#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:44:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179672 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/25/4512541.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_4512541
loop_
_publ_author_name
'Di Nicola, Corrado'
'Garau, Federica'
'Gazzano, Massimo'
'Lanza, Arianna'
'Monari, Magda'
'Nestola, Fabrizio'
'Pandolfo, Luciano'
'Pettinari, Claudio'
_publ_section_title
;
 Interaction of the Trinuclear Triangular Secondary Building Unit
 [Cu3(μ3-OH)(μ-pz)3]2+with 4,4′-Bipyridine. Structural
 Characterizations of New Coordination Polymers and Hexanuclear
 CuIIClusters. 2°
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1259
_journal_paper_doi               10.1021/cg501647r
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C47 H66 Cu3 N12 O14'
_chemical_formula_weight         1213.74
_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                 105.898(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3303(10)
_cell_length_b                   13.9282(7)
_cell_length_c                   18.8191(8)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.92
_cell_volume                     5377.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51733
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4507
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0438P)²+27.4397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                3871
_reflns_number_total             4507
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            cg501647r_si_002.cif
_cod_data_source_block           comp3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4512540--4512546.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4512541
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
Cu1 Cu 0.443562(19) 0.19017(3) 0.29931(2) 0.01702(14) Uani 1 1 d D
Cu2 Cu 0.48892(9) 0.40218(6) 0.23824(10) 0.0199(4) Uani 0.50 1 d PD
N1 N 0.41251(14) 0.3149(2) 0.32606(16) 0.0213(7) Uani 1 1 d .
C1 C 0.47001(18) -0.0216(3) 0.2888(2) 0.0237(8) Uani 1 1 d .
H1 H 0.4452 -0.0415 0.3211 0.028 Uiso 1 1 calc R
C2 C 0.5000 -0.0824(4) 0.2500 0.0293(13) Uani 1 2 d S
H2 H 0.5000 -0.1506 0.2500 0.035 Uiso 1 2 calc SR
N2 N 0.43319(15) 0.3994(2) 0.30483(16) 0.0241(7) Uani 1 1 d .
N3 N 0.48133(14) 0.0696(2) 0.27388(16) 0.0182(6) Uani 1 1 d .
C3 C 0.36708(18) 0.3341(3) 0.3612(2) 0.0267(9) Uani 1 1 d .
H3 H 0.3448 0.2873 0.3818 0.032 Uiso 1 1 calc R
C4 C 0.35742(19) 0.4327(3) 0.3630(2) 0.0323(10) Uani 1 1 d .
H4 H 0.3280 0.4661 0.3840 0.039 Uiso 1 1 calc R
C5 C 0.40082(19) 0.4713(3) 0.3271(2) 0.0269(9) Uani 1 1 d .
H5 H 0.4066 0.5378 0.3196 0.032 Uiso 1 1 calc R
O2 O 0.41245(12) 0.12652(19) 0.38042(13) 0.0236(6) Uani 1 1 d .
O3 O 0.51407(14) 0.1584(2) 0.44448(15) 0.0317(6) Uani 1 1 d .
C6 C 0.4582(2) 0.1299(3) 0.4416(2) 0.0253(8) Uani 1 1 d .
C7 C 0.4408(2) 0.0982(3) 0.5105(2) 0.0403(11) Uani 1 1 d .
H7A H 0.4254 0.0316 0.5047 0.048 Uiso 1 1 calc R
H7B H 0.4063 0.1397 0.5187 0.048 Uiso 1 1 calc R
H7C H 0.4794 0.1028 0.5530 0.048 Uiso 1 1 calc R
N4 N 0.35158(14) 0.1651(2) 0.20064(16) 0.0222(7) Uani 1 1 d .
N5 N 0.08970(15) 0.1182(3) -0.12643(17) 0.0317(8) Uani 1 1 d .
C8 C 0.29047(17) 0.1867(3) 0.2001(2) 0.0239(8) Uani 1 1 d .
H8 H 0.2829 0.2117 0.2439 0.029 Uiso 1 1 calc R
C9 C 0.23757(17) 0.1746(3) 0.1391(2) 0.0225(8) Uani 1 1 d .
