#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:52:30 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179601 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/65/4506565.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_4506565
loop_
_publ_author_name
'Banerjee, Kaustuv'
'Biradha, Kumar'
_publ_section_title
;
 Design and Synthesis of Mixed Valent Coordination Networks Containing
 Pyridine Appended Terpyridyl, Halide, and Dicarboxylates
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4264
_journal_paper_doi               10.1021/cg300770b
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C56 H42 Br2 Cu3 N8 O10'
_chemical_formula_weight         1337.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 102.469(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.353(3)
_cell_length_b                   10.952(2)
_cell_length_c                   19.413(4)
_cell_measurement_reflns_used    4126
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.69
_cell_volume                     2564.4(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker CCD APEX-2'
_diffrn_measurement_method       hemisphere
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31664
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                4126
_reflns_number_total             5017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300770b_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2564.5(10)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4506565
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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
Br1 Br 0.32186(3) 1.34088(3) -0.255795(16) 0.03799(12) Uani 1 1 d .
Cu1 Cu 0.5000 0.76113(4) 0.2500 0.03198(15) Uani 1 2 d S
Cu2 Cu 0.30704(3) 1.49171(3) -0.150933(17) 0.02638(12) Uani 1 1 d .
N1 N 0.34000(19) 1.36102(19) -0.08227(12) 0.0237(5) Uani 1 1 d .
C1 C 0.2571(2) 1.2967(2) -0.06734(14) 0.0247(6) Uani 1 1 d .
C2 C 0.2773(2) 1.1964(3) -0.02264(15) 0.0281(6) Uani 1 1 d .
H2 H 0.2190 1.1497 -0.0137 0.034 Uiso 1 1 calc R
C3 C 0.3876(2) 1.1669(2) 0.00872(15) 0.0275(6) Uani 1 1 d .
C4 C 0.4721(2) 1.2380(3) -0.00737(14) 0.0273(6) Uani 1 1 d .
H4 H 0.5457 1.2201 0.0127 0.033 Uiso 1 1 calc R
C5 C 0.4463(2) 1.3355(2) -0.05337(14) 0.0260(6) Uani 1 1 d .
N11 N 0.4751(2) 1.5100(2) -0.12067(12) 0.0279(5) Uani 1 1 d .
C11 C 0.5249(2) 1.4229(2) -0.07422(14) 0.0250(6) Uani 1 1 d .
C12 C 0.6382(3) 1.4208(3) -0.04926(15) 0.0313(6) Uani 1 1 d .
H12 H 0.6710 1.3613 -0.0174 0.038 Uiso 1 1 calc R
C13 C 0.7022(3) 1.5094(3) -0.07265(18) 0.0391(8) Uani 1 1 d .
H13 H 0.7787 1.5100 -0.0563 0.047 Uiso 1 1 calc R
C14 C 0.6522(3) 1.5953(3) -0.11962(19) 0.0427(8) Uani 1 1 d .
H14 H 0.6941 1.6551 -0.1357 0.051 Uiso 1 1 calc R
C15 C 0.5381(3) 1.5924(3) -0.14319(16) 0.0357(7) Uani 1 1 d .
H15 H 0.5045 1.6503 -0.1760 0.043 Uiso 1 1 calc R
N21 N 0.15165(19) 1.4510(2) -0.13756(12) 0.0281(5) Uani 1 1 d .
C21 C 0.1464(2) 1.3481(2) -0.09931(14) 0.0264(6) Uani 1 1 d .
C22 C 0.0480(3) 1.3000(3) -0.09032(16) 0.0348(7) Uani 1 1 d .
H22 H 0.0466 1.2286 -0.0646 0.042 Uiso 1 1 calc R
C23 C -0.0504(3) 1.3608(3) -0.12078(18) 0.0392(7) Uani 1 1 d .
H23 H -0.1185 1.3297 -0.1163 0.047 Uiso 1 1 calc R
C24 C -0.0447(3) 1.4668(3) -0.15729(18) 0.0405(8) Uani 1 1 d .
H24 H -0.1089 1.5096 -0.1771 0.049 Uiso 1 1 calc R
C25 C 0.0570(3) 1.5091(3) -0.16414(17) 0.0367(7) Uani 1 1 d .
H25 H 0.0601 1.5817 -0.1885 0.044 Uiso 1 1 calc R
N31 N 0.4588(2) 0.8822(2) 0.16465(13) 0.0336(6) Uani 1 1 d .
