#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:10:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179365 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/62/4326221.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_4326221
loop_
_publ_author_name
'Shun-Ze Zhan'
'Mian Li'
'Xiao-Ping Zhou'
'Jia Ni'
'Xiao-Chun Huang'
'Dan Li'
_publ_section_title
;
 From Simple to Complex: Topological Evolution and Luminescence Variation
 in a Copper(I) Pyridylpyrazolate System Tuned via Second Ligating Spacers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8879
_journal_page_last               8892
_journal_paper_doi               10.1021/ic200854s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C26 H18 Cl3 Cu5 N8'
_chemical_formula_sum            'C26 H18 Cl3 Cu5 N8'
_chemical_formula_weight         866.53
_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                 95.614(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2169(16)
_cell_length_b                   12.7604(14)
_cell_length_c                   14.1543(15)
_cell_measurement_reflns_used    3250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.268
_cell_measurement_theta_min      2.461
_cell_volume                     2735.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9255
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    4.153
_exptl_absorpt_correction_T_max  0.4618
_exptl_absorpt_correction_T_min  0.3893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.104
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0331
_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)+(0.0402P)²+0.3312P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                2664
_reflns_number_total             3116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200854s_si_002_8.cif
_cod_data_source_block           6-Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_database_code               4326221
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 0.11315(2) 0.26356(3) 0.61928(3) 0.03127(12) Uani 1 1 d .
Cu2 Cu -0.07312(2) 0.35742(3) 0.51098(3) 0.02743(12) Uani 1 1 d .
Cu3 Cu 0.0000 0.34225(5) 0.7500 0.04193(17) Uani 1 2 d S
Cl1 Cl 0.03310(4) 0.44511(6) 0.62634(5) 0.02631(16) Uani 1 1 d .
Cl2 Cl 0.0000 0.17025(10) 0.7500 0.0491(3) Uani 1 2 d S
N3 N -0.01417(13) 0.24297(16) 0.45804(16) 0.0171(5) Uani 1 1 d .
N2 N 0.06340(13) 0.20508(17) 0.50165(15) 0.0171(5) Uani 1 1 d .
N4 N -0.28211(15) 0.21652(19) 0.20827(16) 0.0221(5) Uani 1 1 d .
N1 N 0.31629(14) -0.06702(18) 0.51315(16) 0.0217(5) Uani 1 1 d .
C4 C 0.24016(16) 0.0953(2) 0.52411(19) 0.0184(5) Uani 1 1 d .
H4 H 0.2423 0.1651 0.5429 0.022 Uiso 1 1 calc R
C3 C 0.31440(16) 0.0333(2) 0.53935(19) 0.0207(6) Uani 1 1 d .
H3 H 0.3656 0.0628 0.5693 0.025 Uiso 1 1 calc R
C2 C 0.24022(18) -0.1079(2) 0.4725(2) 0.0226(6) Uani 1 1 d .
H2 H 0.2398 -0.1780 0.4546 0.027 Uiso 1 1 calc R
C1 C 0.16314(17) -0.0516(2) 0.45587(18) 0.0199(6) Uani 1 1 d .
H1 H 0.1121 -0.0837 0.4282 0.024 Uiso 1 1 calc R
C5 C 0.16224(16) 0.0534(2) 0.48070(17) 0.0157(5) Uani 1 1 d .
C6 C 0.08197(16) 0.1148(2) 0.45727(18) 0.0153(5) Uani 1 1 d .
C7 C 0.01539(17) 0.0929(2) 0.38599(19) 0.0193(6) Uani 1 1 d .
H7 H 0.0109 0.0350 0.3458 0.023 Uiso 1 1 calc R
C8 C -0.04241(16) 0.1754(2) 0.38776(18) 0.0161(5) Uani 1 1 d .
C9 C -0.12428(16) 0.1916(2) 0.32568(18) 0.0165(5) Uani 1 1 d .
C13 C -0.17348(18) 0.1059(2) 0.28962(19) 0.0233(6) Uani 1 1 d .
H13 H -0.1542 0.0382 0.3046 0.028 Uiso 1 1 calc R
C12 C -0.25027(18) 0.1211(2) 0.2321(2) 0.0253(6) Uani 1 1 d .
H12 H -0.2817 0.0627 0.2085 0.030 Uiso 1 1 calc R
C11 C -0.23394(18) 0.2993(2) 0.2419(2) 0.0262(6) Uani 1 1 d .