H9 H 0.1951 0.1905 0.1420 0.027 Uiso 1 1 calc R
C10 C 0.24640(17) 0.1392(3) 0.0736(2) 0.0202(8) Uani 1 1 d .
C11 C 0.31010(18) 0.1156(3) 0.0744(2) 0.0268(9) Uani 1 1 d .
H11 H 0.3192 0.0903 0.0314 0.032 Uiso 1 1 calc R
C12 C 0.36021(18) 0.1293(3) 0.1385(2) 0.0287(9) Uani 1 1 d .
H12 H 0.4032 0.1121 0.1379 0.034 Uiso 1 1 calc R
C13 C 0.07844(18) 0.1310(3) -0.0610(2) 0.0274(9) Uani 1 1 d .
H13 H 0.0344 0.1374 -0.0597 0.033 Uiso 1 1 calc R
C14 C 0.12650(17) 0.1356(3) 0.0053(2) 0.0235(8) Uani 1 1 d .
H14 H 0.1153 0.1430 0.0506 0.028 Uiso 1 1 calc R
C15 C 0.19192(17) 0.1292(2) 0.00480(19) 0.0191(7) Uani 1 1 d .
C16 C 0.20350(18) 0.1160(3) -0.0634(2) 0.0268(9) Uani 1 1 d .
H16 H 0.2470 0.1105 -0.0668 0.032 Uiso 1 1 calc R
C17 C 0.15207(19) 0.1106(3) -0.1266(2) 0.0325(10) Uani 1 1 d .
H17 H 0.1616 0.1010 -0.1725 0.039 Uiso 1 1 calc R
O1W O 0.5000 0.5461(3) 0.2500 0.0666(18) Uani 1 2 d SD
H1W H 0.515(3) 0.581(3) 0.2865(13) 0.080 Uiso 1 1 d D
N6 N 0.65714(19) 0.7689(3) 0.3122(2) 0.0436(10) Uani 1 1 d .
C18 C 0.6705(3) 0.8436(4) 0.3562(3) 0.0586(15) Uani 1 1 d .
H18 H 0.6542 0.9043 0.3365 0.070 Uiso 1 1 calc R
C19 C 0.7065(3) 0.8400(4) 0.4288(3) 0.0512(13) Uani 1 1 d .
H19 H 0.7149 0.8973 0.4573 0.061 Uiso 1 1 calc R
C20 C 0.73050(19) 0.7537(3) 0.4606(2) 0.0299(9) Uani 1 1 d .
C21 C 0.7175(3) 0.6755(4) 0.4145(3) 0.0577(15) Uani 1 1 d .
H21 H 0.7334 0.6138 0.4322 0.069 Uiso 1 1 calc R
C22 C 0.6809(3) 0.6873(4) 0.3418(3) 0.0589(15) Uani 1 1 d .
H22 H 0.6725 0.6319 0.3113 0.071 Uiso 1 1 calc R
C23 C 0.2874(2) -0.0273(4) 0.3010(3) 0.0523(14) Uani 1 1 d .
H23A H 0.2474 0.0080 0.2776 0.063 Uiso 1 1 calc R
H23B H 0.2776 -0.0959 0.3021 0.063 Uiso 1 1 calc R
H23C H 0.3192 -0.0173 0.2727 0.063 Uiso 1 1 calc R
O1M O 0.31368(15) 0.0065(2) 0.37410(19) 0.0441(8) Uani 1 1 d .
H1M H 0.3416 0.0492 0.3745 0.053 Uiso 1 1 calc R
O3W O 0.61640(16) 0.1532(2) 0.56753(17) 0.0408(8) Uani 1 1 d D
H3WA H 0.629(2) 0.0948(18) 0.578(3) 0.049 Uiso 1 1 d D
H3WB H 0.5829(17) 0.149(3) 0.5304(19) 0.049 Uiso 1 1 d D
C24 C 0.4505(3) 0.6234(4) 0.0597(3) 0.0562(14) Uani 1 1 d .
H24A H 0.4069 0.5947 0.0461 0.067 Uiso 1 1 calc R
H24B H 0.4829 0.5742 0.0577 0.067 Uiso 1 1 calc R
H24C H 0.4523 0.6752 0.0250 0.067 Uiso 1 1 calc R
O2M O 0.46436(17) 0.6612(2) 0.13256(18) 0.0444(8) Uani 1 1 d .
