#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:55:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179084 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304653.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_4304653
loop_
_publ_author_name
'Jing-Xiang Zhang'
'Jun He'
'Ye-Gao Yin'
'Mei-Hong Hu'
'Dan Li'
'Xiao-Chun Huang'
_publ_contact_author_address
;
Department of Chemistry
Shantou University
Shantou
Guangdong 515063
People's Republic of China
;
_publ_contact_author_email       ygyin@stu.edu.cn
_publ_contact_author_fax         '+86 754 2902767'
_publ_contact_author_name
;
Prof. Ye-Gao Yin
;
_publ_contact_author_phone       '+86 754 2903699'
_publ_section_title
;
Novel Thermochromism Relating to Supramolecular Cuprophilic Interaction:
Design, Synthesis, and Luminescence of Copper(I) Pyrazolate Trimer and
Polymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3471
_journal_page_last               3473
_journal_paper_doi               10.1021/ic702189f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C33 H30 Cu6 N12'
_chemical_formula_weight         975.99
_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                 106.176(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.561(4)
_cell_length_b                   20.118(3)
_cell_length_c                   8.0845(12)
_cell_measurement_temperature    298(2)
_cell_volume                     3836.6(10)
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_collection       'SMART, 1998.'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9980
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0512
_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)+(0.0718P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                2718
_reflns_number_total             3377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702189f-file003_2.cif
_cod_data_source_block           compound_2
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304653
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.05033(3) 0.41261(3) 0.66673(8) 0.0457(2) Uani 1 1 d . . .
Cu2 Cu 0.0000 0.55415(4) 0.7500 0.0448(3) Uani 1 2 d S . .
Cu3 Cu 0.31566(3) 0.68250(4) 0.22036(12) 0.0809(3) Uani 1 1 d . . .
Cu4 Cu 0.0000 -0.08951(5) 0.7500 0.0803(4) Uani 1 2 d S . .
N' N 0.2667(3) 0.7357(4) 0.0540(10) 0.113(3) Uani 0.50 1 d P . .
N1 N 0.02036(16) 0.33132(17) 0.7077(5) 0.0416(10) Uani 1 1 d . . .
N2 N 0.08526(16) 0.49170(16) 0.6382(5) 0.0381(9) Uani 1 1 d . . .
N3 N 0.06304(16) 0.55259(19) 0.6655(5) 0.0413(9) Uani 1 1 d . . .
N4 N 0.0000 0.0128(3) 0.7500 0.071(2) Uani 1 2 d S . .
N5 N 0.27004(18) 0.6598(2) 0.3924(6) 0.0534(11) Uani 1 1 d . . .
N6 N 0.1131(3) -0.1426(3) 0.7437(9) 0.0978(19) Uani 1 1 d . . .
C' C 0.2667(3) 0.7357(4) 0.0540(10) 0.113(3) Uani 0.50 1 d P . .
C1 C 0.0740(3) 0.2532(3) 0.5799(8) 0.0631(15) Uani 1 1 d . . .
H1A H 0.0858 0.2939 0.5385 0.095 Uiso 1 1 calc R . .
H1B H 0.0562 0.2252 0.4839 0.095 Uiso 1 1 calc R . .
H1C H 0.1064 0.2308 0.6527 0.095 Uiso 1 1 calc R . .
C2 C 0.0331(2) 0.2682(2) 0.6795(6) 0.0423(11) Uani 1 1 d . . .
C3 C 0.0000 0.2258(3) 0.7500 0.0404(16) Uani 1 2 d S . .
C4 C 0.0000 0.1518(3) 0.7500 0.0450(17) Uani 1 2 d S . .
C5 C 0.0454(3) 0.1164(3) 0.7369(10) 0.085(2) Uani 1 1 d . . .
H5A H 0.0779 0.1381 0.7281 0.102 Uiso 1 1 calc R . .
C6 C 0.0432(3) 0.0473(3) 0.7367(12) 0.094(3) Uani 1 1 d . . .
H6A H 0.0749 0.0242 0.7262 0.113 Uiso 1 1 calc R . .
C7 C 0.1656(2) 0.4448(2) 0.5531(6) 0.0457(12) Uani 1 1 d . . .
H7A H 0.1987 0.4373 0.6479 0.069 Uiso 1 1 calc R . .
H7B H 0.1770 0.4543 0.4512 0.069 Uiso 1 1 calc R . .
H7C H 0.1422 0.4058 0.5345 0.069 Uiso 1 1 calc R . .
C8 C 0.13300(19) 0.5024(2) 0.5933(6) 0.0377(11) Uani 1 1 d . . .
C9 C 0.14239(19) 0.5708(2) 0.5866(5) 0.0362(10) Uani 1 1 d . . .
C10 C 0.09690(19) 0.6003(2) 0.6342(5) 0.0367(10) Uani 1 1 d . . .
C11 C 0.0856(2) 0.6718(2) 0.6628(7) 0.0473(12) Uani 1 1 d . . .
H11A H 0.0766 0.6950 0.5549 0.071 Uiso 1 1 calc R . .
H11B H 0.1186 0.6912 0.7404 0.071 Uiso 1 1 calc R . .
H11C H 0.0542 0.6750 0.7116 0.071 Uiso 1 1 calc R . .
C12 C 0.1872(2) 0.6034(2) 0.5311(6) 0.0424(11) Uani 1 1 d . . .
C13 C 0.1785(2) 0.6622(2) 0.4399(6) 0.0436(11) Uani 1 1 d . . .
H13A H 0.1443 0.6847 0.4233 0.052 Uiso 1 1 calc R . .