C31 C 0.5325(3) 0.9680(3) 0.15919(19) 0.0467(9) Uani 1 1 d .
H31 H 0.6009 0.9661 0.1907 0.056 Uiso 1 1 calc R
C32 C 0.5131(3) 1.0597(3) 0.10923(18) 0.0426(8) Uani 1 1 d .
H32 H 0.5675 1.1178 0.1079 0.051 Uiso 1 1 calc R
C33 C 0.4122(2) 1.0654(3) 0.06083(15) 0.0298(6) Uani 1 1 d .
C34 C 0.3360(3) 0.9739(3) 0.06547(16) 0.0328(7) Uani 1 1 d .
H34 H 0.2679 0.9719 0.0336 0.039 Uiso 1 1 calc R
C35 C 0.3617(3) 0.8857(3) 0.11762(16) 0.0337(7) Uani 1 1 d .
H35 H 0.3091 0.8261 0.1202 0.040 Uiso 1 1 calc R
O1A O 0.0329(3) 2.0144(3) -0.43481(13) 0.0714(10) Uani 1 1 d .
H1O H 0.013(4) 2.014(4) -0.4709(17) 0.050 Uiso 1 1 d .
O2A O 0.0860(2) 1.8215(2) -0.43199(12) 0.0488(6) Uani 1 1 d .
O3A O 0.26516(19) 1.63491(18) -0.20807(11) 0.0360(5) Uani 1 1 d .
O4A O 0.27935(19) 1.7336(2) -0.10657(10) 0.0401(5) Uani 1 1 d .
C1A C 0.1202(3) 1.9326(3) -0.32495(15) 0.0312(6) Uani 1 1 d .
C2A C 0.1633(2) 1.8313(2) -0.28609(15) 0.0284(6) Uani 1 1 d .
H2A H 0.1664 1.7571 -0.3089 0.034 Uiso 1 1 calc R
C3A C 0.2021(2) 1.8383(2) -0.21355(15) 0.0261(6) Uani 1 1 d .
C4A C 0.1947(3) 1.9499(3) -0.18010(16) 0.0344(7) Uani 1 1 d .
H4A H 0.2166 1.9554 -0.1313 0.041 Uiso 1 1 calc R
C5A C 0.1555(3) 2.0510(3) -0.21851(18) 0.0468(9) Uani 1 1 d .
H5A H 0.1542 2.1257 -0.1959 0.056 Uiso 1 1 calc R
C6A C 0.1179(3) 2.0435(3) -0.29059(17) 0.0415(8) Uani 1 1 d .
H6A H 0.0909 2.1128 -0.3163 0.050 Uiso 1 1 calc R
C7A C 0.0769(3) 1.9189(3) -0.40339(16) 0.0372(7) Uani 1 1 d .
C8A C 0.2522(2) 1.7291(3) -0.17229(15) 0.0277(6) Uani 1 1 d .
O1W O 0.8618(3) 1.2638(6) 0.0123(2) 0.144(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'
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'
Br Br -0.2901 2.4595 '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
Cu1 Br1 Cu2 117.265(16) 3_675 .
N31 Cu1 N31 101.57(15) 2_655 .
N31 Cu1 Br1 100.93(7) 2_655 3_675
N31 Cu1 Br1 112.79(7) . 3_675
N31 Cu1 Br1 112.79(7) 2_655 4_576
N31 Cu1 Br1 100.93(7) . 4_576
Br1 Cu1 Br1 125.71(3) 3_675 4_576
O3A Cu2 N1 171.02(9) . .
O3A Cu2 N21 96.21(9) . .
N1 Cu2 N21 79.33(9) . .
O3A Cu2 N11 102.45(9) . .
N1 Cu2 N11 79.93(9) . .
N21 Cu2 N11 155.59(9) . .
O3A Cu2 Br1 96.85(7) . .
N1 Cu2 Br1 91.65(7) . .
N21 Cu2 Br1 100.59(7) . .
N11 Cu2 Br1 92.73(7) . .
C1 N1 C5 122.0(2) . .
C1 N1 Cu2 119.02(18) . .
C5 N1 Cu2 118.89(18) . .
N1 C1 C2 120.9(3) . .
N1 C1 C21 113.1(2) . .
C2 C1 C21 125.9(3) . .
C1 C2 C3 118.7(3) . .