H2M H 0.5015 0.6865 0.1439 0.053 Uiso 1 1 calc R
O2W O 0.58327(16) 0.2660(2) 0.66600(17) 0.0400(7) Uani 1 1 d D
H2WA H 0.595(2) 0.225(3) 0.638(2) 0.048 Uiso 1 1 d D
H2WB H 0.602(2) 0.249(3) 0.7095(12) 0.048 Uiso 1 1 d D
O1 O 0.4921(8) 0.2623(3) 0.2379(6) 0.015(2) Uani 0.50 1 d PD
H111 H 0.4581(9) 0.2547(13) 0.1940(9) 0.018 Uiso 0.50 1 d PD
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
N1 Cu1 N3 175.65(12) . .
N1 Cu1 O1 87.5(3) . 2_655
N3 Cu1 O1 88.7(3) . 2_655
N1 Cu1 O1 88.2(3) . .
N3 Cu1 O1 88.7(3) . .
O1 Cu1 O1 13.9(4) 2_655 .
N1 Cu1 O2 89.48(11) . .
N3 Cu1 O2 92.86(11) . .
O1 Cu1 O2 153.0(2) 2_655 .
O1 Cu1 O2 166.8(2) . .
N1 Cu1 N4 93.86(11) . .
N3 Cu1 N4 89.40(11) . .
O1 Cu1 N4 108.0(2) 2_655 .
O1 Cu1 N4 94.1(2) . .
O2 Cu1 N4 99.01(10) . .
Cu2 Cu2 O1 88.8(3) 2_655 .
Cu2 Cu2 N2 91.3(6) 2_655 .
O1 Cu2 N2 90.6(6) . .
Cu2 Cu2 O1 75.3(2) 2_655 2_655
O1 Cu2 O1 13.9(4) . 2_655
N2 Cu2 O1 87.6(6) . 2_655
Cu2 Cu2 O1W 82.16(3) 2_655 .
O1 Cu2 O1W 170.8(3) . .
N2 Cu2 O1W 91.30(12) . .
O1 Cu2 O1W 157.4(2) 2_655 .
Cu2 Cu2 N2 73.0(5) 2_655 2_655
O1 Cu2 N2 86.9(6) . 2_655
N2 Cu2 N2 164.14(7) . 2_655
O1 Cu2 N2 86.3(6) 2_655 2_655
O1W Cu2 N2 88.78(11) . 2_655
Cu2 Cu2 N5 167.0(5) 2_655 7
O1 Cu2 N5 83.8(2) . 7
N2 Cu2 N5 99.43(14) . 7
O1 Cu2 N5 97.7(2) 2_655 7
O1W Cu2 N5 104.70(10) . 7
N2 Cu2 N5 95.88(15) 2_655 7
C3 N1 N2 108.0(3) . .
C3 N1 Cu1 129.8(3) . .
N2 N1 Cu1 122.0(2) . .
N3 C1 C2 109.5(3) . .
C1 C2 C1 104.6(5) . 2_655
C5 N2 N1 108.5(3) . .
C5 N2 Cu2 129.8(3) . .
N1 N2 Cu2 120.8(2) . .
C5 N2 Cu2 130.8(3) . 2_655
N1 N2 Cu2 120.0(2) . 2_655
Cu2 N2 Cu2 15.70(6) . 2_655
C1 N3 N3 108.2(2) . 2_655
C1 N3 Cu1 130.3(2) . .
N3 N3 Cu1 120.88(9) 2_655 .
N1 C3 C4 110.0(4) . .
C3 C4 C5 104.3(4) . .
N2 C5 C4 109.2(4) . .
C6 O2 Cu1 109.4(2) . .
O3 C6 O2 122.2(3) . .
O3 C6 C7 120.9(4) . .
O2 C6 C7 116.9(4) . .
C12 N4 C8 116.6(3) . .
C12 N4 Cu1 117.9(2) . .
C8 N4 Cu1 125.5(2) . .
C13 N5 C17 116.5(3) . .
C13 N5 Cu2 125.9(3) . 7
C17 N5 Cu2 117.5(3) . 7
N4 C8 C9 123.6(3) . .
C8 C9 C10 120.1(3) . .
C9 C10 C11 116.3(3) . .