H11 H -0.2546 0.3662 0.2258 0.031 Uiso 1 1 calc R
C10 C -0.15579(18) 0.2901(2) 0.2989(2) 0.0242(6) Uani 1 1 d .
H10 H -0.1243 0.3497 0.3194 0.029 Uiso 1 1 calc 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'
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'
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
N2 Cu1 N4 147.44(9) . 8_556
N2 Cu1 Cl1 103.41(6) . .
N4 Cu1 Cl1 102.33(7) 8_556 .
N2 Cu1 Cu3 119.54(6) . .
N4 Cu1 Cu3 92.44(7) 8_556 .
Cl1 Cu1 Cu3 49.30(2) . .
N3 Cu2 N1 145.96(9) . 3_455
N3 Cu2 Cl1 107.85(6) . .
N1 Cu2 Cl1 106.17(7) 3_455 .
Cl2 Cu3 Cl1 125.09(2) . .
Cl2 Cu3 Cl1 125.09(2) . 2_556
Cl1 Cu3 Cl1 109.82(4) . 2_556
Cl2 Cu3 Cu1 69.232(15) . .
Cl1 Cu3 Cu1 60.60(2) . .
Cl1 Cu3 Cu1 153.97(2) 2_556 .
Cl2 Cu3 Cu1 69.233(15) . 2_556
Cl1 Cu3 Cu1 153.97(2) . 2_556
Cl1 Cu3 Cu1 60.60(2) 2_556 2_556
Cu1 Cu3 Cu1 138.47(3) . 2_556
Cu3 Cl1 Cu2 93.88(3) . .
Cu3 Cl1 Cu1 70.10(3) . .
Cu2 Cl1 Cu1 81.37(2) . .
C8 N3 N2 107.73(19) . .
C8 N3 Cu2 130.48(17) . .
N2 N3 Cu2 120.85(16) . .
C6 N2 N3 107.55(19) . .
C6 N2 Cu1 130.75(16) . .
N3 N2 Cu1 120.43(16) . .
C12 N4 C11 116.9(2) . .
C12 N4 Cu1 122.23(19) . 8_455
C11 N4 Cu1 120.60(19) . 8_455
C3 N1 C2 116.7(2) . .
C3 N1 Cu2 121.53(18) . 3_545
C2 N1 Cu2 120.73(18) . 3_545
C3 C4 C5 120.0(2) . .
N1 C3 C4 123.1(2) . .
N1 C2 C1 123.6(3) . .
C2 C1 C5 119.4(2) . .
C1 C5 C4 117.1(2) . .
C1 C5 C6 119.3(2) . .
C4 C5 C6 123.6(2) . .
N2 C6 C7 109.8(2) . .
N2 C6 C5 123.9(2) . .
C7 C6 C5 126.3(2) . .
C8 C7 C6 104.8(2) . .
N3 C8 C7 110.1(2) . .
N3 C8 C9 122.7(2) . .
C7 C8 C9 127.2(2) . .
C10 C9 C13 116.9(2) . .
C10 C9 C8 122.9(2) . .
C13 C9 C8 120.2(2) . .
C12 C13 C9 120.1(3) . .
N4 C12 C13 123.0(3) . .
N4 C11 C10 123.4(3) . .
C11 C10 C9 119.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.912(2) .
Cu1 N4 1.949(2) 8_556
Cu1 Cl1 2.6238(8) .
Cu1 Cu3 2.8319(5) .
Cu2 N3 1.905(2) .
Cu2 N1 1.942(2) 3_455
Cu2 Cl1 2.4525(8) .
Cu3 Cl2 2.1948(14) .
Cu3 Cl1 2.2831(8) .
Cu3 Cl1 2.2831(8) 2_556
Cu3 Cu1 2.8319(5) 2_556
N3 C8 1.355(3) .
N3 N2 1.366(3) .
N2 C6 1.355(3) .
N4 C12 1.341(4) .
N4 C11 1.346(4) .
N4 Cu1 1.949(2) 8_455
N1 C3 1.333(3) .
N1 C2 1.346(4) .
N1 Cu2 1.942(2) 3_545
C4 C3 1.379(3) .
C4 C5 1.388(3) .
C2 C1 1.376(4) .
C1 C5 1.386(4) .
C5 C6 1.462(3) .
C6 C7 1.387(3) .
C7 C8 1.374(3) .
C8 C9 1.467(3) .
C9 C10 1.385(4) .
C9 C13 1.394(4) .
C13 C12 1.371(4) .
C11 C10 1.375(4) .
