#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:01:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179947 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/42/7024242.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_7024242
loop_
_publ_author_name
'Yuste, Consuelo'
'Cañadillas-Delgado, Laura'
'Ruiz-Pérez, Catalina'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Dinuclear, tetranuclear and one-dimensional pyrazine-based copper(II)
 complexes: preparation, X-ray structure and magnetic properties.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              167
_journal_page_last               179
_journal_paper_doi               10.1039/b913274k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C24 H22 Cr Cu N6 O7'
_chemical_formula_weight         622.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.576(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5171(7)
_cell_length_b                   27.088(2)
_cell_length_c                   7.8068(7)
_cell_measurement_reflns_used    105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.25
_cell_measurement_theta_min      7.67
_cell_volume                     2434.6(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25322
_diffrn_reflns_theta_full        30.20
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.8977
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0453
_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)+(0.0242P)²+3.5399P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                5465
_reflns_number_total             7206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913274k.txt
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7024242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cr1 Cr 0.25574(3) 0.167570(14) -0.32626(5) 0.01026(9) Uani 1 1 d .
Cu1 Cu 0.24142(3) 0.218444(10) 0.10378(4) 0.00964(7) Uani 1 1 d .
C1 C 0.4848(2) 0.23820(9) 0.0107(3) 0.0167(5) Uani 1 1 d .
H1 H 0.4590 0.2702 -0.0111 0.020 Uiso 1 1 calc R
C2 C 0.5977(2) 0.22593(10) -0.0271(4) 0.0211(6) Uani 1 1 d .
H2 H 0.6477 0.2494 -0.0710 0.025 Uiso 1 1 calc R
C3 C 0.6350(2) 0.17801(10) 0.0017(4) 0.0197(6) Uani 1 1 d .
H3 H 0.7103 0.1687 -0.0242 0.024 Uiso 1 1 calc R
C4 C 0.5588(2) 0.14388(9) 0.0696(3) 0.0154(5) Uani 1 1 d .
H4 H 0.5823 0.1115 0.0889 0.019 Uiso 1 1 calc R
C5 C 0.4473(2) 0.15886(9) 0.1082(3) 0.0110(5) Uani 1 1 d .
C6 C 0.0581(2) 0.16543(9) 0.2572(3) 0.0114(5) Uani 1 1 d .
C7 C -0.0434(2) 0.15502(9) 0.3412(3) 0.0144(5) Uani 1 1 d .
H7 H -0.0550 0.1242 0.3906 0.017 Uiso 1 1 calc R
C8 C -0.1274(2) 0.19166(10) 0.3498(3) 0.0182(5) Uani 1 1 d .
H8 H -0.1970 0.1855 0.4036 0.022 Uiso 1 1 calc R
C9 C -0.1069(2) 0.23713(10) 0.2781(4) 0.0187(5) Uani 1 1 d .
H9 H -0.1630 0.2618 0.2806 0.022 Uiso 1 1 calc R
C10 C -0.0013(2) 0.24577(9) 0.2019(3) 0.0142(5) Uani 1 1 d .
H10 H 0.0135 0.2768 0.1564 0.017 Uiso 1 1 calc R
C11 C 0.4542(2) 0.04244(9) 0.2477(3) 0.0122(5) Uani 1 1 d .
C12 C 0.4442(2) -0.00691(9) 0.2012(3) 0.0159(5) Uani 1 1 d .
H12 H 0.3801 -0.0179 0.1368 0.019 Uiso 1 1 calc R
C13 C 0.5312(2) -0.03949(10) 0.2523(3) 0.0193(6) Uani 1 1 d .
H13 H 0.5272 -0.0726 0.2216 0.023 Uiso 1 1 calc R
C14 C 0.6235(2) -0.02178(10) 0.3494(3) 0.0198(6) Uani 1 1 d .
H14 H 0.6814 -0.0430 0.3900 0.024 Uiso 1 1 calc R
C15 C 0.6289(2) 0.02821(10) 0.3859(3) 0.0190(5) Uani 1 1 d .
H15 H 0.6931 0.0400 0.4481 0.023 Uiso 1 1 calc R
C16 C -0.1299(2) 0.03316(11) 0.0919(4) 0.0223(6) Uani 1 1 d .
