#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:30:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179483 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/80/4338095.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_4338095
loop_
_publ_author_name
'Liu, Min-Min'
'Hou, Juan-Juan'
'Qi, Zhi-Kai'
'Duan, Li Na'
'Ji, Wen-Juan'
'Han, Cai-Yun'
'Zhang, Xian-Ming'
_publ_section_title
;
 Tuning of valence States, bonding types, hierarchical structures, and
 physical properties in copper/halide/isonicotinate system.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4130
_journal_page_last               4143
_journal_paper_doi               10.1021/ic5001232
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C12 H12 Cl2 Cu2 N2 O6'
_chemical_formula_weight         478.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.0190(10)
_cell_angle_beta                 100.5900(10)
_cell_angle_gamma                105.6750(10)
_cell_formula_units_Z            2
_cell_length_a                   7.5825(3)
_cell_length_b                   10.5201(5)
_cell_length_c                   11.2163(5)
_cell_measurement_temperature    298(2)
_cell_volume                     783.48(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4299
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    3.088
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0426P)²+0.5752P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2417
_reflns_number_total             2742
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5001232_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4338090--4338098.cif.'
_cod_database_code               4338095
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.790
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu2 Cu 0.30691(7) 0.13497(5) 0.12122(4) 0.02684(15) Uani 1 1 d . .
O1 O 0.2879(4) 0.0044(3) 0.2149(3) 0.0374(7) Uani 1 1 d . .
O2 O 0.2996(4) 0.2350(3) 0.0017(3) 0.0377(7) Uani 1 1 d . .
N3 N 0.2440(4) 0.3966(3) -0.3742(3) 0.0269(7) Uani 1 1 d . .
O4 O 0.2065(4) -0.1916(3) 0.0347(3) 0.0382(7) Uani 1 1 d . .
N5 N 0.2615(4) -0.3758(3) 0.3951(3) 0.0255(7) Uani 1 1 d . .
O6 O 0.5645(4) 0.1411(3) 0.1208(2) 0.0310(6) Uani 1 1 d . .
H6A H 0.5921 0.0822 0.1523 0.046 Uiso 1 1 d R U
H6B H 0.6438 0.2253 0.1680 0.046 Uiso 1 1 d R U
O7 O 0.2979(6) 0.0513(3) -0.1663(3) 0.0608(10) Uani 1 1 d . .
O3 O 0.0507(4) 0.1344(3) 0.1260(3) 0.0351(6) Uani 1 1 d . .
H3A H -0.0194 0.0523 0.1201 0.053 Uiso 1 1 d R U
H3B H -0.0010 0.1525 0.0614 0.053 Uiso 1 1 d R U
C1 C 0.2757(6) 0.4632(4) -0.2448(4) 0.0310(9) Uani 1 1 d . .
H1 H 0.2908 0.5594 -0.2119 0.037 Uiso 1 1 calc R U
C2 C 0.2984(5) -0.2348(4) 0.4490(4) 0.0292(8) Uani 1 1 d . .
H2 H 0.3278 -0.1914 0.5395 0.035 Uiso 1 1 calc R U
C3 C 0.2550(5) -0.2139(4) 0.2411(3) 0.0252(8) Uani 1 1 d . .
C4 C 0.2201(6) 0.2580(4) -0.4202(4) 0.0315(9) Uani 1 1 d . .
H4 H 0.1931 0.2103 -0.5100 0.038 Uiso 1 1 calc R U
C5 C 0.2942(5) -0.1518(4) 0.3750(4) 0.0283(8) Uani 1 1 d . .
H5 H 0.3176 -0.0548 0.4153 0.034 Uiso 1 1 calc R U
C6 C 0.2248(5) -0.4351(4) 0.2647(4) 0.0297(8) Uani 1 1 d . .
H6 H 0.2015 -0.5324 0.2263 0.036 Uiso 1 1 calc R U
C7 C 0.2337(6) 0.1830(4) -0.3399(4) 0.0328(9) Uani 1 1 d . .
H7 H 0.2199 0.0872 -0.3751 0.039 Uiso 1 1 calc R U
C8 C 0.2487(5) -0.1277(4) 0.1554(4) 0.0289(8) Uani 1 1 d . .
C9 C 0.2680(5) 0.2509(4) -0.2066(4) 0.0262(8) Uani 1 1 d . .