C2 C3 C4 118.6(2) . .
C2 C3 C33 120.2(3) . .
C4 C3 C33 121.2(3) . .
C5 C4 C3 119.8(3) . .
N1 C5 C4 120.0(3) . .
N1 C5 C11 113.0(2) . .
C4 C5 C11 127.0(3) . .
C15 N11 C11 118.7(3) . .
C15 N11 Cu2 127.2(2) . .
C11 N11 Cu2 113.97(18) . .
N11 C11 C12 121.4(3) . .
N11 C11 C5 113.8(2) . .
C12 C11 C5 124.7(3) . .
C11 C12 C13 118.7(3) . .
C14 C13 C12 119.6(3) . .
C13 C14 C15 119.2(3) . .
N11 C15 C14 122.3(3) . .
C25 N21 C21 117.8(3) . .
C25 N21 Cu2 128.1(2) . .
C21 N21 Cu2 114.07(18) . .
N21 C21 C22 122.5(3) . .
N21 C21 C1 113.2(2) . .
C22 C21 C1 124.3(2) . .
C21 C22 C23 118.4(3) . .
C24 C23 C22 119.0(3) . .
C25 C24 C23 119.1(3) . .
N21 C25 C24 123.1(3) . .
C31 N31 C35 116.9(3) . .
C31 N31 Cu1 117.1(2) . .
C35 N31 Cu1 125.8(2) . .
N31 C31 C32 123.5(3) . .
C31 C32 C33 120.1(3) . .
C34 C33 C32 116.4(3) . .
C34 C33 C3 122.7(3) . .
C32 C33 C3 120.9(3) . .
C35 C34 C33 119.9(3) . .
N31 C35 C34 123.2(3) . .
C8A O3A Cu2 113.29(18) . .
C2A C1A C6A 119.0(3) . .
C2A C1A C7A 118.8(3) . .
C6A C1A C7A 122.2(3) . .
C1A C2A C3A 121.1(3) . .
C2A C3A C4A 118.5(3) . .
C2A C3A C8A 120.7(2) . .
C4A C3A C8A 120.8(3) . .
C5A C4A C3A 120.5(3) . .
C4A C5A C6A 120.6(3) . .
C5A C6A C1A 120.1(3) . .
O2A C7A O1A 125.0(3) . .
O2A C7A C1A 120.0(3) . .
O1A C7A C1A 115.1(3) . .
O4A C8A O3A 123.5(3) . .
O4A C8A C3A 120.3(3) . .
O3A C8A C3A 116.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Cu1 2.4488(6) 3_675
Br1 Cu2 2.6584(6) .
Cu1 N31 2.097(2) 2_655
Cu1 N31 2.097(2) .
Cu1 Br1 2.4488(6) 3_675
Cu1 Br1 2.4488(6) 4_576
Cu2 O3A 1.9260(19) .
Cu2 N1 1.938(2) .
Cu2 N21 2.041(2) .
Cu2 N11 2.042(3) .
N1 C1 1.326(3) .
N1 C5 1.341(4) .
C1 C2 1.389(4) .
C1 C21 1.485(4) .
C2 C3 1.404(4) .
C3 C4 1.391(4) .
C3 C33 1.490(4) .
C4 C5 1.384(4) .
C5 C11 1.481(4) .
N11 C15 1.326(4) .
N11 C11 1.365(3) .
C11 C12 1.378(4) .
C12 C13 1.388(4) .
C13 C14 1.362(5) .
C14 C15 1.384(5) .
N21 C25 1.333(4) .
N21 C21 1.359(3) .
C21 C22 1.370(4) .
C22 C23 1.399(4) .
C23 C24 1.370(5) .
C24 C25 1.372(5) .
N31 C31 1.329(4) .
N31 C35 1.342(4) .
C31 C32 1.381(4) .
C32 C33 1.391(4) .
C33 C34 1.391(4) .
C34 C35 1.385(4) .
O1A C7A 1.272(4) .
O2A C7A 1.218(4) .
O3A C8A 1.273(4) .
O4A C8A 1.248(3) .
C1A C2A 1.382(4) .
C1A C6A 1.389(4) .
C1A C7A 1.509(4) .
C2A C3A 1.388(4) .
C3A C4A 1.396(4) .
C3A C8A 1.497(4) .
C4A C5A 1.364(4) .
C5A C6A 1.378(5) .