H16 H -0.1907 0.0440 0.0206 0.027 Uiso 1 1 calc R
C17 C -0.1367(3) -0.01364(11) 0.1608(4) 0.0244(6) Uani 1 1 d .
H17 H -0.2002 -0.0338 0.1346 0.029 Uiso 1 1 calc R
C18 C -0.0488(3) -0.03017(10) 0.2682(4) 0.0231(6) Uani 1 1 d .
H18 H -0.0524 -0.0613 0.3182 0.028 Uiso 1 1 calc R
C19 C 0.0455(2) 0.00045(9) 0.3006(3) 0.0172(5) Uani 1 1 d .
H19 H 0.1070 -0.0098 0.3718 0.021 Uiso 1 1 calc R
C20 C 0.0464(2) 0.04649(9) 0.2248(3) 0.0125(5) Uani 1 1 d .
C21 C 0.3545(2) 0.12682(9) 0.1782(3) 0.0103(4) Uani 1 1 d .
C22 C 0.3538(2) 0.07608(9) 0.2181(3) 0.0107(4) Uani 1 1 d .
C23 C 0.1519(2) 0.07786(9) 0.2360(3) 0.0114(5) Uani 1 1 d .
C24 C 0.1538(2) 0.12974(9) 0.2320(3) 0.0102(4) Uani 1 1 d .
N1 N 0.41168(18) 0.20578(7) 0.0774(3) 0.0117(4) Uani 1 1 d .
N2 N 0.07972(17) 0.21058(7) 0.1924(2) 0.0105(4) Uani 1 1 d .
N3 N 0.54630(18) 0.06050(8) 0.3360(3) 0.0146(4) Uani 1 1 d .
N4 N -0.04050(19) 0.06363(8) 0.1223(3) 0.0160(4) Uani 1 1 d .
N5 N 0.25376(17) 0.15115(7) 0.1928(2) 0.0091(4) Uani 1 1 d .
N6 N 0.25156(18) 0.05317(7) 0.2361(3) 0.0116(4) Uani 1 1 d .
O1 O 0.18718(15) 0.18024(7) -0.1472(2) 0.0153(4) Uani 1 1 d .
O2 O 0.20278(17) 0.11797(6) -0.4136(2) 0.0176(4) Uani 1 1 d .
O1W O -0.0478(2) 0.14507(8) -0.1192(3) 0.0241(5) Uani 1 1 d .
O3 O 0.39420(16) 0.16066(7) -0.2841(2) 0.0205(4) Uani 1 1 d .
O2W O 0.59736(19) 0.14988(8) -0.4708(3) 0.0239(5) Uani 1 1 d .
O4 O 0.23515(15) 0.21487(6) -0.4681(2) 0.0137(3) Uani 1 1 d .
O3W O 0.2086(3) -0.09737(10) 0.3362(5) 0.0564(9) Uani 1 1 d .
H1WA H -0.040(3) 0.1225(15) -0.045(5) 0.045(12) Uiso 1 1 d .
H2WA H 0.581(3) 0.1279(15) -0.529(5) 0.040(12) Uiso 1 1 d .
H2WB H 0.541(4) 0.1523(15) -0.418(5) 0.048(13) Uiso 1 1 d .
H1WB H 0.013(3) 0.1531(15) -0.136(5) 0.040(12) Uiso 1 1 d .
H3WA H 0.261(4) -0.1150(16) 0.358(5) 0.052(13) Uiso 1 1 d .
H3WB H 0.167(4) -0.1131(17) 0.286(6) 0.060(15) Uiso 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'
Cr Cr 0.3209 0.6236 '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'
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'
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
O2 Cr1 O3 110.19(10) . .
O2 Cr1 O1 110.11(9) . .
O3 Cr1 O1 109.80(9) . .
O2 Cr1 O4 107.83(9) . .
O3 Cr1 O4 109.59(9) . .
O1 Cr1 O4 109.29(9) . .
O4 Cu1 N5 175.93(8) 4_566 .
O4 Cu1 N1 99.34(8) 4_566 .
N5 Cu1 N1 79.36(8) . .
O4 Cu1 N2 100.05(8) 4_566 .