C10 C 0.2867(6) 0.3938(4) -0.1591(4) 0.0309(9) Uani 1 1 d . .
H10 H 0.3065 0.4424 -0.0703 0.037 Uiso 1 1 calc R U
C11 C 0.2889(5) 0.1712(4) -0.1171(4) 0.0321(9) Uani 1 1 d . .
C12 C 0.2202(6) -0.3585(4) 0.1853(4) 0.0305(9) Uani 1 1 d . .
H12 H 0.1940 -0.4035 0.0951 0.037 Uiso 1 1 calc R U
Cu1 Cu 0.25034(6) 0.50655(5) -0.49262(4) 0.02689(14) Uani 1 1 d . .
Cl1 Cl 0.55779(13) 0.65469(9) -0.36047(8) 0.0272(2) Uani 1 1 d . .
Cl16 Cl -0.03949(13) 0.34205(10) -0.63470(9) 0.0290(2) 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'
Cl Cl 0.1484 0.1585 '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'
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'
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
O6 Cu2 O2 91.20(11) . .
O6 Cu2 O3 178.28(12) . .
O2 Cu2 O3 88.75(11) . .
O6 Cu2 O1 90.71(11) . .
O2 Cu2 O1 170.10(12) . .
O3 Cu2 O1 89.63(11) . .
O6 Cu2 Cl1 90.70(8) . 2_665
O2 Cu2 Cl1 103.95(9) . 2_665
O3 Cu2 Cl1 87.64(8) . 2_665
O1 Cu2 Cl1 85.73(9) . 2_665
C8 O1 Cu2 121.5(2) . .
C11 O2 Cu2 119.6(2) . .
C4 N3 C1 118.1(3) . .
C4 N3 Cu1 121.1(2) . .
C1 N3 Cu1 120.6(2) . .
C6 N5 C2 117.6(3) . .
C6 N5 Cu1 121.9(2) . 1_546
C2 N5 Cu1 120.5(2) . 1_546
N3 C1 C10 122.3(3) . .
N5 C2 C5 122.5(3) . .
C5 C3 C12 118.4(3) . .
C5 C3 C8 121.5(3) . .
C12 C3 C8 120.1(3) . .
N3 C4 C7 122.6(3) . .
C3 C5 C2 119.4(3) . .
N5 C6 C12 122.9(3) . .
C4 C7 C9 119.6(3) . .
O4 C8 O1 126.0(3) . .
O4 C8 C3 118.1(3) . .
O1 C8 C3 115.9(3) . .
C7 C9 C10 117.9(3) . .
C7 C9 C11 120.2(3) . .
C10 C9 C11 121.9(3) . .
C1 C10 C9 119.4(3) . .
O7 C11 O2 126.6(3) . .
O7 C11 C9 116.6(3) . .
O2 C11 C9 116.8(3) . .
C6 C12 C3 119.2(3) . .
N3 Cu1 N5 177.69(12) . 1_564
N3 Cu1 Cl16 90.68(9) . .
N5 Cu1 Cl16 91.16(9) 1_564 .
N3 Cu1 Cl1 88.33(9) . .
N5 Cu1 Cl1 90.00(9) 1_564 .
Cl16 Cu1 Cl1 173.66(4) . .
Cu1 Cl1 Cu2 132.89(4) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu2 O6 1.937(2) .
Cu2 O2 1.945(2) .
Cu2 O3 1.951(3) .
Cu2 O1 1.963(2) .
Cu2 Cl1 2.6904(10) 2_665
O1 C8 1.263(5) .
O2 C11 1.268(5) .
N3 C4 1.335(5) .
N3 C1 1.344(5) .
N3 Cu1 2.011(3) .
O4 C8 1.244(5) .
N5 C6 1.341(5) .
N5 C2 1.343(5) .
N5 Cu1 2.018(3) 1_546
O7 C11 1.237(5) .
C1 C10 1.378(5) .
C2 C5 1.380(5) .
C3 C5 1.377(5) .
C3 C12 1.381(5) .
C3 C8 1.515(5) .
C4 C7 1.376(5) .
C6 C12 1.376(5) .
C7 C9 1.381(5) .
C9 C10 1.388(5) .
C9 C11 1.508(5) .
Cu1 N5 2.018(3) 1_564
Cu1 Cl16 2.3056(10) .
Cu1 Cl1 2.3234(10) .
Cl1 Cu2 2.6903(10) 2_665
