#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:54:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179430 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/27/4332720.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332720
loop_
_publ_author_name
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Investigations on the Synthesis, Structures, and Properties of New
 Copper(I) 2,3-Dimethylpyrazine Coordination Compounds
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7446
_journal_page_last               7454
_journal_paper_doi               10.1021/ic060747b
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C6 H8 Cl2 Cu2 N2'
_chemical_formula_weight         306.12
_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                 100.388(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.303(2)
_cell_length_b                   3.9135(2)
_cell_length_c                   15.1940(12)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      10
_cell_volume                     1772.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8128
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    5.339
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0363
_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)+(0.0445P)²+7.5082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                1722
_reflns_number_total             2068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060747bsup4.cif
_cod_data_source_block           d9
_cod_original_cell_volume        1772.4(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4332720
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 0.708899(17) 0.64194(15) 0.25557(3) 0.04468(17) Uani 1 1 d .
Cl1 Cl 0.78848(3) 0.6482(2) 0.33279(5) 0.02894(18) Uani 1 1 d .
Cu2 Cu 0.520436(16) 0.70714(15) 0.44095(4) 0.04776(17) Uani 1 1 d .
Cl2 Cl 0.47784(3) 0.2079(2) 0.39499(5) 0.03148(19) Uani 1 1 d .
N1 N 0.65540(9) 0.6536(8) 0.31696(18) 0.0278(6) Uani 1 1 d .
C1 C 0.65517(9) 0.5190(8) 0.39841(19) 0.0230(6) Uani 1 1 d .
C2 C 0.61626(9) 0.5318(8) 0.43688(19) 0.0221(6) Uani 1 1 d .
N2 N 0.57833(9) 0.6793(8) 0.39335(18) 0.0274(6) Uani 1 1 d .
C3 C 0.57904(12) 0.8068(10) 0.3114(2) 0.0354(8) Uani 1 1 d .
H3 H 0.5531 0.9055 0.2794 0.042 Uiso 1 1 calc R
C4 C 0.61692(12) 0.7958(10) 0.2736(2) 0.0333(7) Uani 1 1 d .
H4 H 0.6161 0.8881 0.2169 0.040 Uiso 1 1 calc R
C5 C 0.69805(11) 0.3652(10) 0.4466(2) 0.0326(7) Uani 1 1 d .
H5A H 0.6914 0.1869 0.4856 0.049 Uiso 0.62 1 calc PR
H5B H 0.7157 0.5384 0.4812 0.049 Uiso 0.62 1 calc PR
H5C H 0.7145 0.2718 0.4038 0.049 Uiso 0.62 1 calc PR
H5D H 0.7230 0.4778 0.4281 0.049 Uiso 0.38 1 calc PR
H5E H 0.6987 0.1263 0.4325 0.049 Uiso 0.38 1 calc PR
H5F H 0.6999 0.3930 0.5099 0.049 Uiso 0.38 1 calc PR
C6 C 0.61536(11) 0.3882(10) 0.5281(2) 0.0318(7) Uani 1 1 d .
H6A H 0.6396 0.2291 0.5440 0.048 Uiso 0.62 1 calc PR
H6B H 0.5873 0.2732 0.5278 0.048 Uiso 0.62 1 calc PR
H6C H 0.6185 0.5706 0.5711 0.048 Uiso 0.62 1 calc PR
H6D H 0.5907 0.4861 0.5512 0.048 Uiso 0.38 1 calc PR
H6E H 0.6430 0.4421 0.5674 0.048 Uiso 0.38 1 calc PR
H6F H 0.6118 0.1447 0.5241 0.048 Uiso 0.38 1 calc PR
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
N1 Cu1 Cl1 113.24(9) . 4_645
N1 Cu1 Cl1 110.55(9) . 4_655
Cl1 Cu1 Cl1 110.42(4) 4_645 4_655
N1 Cu1 Cl1 125.15(8) . .
Cl1 Cu1 Cl1 98.46(3) 4_645 .
Cl1 Cu1 Cl1 97.39(3) 4_655 .
Cu1 Cl1 Cu1 110.42(4) 4_655 4_645
Cu1 Cl1 Cu1 82.47(3) 4_655 .
Cu1 Cl1 Cu1 81.67(3) 4_645 .
N2 Cu2 Cl2 108.16(9) . .
N2 Cu2 Cl2 113.56(9) . 1_565
Cl2 Cu2 Cl2 110.71(4) . 1_565
N2 Cu2 Cl2 120.02(8) . 5_666
Cl2 Cu2 Cl2 108.31(3) . 5_666
Cl2 Cu2 Cl2 95.48(3) 1_565 5_666
N2 Cu2 Cu2 134.19(9) . 5_666
Cl2 Cu2 Cu2 56.27(3) . 5_666
Cl2 Cu2 Cu2 112.17(3) 1_565 5_666
Cl2 Cu2 Cu2 52.04(3) 5_666 5_666
Cu2 Cl2 Cu2 110.71(4) . 1_545
Cu2 Cl2 Cu2 71.69(3) . 5_666
Cu2 Cl2 Cu2 84.52(3) 1_545 5_666
C1 N1 C4 117.6(3) . .
C1 N1 Cu1 123.7(2) . .
C4 N1 Cu1 118.7(2) . .
N1 C1 C2 120.7(3) . .
N1 C1 C5 117.3(3) . .
C2 C1 C5 121.9(3) . .
N2 C2 C1 121.0(3) . .
N2 C2 C6 117.2(3) . .
C1 C2 C6 121.8(3) . .
C3 N2 C2 117.3(3) . .
C3 N2 Cu2 118.2(2) . .
C2 N2 Cu2 124.5(2) . .
N2 C3 C4 122.0(3) . .
N1 C4 C3 121.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.011(3) .
Cu1 Cl1 2.3625(10) 4_645
Cu1 Cl1 2.4027(10) 4_655
Cu1 Cl1 2.4844(10) .
Cl1 Cu1 2.3625(10) 4_655
Cl1 Cu1 2.4027(10) 4_645
Cu2 N2 2.017(3) .
Cu2 Cl2 2.3760(10) .
Cu2 Cl2 2.3810(10) 1_565
Cu2 Cl2 2.5060(10) 5_666
Cu2 Cu2 2.8608(11) 5_666
Cl2 Cu2 2.3810(10) 1_545
Cl2 Cu2 2.5060(10) 5_666
N1 C1 1.346(4) .
N1 C4 1.351(4) .
C1 C2 1.408(4) .
C1 C5 1.498(4) .
C2 N2 1.348(4) .
C2 C6 1.501(4) .
N2 C3 1.345(5) .
C3 C4 1.374(5) .