C9 C10 C15 122.8(3) . .
C11 C10 C15 120.9(3) . .
C12 C11 C10 119.6(3) . .
N4 C12 C11 123.8(3) . .
N5 C13 C14 124.4(3) . .
C13 C14 C15 119.0(3) . .
C16 C15 C14 116.5(3) . .
C16 C15 C10 121.5(3) . .
C14 C15 C10 122.0(3) . .
C17 C16 C15 120.3(4) . .
N5 C17 C16 123.4(4) . .
Cu2 O1W Cu2 15.67(6) . 2_655
C22 N6 C18 115.4(4) . .
N6 C18 C19 124.4(5) . .
C18 C19 C20 120.3(5) . .
C21 C20 C19 115.5(4) . .
C21 C20 C20 122.3(5) . 7_666
C19 C20 C20 122.1(5) . 7_666
C20 C21 C22 119.4(5) . .
N6 C22 C21 125.0(5) . .
O1 O1 Cu2 90.7(3) 2_655 .
O1 O1 Cu1 88(4) 2_655 2_655
Cu2 O1 Cu1 122.5(10) . 2_655
O1 O1 Cu2 75.3(3) 2_655 2_655
Cu2 O1 Cu2 15.89(7) . 2_655
Cu1 O1 Cu2 117.0(9) 2_655 2_655
O1 O1 Cu1 78(4) 2_655 .
Cu2 O1 Cu1 118.1(9) . .
Cu1 O1 Cu1 117.7(2) 2_655 .
Cu2 O1 Cu1 117.2(8) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.973(3) .
Cu1 N3 1.977(3) .
Cu1 O1 1.976(18) 2_655
Cu1 O1 2.018(18) .
Cu1 O2 2.028(2) .
Cu1 N4 2.329(3) .
Cu2 Cu2 0.552(2) 2_655
Cu2 O1 1.950(4) .
Cu2 N2 1.950(4) .
Cu2 O1 2.016(5) 2_655
Cu2 O1W 2.024(4) .
Cu2 N2 2.039(4) 2_655
Cu2 N5 2.321(3) 7
N1 C3 1.341(5) .
N1 N2 1.355(4) .
C1 N3 1.337(5) .
C1 C2 1.384(5) .
C2 C1 1.384(5) 2_655
N2 C5 1.347(5) .
N2 Cu2 2.039(4) 2_655
N3 N3 1.354(6) 2_655
C3 C4 1.390(6) .
C4 C5 1.394(6) .
O2 C6 1.290(5) .
O3 C6 1.244(5) .
C6 C7 1.510(5) .
N4 C12 1.329(5) .
N4 C8 1.335(5) .
N5 C13 1.330(5) .
N5 C17 1.335(5) .
N5 Cu2 2.321(3) 7
C8 C9 1.381(5) .
C9 C10 1.388(5) .
C10 C11 1.394(5) .
C10 C15 1.490(5) .
C11 C12 1.388(5) .
C13 C14 1.382(5) .
C14 C15 1.401(5) .
C15 C16 1.384(5) .
C16 C17 1.382(5) .
O1W Cu2 2.024(4) 2_655
N6 C22 1.305(7) .
N6 C18 1.312(7) .
C18 C19 1.373(7) .
C19 C20 1.377(6) .
C20 C21 1.373(7) .
C20 C20 1.491(8) 7_666
C21 C22 1.387(7) .
C23 O1M 1.417(6) .
C24 O2M 1.423(6) .
O1 O1 0.485(15) 2_655
O1 Cu1 1.976(18) 2_655
O1 Cu2 2.016(5) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M H1M O2 0.84 1.83 2.666(4) 170.6 .
O2M H2M O2W 0.84 1.80 2.643(5) 176.2 6_565
O1W H1W O2M 0.827(19) 1.85(2) 2.666(4) 171(7) 2_655
O2W H2WA O3W 0.854(19) 1.82(2) 2.669(5) 170(5) .
O3W H3WA O1M 0.861(19) 1.92(2) 2.735(5) 156(4) 5_656
O3W H3WB O3 0.853(19) 1.87(2) 2.713(4) 171(5) .
O2W H2WB N6 0.841(19) 1.98(2) 2.813(5) 168(5) 6_566
