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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/28/1512899.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_1512899
loop_
_publ_author_name
'Mark B. Bushuev'
'Yuri V. Gatilov'
'Elena B. Nikolaenkova'
'Vladimir G. Vasiliev'
'Viktor P. Krivopalov'
_publ_section_title
;
 Mono-, di-, tetra- and heptanuclear copper(II) complexes with
 4-(3,5-di-R-1H-pyrazol-1-yl)-6-methyl-2-(pyridin-2-yl)pyrimidines (R = H,
 Me): Syntheses, crystal structures and electrospray ionization mass
 spectrometry
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              95
_journal_page_last               103
_journal_paper_doi               10.1016/j.ica.2012.10.018
_journal_volume                  395
_journal_year                    2013
_chemical_formula_moiety         'C30 H30 Cl8 Cu4 N10'
_chemical_formula_sum            'C30 H30 Cl8 Cu4 N10'
_chemical_formula_weight         1068.40
_chemical_name_systematic
; 
 octachloridobis(4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-(pyridin-2-yl)-6-
methylpyrimidine)tetracopper 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.518(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1333(6)
_cell_length_b                   11.6425(6)
_cell_length_c                   17.1806(6)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.19
_cell_volume                     3720.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38430
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.871
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0303
_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)+(0.0280P)²+5.8522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                4214
_reflns_number_total             5432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-95-103-6.cif
_cod_data_source_block           6_k148
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               1512899
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 0.159411(16) 0.18669(2) 0.494350(15) 0.02704(8) Uani 1 1 d .
Cl1 Cl 0.02845(3) 0.19081(5) 0.50437(4) 0.03468(13) Uani 1 1 d .
C1 C 0.17578(11) -0.05300(17) 0.52985(13) 0.0240(4) Uani 1 1 d .
N1 N 0.17310(11) -0.16585(15) 0.51989(12) 0.0288(4) Uani 1 1 d .
Cu2 Cu 0.033489(16) 0.37219(2) 0.550770(17) 0.03021(8) Uani 1 1 d .
Cl2 Cl 0.18967(4) 0.36853(5) 0.52838(4) 0.04037(16) Uani 1 1 d .
N2 N 0.15271(10) 0.02402(14) 0.46772(11) 0.0241(4) Uani 1 1 d .
C2 C 0.12769(11) -0.01203(17) 0.38806(13) 0.0239(4) Uani 1 1 d .
Cl3 Cl 0.04932(4) 0.56565(5) 0.57784(4) 0.04573(18) Uani 1 1 d .
N3 N 0.20556(10) 0.11777(15) 0.61231(11) 0.0258(4) Uani 1 1 d .
C3 C 0.12280(12) -0.12863(18) 0.37068(14) 0.0281(5) Uani 1 1 d .
H3 H 0.1055 -0.1560 0.3156 0.034 Uiso 1 1 calc R
Cl4 Cl 0.07832(4) 0.32679(6) 0.68661(4) 0.04729(18) Uani 1 1 d .
N4 N 0.10896(10) 0.07985(15) 0.33131(11) 0.0256(4) Uani 1 1 d .
C4 C 0.14492(12) -0.20308(18) 0.43940(14) 0.0279(4) Uani 1 1 d .
N5 N 0.11783(10) 0.18909(14) 0.36651(11) 0.0254(4) Uani 1 1 d .
C5 C 0.13825(15) -0.32998(19) 0.42547(17) 0.0380(6) Uani 1 1 d .
H5A H 0.1555 -0.3687 0.4789 0.057 Uiso 1 1 calc R
H5B H 0.1663 -0.3532 0.3938 0.057 Uiso 1 1 calc R
H5C H 0.0887 -0.3495 0.3947 0.057 Uiso 1 1 calc R
C6 C 0.20741(12) 0.00136(18) 0.61416(13) 0.0249(4) Uani 1 1 d .
C7 C 0.23746(14) -0.0593(2) 0.68813(14) 0.0349(5) Uani 1 1 d .
H7 H 0.2383 -0.1392 0.6876 0.042 Uiso 1 1 calc R
C8 C 0.26639(15) 0.0003(2) 0.76350(14) 0.0384(6) Uani 1 1 d .
H8 H 0.2873 -0.0390 0.8142 0.046 Uiso 1 1 calc R
C9 C 0.26376(15) 0.1180(2) 0.76218(14) 0.0370(6) Uani 1 1 d .
H9 H 0.2823 0.1596 0.8121 0.044 Uiso 1 1 calc R
C10 C 0.23308(13) 0.17424(19) 0.68530(14) 0.0314(5) Uani 1 1 d .
H10 H 0.2317 0.2541 0.6847 0.038 Uiso 1 1 calc R
C11 C 0.09675(12) 0.26151(18) 0.30237(13) 0.0259(4) Uani 1 1 d .
C12 C 0.07466(13) 0.19995(19) 0.22554(13) 0.0293(5) Uani 1 1 d .
H12 H 0.0580 0.2316 0.1718 0.035 Uiso 1 1 calc R
C13 C 0.08218(12) 0.08627(19) 0.24464(13) 0.0261(4) Uani 1 1 d .
C14 C 0.09546(14) 0.38784(19) 0.31500(15) 0.0340(5) Uani 1 1 d .
H14C H 0.0587 0.4062 0.3358 0.073(11) Uiso 1 1 calc R
H14B H 0.0855 0.4264 0.2623 0.088 Uiso 1 1 calc R
H14A H 0.1413 0.4124 0.3551 0.088 Uiso 1 1 calc R
C15 C 0.06457(14) -0.0143(2) 0.18700(14) 0.0343(5) Uani 1 1 d .
