#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:27:13 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180394 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/63/7206366.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_7206366
loop_
_publ_author_name
'Biswas, Apurba'
'Saha, Rajat'
'Ghosh, Ashutosh'
_publ_section_title
;
 Two unusual mixed-valent trinuclear CuII2CuI complexes containing
 copper(i) tribromide dianion as bridging ligand: Identification of an
 unprecedented doubly hydrogen-bonded water dimer
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5342
_journal_paper_doi               10.1039/c0ce00784f
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C22 H32 Br5 Cu3 N4 O2, 2(H2 O)'
_chemical_formula_sum            'C22 H36 Br5 Cu3 N4 O4'
_chemical_formula_weight         1010.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 118.944(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.979(10)
_cell_length_b                   10.157(4)
_cell_length_c                   15.902(7)
_cell_measurement_reflns_used    2239
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.03
_cell_volume                     3248(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for windows (Farrugia, 1997)'
_computing_publication_material  'Platon99 (Spek, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6068
_diffrn_reflns_theta_full        23.03
_diffrn_reflns_theta_max         23.03
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    8.131
_exptl_absorpt_correction_T_max  0.375
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    nonref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0624
_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)+(0.1234P)²+13.6695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2024
_reflns_number_gt                1508
_reflns_number_total             2239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00784f.txt
_cod_data_source_block           1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7206366
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
Br4 Br 0.19908(8) 0.9554(2) 0.27629(12) 0.0989(7) Uani 1 1 d .
Br1 Br 0.53508(9) 1.09392(14) 0.39815(9) 0.0790(6) Uani 1 1 d .
Br2 Br 0.5000 1.4398(2) 0.2500 0.1146(10) Uani 1 2 d S
Cu1 Cu 0.53266(6) 0.83447(14) 0.35947(9) 0.0429(5) Uani 1 1 d .
Cu2 Cu 0.5000 1.2088(3) 0.2500 0.0741(8) Uani 1 2 d S
O1 O 0.4455(3) 0.8486(8) 0.2442(5) 0.0481(19) Uani 1 1 d .
N2 N 0.6208(5) 0.7704(11) 0.4708(6) 0.060(3) Uani 1 1 d .
C4 C 0.2789(6) 0.9238(16) 0.2681(9) 0.067(4) Uani 1 1 d .
C5 C 0.3209(5) 0.8280(12) 0.3224(8) 0.044(3) Uani 1 1 d .
H5 H 0.3127 0.7800 0.3654 0.053 Uiso 1 1 calc R
C6 C 0.3763(5) 0.8031(11) 0.3126(7) 0.040(3) Uani 1 1 d .
C7 C 0.4249(6) 0.6988(11) 0.3731(9) 0.052(3) Uani 1 1 d .
H7A H 0.4095 0.6569 0.4136 0.062 Uiso 1 1 calc R
H7B H 0.4282 0.6321 0.3320 0.062 Uiso 1 1 calc R
N1 N 0.4913(4) 0.7597(9) 0.4340(6) 0.045(2) Uani 1 1 d .
H1 H 0.4856 0.8272 0.4669 0.054 Uiso 1 1 calc R
C1 C 0.3898(5) 0.8747(12) 0.2520(8) 0.051(3) Uani 1 1 d .
C2 C 0.3497(7) 0.9804(15) 0.2021(10) 0.071(4) Uani 1 1 d .
H2 H 0.3609 1.0337 0.1645 0.086 Uiso 1 1 calc R
C3 C 0.2930(7) 1.0059(16) 0.2090(10) 0.076(4) Uani 1 1 d .
H3 H 0.2649 1.0754 0.1755 0.092 Uiso 1 1 calc R
C8 C 0.5393(6) 0.6684(13) 0.5051(10) 0.068(4) Uani 1 1 d .
H8A H 0.5394 0.5858 0.4744 0.081 Uiso 1 1 calc R
H8B H 0.5275 0.6506 0.5548 0.081 Uiso 1 1 calc R
C9 C 0.6063(7) 0.7304(16) 0.5478(9) 0.078(4) Uani 1 1 d .
H9A H 0.6076 0.8068 0.5853 0.094 Uiso 1 1 calc R
H9B H 0.6397 0.6683 0.5903 0.094 Uiso 1 1 calc R
C10 C 0.6765(7) 0.8643(17) 0.5160(10) 0.092(5) Uani 1 1 d .
H10A H 0.6886 0.8939 0.4692 0.138 Uiso 1 1 calc R
H10B H 0.7140 0.8218 0.5680 0.138 Uiso 1 1 calc R
H10C H 0.6633 0.9384 0.5403 0.138 Uiso 1 1 calc R
C11 C 0.6439(7) 0.6586(15) 0.4354(11) 0.084(4) Uani 1 1 d .