C14 C 0.2197(2) 0.6881(2) 0.3731(7) 0.0508(13) Uani 1 1 d . . .
H14A H 0.2120 0.7275 0.3110 0.061 Uiso 1 1 calc R . .
C15 C 0.2801(2) 0.6048(3) 0.4893(8) 0.0603(15) Uani 1 1 d . . .
H15A H 0.3157 0.5854 0.5106 0.072 Uiso 1 1 calc R . .
C16 C 0.2412(2) 0.5753(3) 0.5592(7) 0.0570(14) Uani 1 1 d . . .
H16A H 0.2507 0.5369 0.6249 0.068 Uiso 1 1 calc R . .
C17 C 0.0691(3) -0.1212(3) 0.7395(10) 0.0713(18) 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'
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
_geom_angle_publ_flag
N2 Cu1 N1 175.64(17) . . ?
N3 Cu2 N3 178.1(2) 2_556 . ?
N' Cu3 N6 138.0(3) . 7_556 ?
N' Cu3 N5 104.5(2) . . ?
N6 Cu3 N5 117.3(2) 7_556 . ?
C17 Cu4 C17 139.4(4) 2_556 . ?
C17 Cu4 N4 110.31(18) 2_556 . ?
C17 Cu4 N4 110.31(18) . . ?
C' N' N' 0.0(8) 7_565 7_565 ?
C' N' Cu3 174.3(11) 7_565 . ?
N' N' Cu3 174.3(11) 7_565 . ?
C2 N1 N1 108.9(3) . 2_556 ?
C2 N1 Cu1 132.7(3) . . ?
N1 N1 Cu1 118.19(12) 2_556 . ?
C8 N2 N3 108.3(3) . . ?
C8 N2 Cu1 130.1(3) . . ?
N3 N2 Cu1 121.6(3) . . ?
C10 N3 N2 108.1(4) . . ?
C10 N3 Cu2 133.0(3) . . ?
N2 N3 Cu2 118.7(3) . . ?
C6 N4 C6 115.4(7) . 2_556 ?
C6 N4 Cu4 122.3(3) . . ?
C6 N4 Cu4 122.3(3) 2_556 . ?
C14 N5 C15 115.9(5) . . ?
C14 N5 Cu3 119.1(4) . . ?
C15 N5 Cu3 122.1(4) . . ?
C17 N6 Cu3 172.0(6) . 7_556 ?
N1 C2 C3 108.4(4) . . ?
N1 C2 C1 120.6(4) . . ?
C3 C2 C1 130.8(4) . . ?
C2 C3 C2 105.2(6) . 2_556 ?
C2 C3 C4 127.4(3) . . ?
C2 C3 C4 127.4(3) 2_556 . ?
C5 C4 C5 116.5(7) 2_556 . ?
C5 C4 C3 121.8(3) 2_556 . ?
C5 C4 C3 121.8(3) . . ?
C4 C5 C6 119.5(6) . . ?
N4 C6 C5 124.5(6) . . ?
N2 C8 C9 109.6(4) . . ?
N2 C8 C7 119.8(4) . . ?
C9 C8 C7 130.5(4) . . ?
C8 C9 C10 104.5(4) . . ?
C8 C9 C12 127.0(4) . . ?
C10 C9 C12 128.4(4) . . ?
N3 C10 C9 109.4(4) . . ?
N3 C10 C11 120.5(4) . . ?
C9 C10 C11 130.0(4) . . ?
C13 C12 C16 115.6(5) . . ?
C13 C12 C9 122.2(4) . . ?
C16 C12 C9 122.2(4) . . ?
C14 C13 C12 120.8(5) . . ?
N5 C14 C13 123.7(5) . . ?
N5 C15 C16 124.3(5) . . ?
C15 C16 C12 119.7(5) . . ?
N6 C17 Cu4 175.6(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.852(3) . ?
Cu1 N1 1.861(3) . ?
Cu2 N3 1.859(4) 2_556 ?
Cu2 N3 1.859(4) . ?
Cu3 N' 1.871(6) . ?
Cu3 N6 1.872(7) 7_556 ?
Cu3 N5 2.066(4) . ?
Cu4 C17 1.838(6) 2_556 ?
Cu4 C17 1.838(6) . ?
Cu4 N4 2.059(6) . ?
N' C' 1.168(12) 7_565 ?
N' N' 1.168(12) 7_565 ?
N1 C2 1.343(6) . ?
N1 N1 1.360(7) 2_556 ?
N2 C8 1.338(6) . ?
N2 N3 1.383(5) . ?
N3 C10 1.339(5) . ?
N4 C6 1.297(7) . ?
N4 C6 1.297(7) 2_556 ?
N5 C14 1.330(6) . ?
N5 C15 1.337(7) . ?
N6 C17 1.154(8) . ?
N6 Cu3 1.872(7) 7_556 ?
C1 C2 1.482(7) . ?
C2 C3 1.404(6) . ?
C3 C2 1.404(6) 2_556 ?
C3 C4 1.490(9) . ?
C4 C5 1.352(6) 2_556 ?
C4 C5 1.352(6) . ?
C5 C6 1.391(8) . ?
C7 C8 1.496(6) . ?
C8 C9 1.399(6) . ?
C9 C10 1.409(6) . ?
C9 C12 1.455(6) . ?
C10 C11 1.495(6) . ?
C12 C13 1.381(7) . ?
C12 C16 1.401(7) . ?
C13 C14 1.376(7) . ?
C15 C16 1.372(8) . ?