H15C H 0.0214 -0.0501 0.1864 0.058(9) Uiso 1 1 calc R
H15B H 0.1034 -0.0685 0.2062 0.069 Uiso 1 1 calc R
H15A H 0.0574 0.0107 0.1311 0.069 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_3
N2 Cu1 N5 78.21(7) .
N2 Cu1 N3 79.32(7) .
N5 Cu1 N3 157.18(7) .
N2 Cu1 Cl2 168.68(6) .
N5 Cu1 Cl2 103.29(5) .
N3 Cu1 Cl2 97.97(5) .
N2 Cu1 Cl1 92.91(6) .
N5 Cu1 Cl1 93.47(6) .
N3 Cu1 Cl1 91.60(6) .
Cl2 Cu1 Cl1 98.17(2) .
Cu2 Cl1 Cu1 97.27(2) .
N1 C1 N2 125.41(19) .
N1 C1 C6 122.09(18) .
N2 C1 C6 112.49(18) .
C1 N1 C4 115.58(18) .
Cl4 Cu2 Cl1 95.40(2) .
Cl4 Cu2 Cl3 92.96(2) .
Cl1 Cu2 Cl3 167.88(3) .
Cl4 Cu2 Cl3 158.71(3) 5_566
Cl1 Cu2 Cl3 92.12(2) 5_566
Cl3 Cu2 Cl3 83.12(2) 5_566
C2 N2 C1 119.28(18) .
C2 N2 Cu1 120.96(14) .
C1 N2 Cu1 119.72(14) .
N2 C2 C3 119.86(19) .
N2 C2 N4 111.73(17) .
C3 C2 N4 128.41(19) .
Cu2 Cl3 Cu2 96.88(2) 5_566
C10 N3 C6 118.21(18) .
C10 N3 Cu1 127.33(15) .
C6 N3 Cu1 114.45(14) .
C2 C3 C4 117.0(2) .
C2 C3 H3 121.5 .
C4 C3 H3 121.5 .
C13 N4 N5 110.64(17) .
C13 N4 C2 133.19(18) .
N5 N4 C2 116.17(16) .
N1 C4 C3 122.76(19) .
N1 C4 C5 117.3(2) .
C3 C4 C5 120.0(2) .
C11 N5 N4 105.91(16) .
C11 N5 Cu1 141.16(15) .
N4 N5 Cu1 112.91(12) .
C4 C5 H5A 109.5 .
C4 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C4 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
N3 C6 C7 122.2(2) .
N3 C6 C1 113.97(17) .
C7 C6 C1 123.78(19) .
C6 C7 C8 119.0(2) .
C6 C7 H7 120.5 .
C8 C7 H7 120.5 .
C9 C8 C7 119.0(2) .
C9 C8 H8 120.5 .
C7 C8 H8 120.5 .
C8 C9 C10 119.1(2) .
C8 C9 H9 120.4 .
C10 C9 H9 120.4 .
N3 C10 C9 122.3(2) .
N3 C10 H10 118.8 .
C9 C10 H10 118.8 .
N5 C11 C12 109.90(19) .
N5 C11 C14 121.78(19) .
C12 C11 C14 128.28(19) .
C13 C12 C11 107.58(18) .
C13 C12 H12 126.2 .
C11 C12 H12 126.2 .
C12 C13 N4 105.98(18) .
C12 C13 C15 129.1(2) .
N4 C13 C15 124.9(2) .
C11 C14 H14C 109.5 .
C11 C14 H14B 109.5 .
H14C C14 H14B 109.5 .
C11 C14 H14A 109.5 .
H14C C14 H14A 109.5 .
H14B C14 H14A 109.5 .
C13 C15 H15C 109.5 .
C13 C15 H15B 109.5 .
H15C C15 H15B 109.5 .
C13 C15 H15A 109.5 .
H15C C15 H15A 109.5 .
H15B C15 H15A 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.9409(17) .
Cu1 N5 2.0290(17) .
Cu1 N3 2.0426(17) .
Cu1 Cl2 2.2186(6) .
Cu1 Cl1 2.7078(7) .
Cl1 Cu2 2.2457(6) .
C1 N1 1.323(3) .
C1 N2 1.334(3) .
C1 C6 1.483(3) .
N1 C4 1.349(3) .
Cu2 Cl4 2.2198(6) .
Cu2 Cl3 2.2973(6) .
Cu2 Cl3 2.3160(6) 5_566
N2 C2 1.332(3) .
C2 C3 1.385(3) .
C2 N4 1.398(3) .
Cl3 Cu2 2.3160(6) 5_566
N3 C10 1.334(3) .
N3 C6 1.356(3) .
C3 C4 1.393(3) .
C3 H3 0.9300 .
N4 C13 1.378(3) .
N4 N5 1.390(2) .
C4 C5 1.495(3) .
N5 C11 1.322(3) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.375(3) .
C7 C8 1.385(3) .
C7 H7 0.9300 .
C8 C9 1.371(3) .
C8 H8 0.9300 .
C9 C10 1.389(3) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.416(3) .
C11 C14 1.488(3) .
C12 C13 1.358(3) .
C12 H12 0.9300 .
C13 C15 1.486(3) .
C14 H14C 0.9600 .
C14 H14B 0.9600 .
C14 H14A 0.9600 .
C15 H15C 0.9600 .
C15 H15B 0.9600 .
C15 H15A 0.9600 .