H11A H 0.6529 0.6884 0.3856 0.126 Uiso 1 1 calc R
H11B H 0.6100 0.5920 0.4101 0.126 Uiso 1 1 calc R
H11C H 0.6837 0.6225 0.4873 0.126 Uiso 1 1 calc R
O2W O 0.3146(16) 0.689(2) 0.5274(15) 0.43(3) Uani 1 1 d .
H1W2 H 0.2913 0.7279 0.5484 0.515 Uiso 1 1 d R
H2W2 H 0.3665 0.7063 0.5833 0.515 Uiso 1 1 d R
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
Cu2 Br1 Cu1 106.96(8) . .
O1 Cu1 O1 76.6(3) 2_655 .
O1 Cu1 N1 157.5(4) 2_655 .
O1 Cu1 N1 91.1(3) . .
O1 Cu1 N2 101.7(3) 2_655 .
O1 Cu1 N2 165.5(4) . .
N1 Cu1 N2 85.5(4) . .
O1 Cu1 Br1 97.8(2) 2_655 .
O1 Cu1 Br1 92.3(2) . .
N1 Cu1 Br1 101.5(3) . .
N2 Cu1 Br1 102.1(3) . .
O1 Cu1 Cu1 38.8(2) 2_655 2_655
O1 Cu1 Cu1 38.46(19) . 2_655
N1 Cu1 Cu1 124.4(3) . 2_655
N2 Cu1 Cu1 136.2(3) . 2_655
Br1 Cu1 Cu1 101.79(4) . 2_655
Br2 Cu2 Br1 119.19(7) . 2_655
Br2 Cu2 Br1 119.19(7) . .
Br1 Cu2 Br1 121.62(13) 2_655 .
C1 O1 Cu1 136.5(6) . 2_655
C1 O1 Cu1 120.4(6) . .
Cu1 O1 Cu1 102.8(3) 2_655 .
C9 N2 C10 105.4(11) . .
C9 N2 C11 111.9(12) . .
C10 N2 C11 107.3(11) . .
C9 N2 Cu1 106.2(7) . .
C10 N2 Cu1 118.6(9) . .
C11 N2 Cu1 107.6(7) . .
C5 C4 C3 122.2(11) . .
C5 C4 Br4 119.1(11) . .
C3 C4 Br4 118.7(11) . .
C4 C5 C6 118.2(11) . .
C4 C5 H5 120.9 . .
C6 C5 H5 120.9 . .
C1 C6 C5 121.5(10) . .
C1 C6 C7 118.5(9) . .
C5 C6 C7 119.9(9) . .
N1 C7 C6 109.6(9) . .
N1 C7 H7A 109.8 . .
C6 C7 H7A 109.8 . .
N1 C7 H7B 109.8 . .
C6 C7 H7B 109.8 . .
H7A C7 H7B 108.2 . .
C8 N1 C7 113.1(9) . .
C8 N1 Cu1 107.6(7) . .
C7 N1 Cu1 113.9(6) . .
C8 N1 H1 107.3 . .
C7 N1 H1 107.3 . .
Cu1 N1 H1 107.3 . .
C6 C1 O1 120.3(10) . .
C6 C1 C2 120.3(10) . .
O1 C1 C2 119.2(11) . .
C3 C2 C1 119.2(13) . .
C3 C2 H2 120.4 . .
C1 C2 H2 120.4 . .
C2 C3 C4 118.1(13) . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
N1 C8 C9 108.1(10) . .
N1 C8 H8A 110.1 . .
C9 C8 H8A 110.1 . .
N1 C8 H8B 110.1 . .
C9 C8 H8B 110.1 . .
H8A C8 H8B 108.4 . .
N2 C9 C8 109.7(11) . .
N2 C9 H9A 109.7 . .
C8 C9 H9A 109.7 . .
N2 C9 H9B 109.7 . .
C8 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
N2 C10 H10A 109.5 . .
N2 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N2 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N2 C11 H11A 109.5 . .
N2 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N2 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
H1W2 O2W H2W2 104.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br4 C4 1.928(12) .
Br1 Cu2 2.392(2) .
Br1 Cu1 2.701(2) .
Br2 Cu2 2.346(4) .
Cu1 O1 1.947(6) 2_655
Cu1 O1 1.959(7) .
Cu1 N1 1.994(8) .
Cu1 N2 2.047(9) .
Cu1 Cu1 3.052(3) 2_655
Cu2 Br1 2.392(2) 2_655
O1 C1 1.371(12) .
O1 Cu1 1.947(6) 2_655
N2 C9 1.473(15) .
N2 C10 1.475(17) .
N2 C11 1.476(16) .
C4 C5 1.348(18) .
C4 C3 1.406(19) .
C5 C6 1.378(13) .
C5 H5 0.9300 .
C6 C1 1.358(15) .
C6 C7 1.502(15) .
C7 N1 1.490(14) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
N1 C8 1.465(14) .
N1 H1 0.9100 .
C1 C2 1.387(17) .
C2 C3 1.386(17) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C8 C9 1.488(18) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
O2W H1W2 0.8512 .
O2W H2W2 1.1025 .
