Cu Cu -0.16463(3) 0.07028(10) 0.36426(4) 0.0778(3) Uani 1 1 d . . .
C1 C -0.04075(17) 0.3480(4) 0.11695(19) 0.0224(7) Uani 1 1 d . . .
C2 C -0.07535(17) 0.2797(4) 0.17285(19) 0.0226(7) Uani 1 1 d . . .
C3 C -0.1007(2) 0.3635(4) 0.2225(2) 0.0367(9) Uani 1 1 d . . .
H3A H -0.0982 0.4632 0.2209 0.044 Uiso 1 1 calc R . .
C4 C -0.1301(2) 0.2964(5) 0.2747(3) 0.0447(11) Uani 1 1 d . . .
H4A H -0.1481 0.3535 0.3072 0.054 Uiso 1 1 calc R . .
C5 C -0.1111(3) 0.0757(5) 0.2310(4) 0.0614(16) Uani 1 1 d . . .
H5A H -0.1152 -0.0236 0.2328 0.074 Uiso 1 1 calc R . .
C6 C -0.0815(2) 0.1336(4) 0.1766(3) 0.0460(11) Uani 1 1 d . . .
H6A H -0.0659 0.0741 0.1429 0.055 Uiso 1 1 calc R . .
C7 C 0.12865(16) 0.5218(4) 0.05077(19) 0.0233(7) Uani 1 1 d . . .
C8 C 0.18406(17) 0.4890(4) 0.0142(2) 0.0275(7) Uani 1 1 d . . .
C9 C 0.1772(2) 0.3843(5) -0.0427(3) 0.0503(13) Uani 1 1 d . . .
H9A H 0.1411 0.3226 -0.0538 0.060 Uiso 1 1 calc R . .
C10 C 0.2241(2) 0.3709(6) -0.0837(3) 0.0599(15) Uani 1 1 d . . .
H10A H 0.2181 0.3003 -0.1230 0.072 Uiso 1 1 calc R . .
C11 C 0.2864(3) 0.5486(6) -0.0108(3) 0.0680(18) Uani 1 1 d . . .
H11A H 0.3249 0.6033 0.0023 0.082 Uiso 1 1 calc R . .
C12 C 0.2405(2) 0.5699(6) 0.0322(3) 0.0597(16) Uani 1 1 d . . .
H12A H 0.2482 0.6385 0.0727 0.072 Uiso 1 1 calc R . .
C13 C -0.03588(16) 0.9837(3) -0.02343(19) 0.0206(6) Uani 1 1 d . . .
C14 C -0.03745(16) 0.7443(3) 0.23189(19) 0.0206(6) Uani 1 1 d . . .
N1 N -0.13383(17) 0.1547(4) 0.2808(2) 0.0422(9) Uani 1 1 d . . .
N2 N 0.27729(17) 0.4534(5) -0.0698(2) 0.0472(9) Uani 1 1 d . . .
O1 O -0.01825(13) 0.4718(3) 0.13507(15) 0.0301(6) Uani 1 1 d . . .
O2 O -0.03921(14) 0.2772(3) 0.05639(15) 0.0311(6) Uani 1 1 d . . .
O3 O 0.13566(13) 0.6231(3) 0.09922(16) 0.0345(6) Uani 1 1 d . . .
O4 O 0.07548(12) 0.4510(3) 0.02771(14) 0.0263(5) Uani 1 1 d . . .
O5 O -0.06463(12) 1.0715(2) -0.07681(14) 0.0256(5) Uani 1 1 d . . .
O6 O -0.06134(12) 0.8724(3) -0.00439(15) 0.0277(5) Uani 1 1 d . . .
O7 O -0.07160(12) 0.7263(3) 0.28030(14) 0.0266(5) Uani 1 1 d . . .
O8 O -0.05858(12) 0.7650(3) 0.15794(13) 0.0278(5) Uani 1 1 d . . .
OW O -0.2051(2) -0.1905(5) 0.2675(3) 0.0919(15) 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'
Pr Pr -0.2180 2.8214 '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 Pr O2 132.64(8) . 5_565 ?
O1 Pr O6 126.64(9) . . ?
O2 Pr O6 71.04(8) 5_565 . ?
O1 Pr O5 153.48(8) . 5_575 ?
O2 Pr O5 71.92(8) 5_565 5_575 ?
O6 Pr O5 64.99(8) . 5_575 ?
O1 Pr O4 69.87(8) . 5_565 ?
O2 Pr O4 75.76(8) 5_565 5_565 ?
O6 Pr O4 74.81(8) . 5_565 ?
O5 Pr O4 134.53(8) 5_575 5_565 ?
O1 Pr O8 72.26(8) . . ?
O2 Pr O8 143.90(9) 5_565 . ?
O6 Pr O8 72.86(8) . . ?
O5 Pr O8 92.22(8) 5_575 . ?
O4 Pr O8 95.60(8) 5_565 . ?
O1 Pr O7 78.32(8) . 2 ?
O2 Pr O7 136.32(8) 5_565 2 ?
O6 Pr O7 119.19(8) . 2 ?
O5 Pr O7 75.53(8) 5_575 2 ?
O4 Pr O7 146.55(7) 5_565 2 ?
O8 Pr O7 64.21(8) . 2 ?
O1 Pr O3 97.71(9) . . ?
O2 Pr O3 74.16(9) 5_565 . ?
O6 Pr O3 135.20(9) . . ?
O5 Pr O3 78.05(9) 5_575 . ?
O4 Pr O3 122.27(8) 5_565 . ?
O8 Pr O3 135.38(8) . . ?
O7 Pr O3 71.21(8) 2 . ?
O1 Pr O4 72.62(8) . . ?
O2 Pr O4 67.36(8) 5_565 . ?
O6 Pr O4 132.85(8) . . ?
O5 Pr O4 119.11(7) 5_575 . ?
O4 Pr O4 74.39(8) 5_565 . ?
O8 Pr O4 144.81(8) . . ?
O7 Pr O4 106.13(8) 2 . ?
O3 Pr O4 48.76(8) . . ?
O1 Pr C7 89.14(9) . . ?
O2 Pr C7 64.06(9) 5_565 . ?
O6 Pr C7 134.87(8) . . ?
O5 Pr C7 95.96(9) 5_575 . ?
O4 Pr C7 97.76(9) 5_565 . ?
O8 Pr C7 151.69(8) . . ?
O7 Pr C7 91.71(8) 2 . ?
O3 Pr C7 24.51(9) . . ?
O4 Pr C7 25.15(8) . . ?
N2 Cu N1 155.77(16) 8_456 . ?
O2 C1 O1 126.8(3) . . ?
O2 C1 C2 116.8(3) . . ?
O1 C1 C2 116.4(3) . . ?
C6 C2 C3 118.3(3) . . ?
C6 C2 C1 121.2(3) . . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C4 118.6(4) . . ?
N1 C4 C3 123.3(4) . . ?
N1 C5 C6 123.2(4) . . ?
C2 C6 C5 119.1(4) . . ?
O3 C7 O4 122.3(3) . . ?
O3 C7 C8 118.5(3) . . ?
O4 C7 C8 119.0(3) . . ?
O3 C7 Pr 58.24(17) . . ?
O4 C7 Pr 67.74(17) . . ?
C8 C7 Pr 156.1(2) . . ?
C9 C8 C12 117.6(3) . . ?
C9 C8 C7 120.7(3) . . ?
C12 C8 C7 121.5(3) . . ?
C8 C9 C10 119.6(4) . . ?
N2 C10 C9 123.3(4) . . ?
N2 C11 C12 122.4(4) . . ?
C8 C12 C11 119.5(4) . . ?
O6 C13 O5 125.3(3) . . ?
O6 C13 C13 117.1(4) . 5_575 ?
O5 C13 C13 117.5(3) . 5_575 ?
O8 C14 O7 126.7(3) . . ?
O8 C14 C14 116.8(3) . 2 ?
O7 C14 C14 116.4(3) . 2 ?
C5 N1 C4 117.4(3) . . ?
C5 N1 Cu 121.9(3) . . ?
C4 N1 Cu 120.5(3) . . ?
C10 N2 C11 117.3(3) . . ?
C10 N2 Cu 118.6(3) . 8 ?
C11 N2 Cu 124.1(3) . 8 ?
C1 O1 Pr 140.2(2) . . ?
C1 O2 Pr 138.5(2) . 5_565 ?
C7 O3 Pr 97.2(2) . . ?
C7 O4 Pr 154.6(2) . 5_565 ?
C7 O4 Pr 87.10(19) . . ?
Pr O4 Pr 105.61(8) 5_565 . ?
C13 O5 Pr 117.2(2) . 5_575 ?
C13 O6 Pr 118.0(2) . . ?
C14 O7 Pr 119.1(2) . 2 ?
C14 O8 Pr 117.0(2) . . ?
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
Pr O1 2.431(2) . ?
Pr O2 2.480(2) 5_565 ?
Pr O6 2.490(2) . ?
Pr O5 2.511(2) 5_575 ?
Pr O4 2.515(3) 5_565 ?
Pr O8 2.517(2) . ?
Pr O7 2.522(2) 2 ?
Pr O3 2.548(3) . ?
Pr O4 2.755(2) . ?
Pr C7 2.973(3) . ?
Cu N2 1.911(3) 8_456 ?
Cu N1 1.915(3) . ?
C1 O2 1.248(4) . ?
C1 O1 1.252(4) . ?
C1 C2 1.509(4) . ?
C2 C6 1.369(5) . ?
C2 C3 1.377(5) . ?
C3 C4 1.382(5) . ?
C4 N1 1.328(6) . ?
C5 N1 1.323(6) . ?
C5 C6 1.380(5) . ?
C7 O3 1.243(4) . ?
C7 O4 1.265(4) . ?
C7 C8 1.510(4) . ?
C8 C9 1.366(5) . ?
C8 C12 1.370(5) . ?
C9 C10 1.376(6) . ?
C10 N2 1.326(6) . ?
C11 N2 1.326(6) . ?
C11 C12 1.393(5) . ?
C13 O6 1.254(4) . ?
C13 O5 1.256(4) . ?
C13 C13 1.534(7) 5_575 ?
C14 O8 1.249(4) . ?
C14 O7 1.263(4) . ?
C14 C14 1.528(7) 2 ?
N2 Cu 1.911(3) 8 ?
O2 Pr 2.480(2) 5_565 ?
O4 Pr 2.515(3) 5_565 ?
O5 Pr 2.511(2) 5_575 ?
O7 Pr 2.522(2) 2 ?