N5 Cu1 N2 80.69(8) . .
N1 Cu1 N2 158.71(8) . .
O4 Cu1 O1 99.83(7) 4_566 .
N5 Cu1 O1 84.15(7) . .
N1 Cu1 O1 94.54(7) . .
N2 Cu1 O1 90.75(7) . .
N1 C1 C2 122.3(2) . .
C1 C2 C3 118.7(2) . .
C2 C3 C4 119.3(2) . .
C5 C4 C3 119.1(2) . .
N1 C5 C4 120.8(2) . .
N1 C5 C21 113.3(2) . .
C4 C5 C21 125.9(2) . .
N2 C6 C7 121.9(2) . .
N2 C6 C24 113.3(2) . .
C7 C6 C24 124.7(2) . .
C6 C7 C8 118.4(2) . .
C9 C8 C7 119.5(2) . .
C8 C9 C10 119.2(2) . .
N2 C10 C9 121.6(2) . .
N3 C11 C12 123.0(2) . .
N3 C11 C22 117.2(2) . .
C12 C11 C22 119.4(2) . .
C13 C12 C11 118.9(2) . .
C14 C13 C12 118.6(2) . .
C13 C14 C15 119.0(2) . .
N3 C15 C14 123.4(3) . .
N4 C16 C17 123.4(3) . .
C18 C17 C16 119.3(3) . .
C17 C18 C19 118.6(3) . .
C20 C19 C18 118.6(3) . .
N4 C20 C19 123.5(2) . .
N4 C20 C23 115.6(2) . .
C19 C20 C23 120.5(2) . .
N5 C21 C22 116.7(2) . .
N5 C21 C5 112.0(2) . .
C22 C21 C5 131.1(2) . .
N6 C22 C21 119.0(2) . .
N6 C22 C11 112.4(2) . .
C21 C22 C11 128.5(2) . .
N6 C23 C24 119.3(2) . .
N6 C23 C20 114.7(2) . .
C24 C23 C20 125.8(2) . .
N5 C24 C23 117.0(2) . .
N5 C24 C6 113.4(2) . .
C23 C24 C6 129.5(2) . .
C1 N1 C5 119.7(2) . .
C1 N1 Cu1 123.88(17) . .
C5 N1 Cu1 115.71(16) . .
C10 N2 C6 119.3(2) . .
C10 N2 Cu1 126.59(17) . .
C6 N2 Cu1 113.95(16) . .
C11 N3 C15 117.1(2) . .
C16 N4 C20 116.7(2) . .
C24 N5 C21 124.1(2) . .
C24 N5 Cu1 115.66(16) . .
C21 N5 Cu1 118.84(16) . .
C23 N6 C22 121.8(2) . .
Cr1 O1 Cu1 133.61(10) . .
Cr1 O4 Cu1 121.41(10) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O2 1.6183(18) .
Cr1 O3 1.6302(19) .
Cr1 O1 1.6604(17) .
Cr1 O4 1.7056(17) .
Cu1 O4 1.8923(17) 4_566
Cu1 N5 1.9546(19) .
Cu1 N1 2.007(2) .
Cu1 N2 2.016(2) .
Cu1 O1 2.2873(17) .
C1 N1 1.333(3) .
C1 C2 1.382(4) .
C2 C3 1.384(4) .
C3 C4 1.390(4) .
C4 C5 1.388(3) .
C5 N1 1.355(3) .
C5 C21 1.491(3) .
C6 N2 1.349(3) .
C6 C7 1.385(3) .
C6 C24 1.483(3) .
C7 C8 1.389(3) .
C8 C9 1.376(4) .
C9 C10 1.388(4) .
C10 N2 1.337(3) .
C11 N3 1.341(3) .
C11 C12 1.389(3) .
C11 C22 1.486(3) .
C12 C13 1.386(4) .
C13 C14 1.375(4) .
C14 C15 1.385(4) .
C15 N3 1.342(3) .
C16 N4 1.336(3) .
C16 C17 1.380(4) .
C17 C18 1.373(4) .
C18 C19 1.384(4) .
C19 C20 1.380(3) .
C20 N4 1.347(3) .
C20 C23 1.484(3) .
C21 N5 1.342(3) .
C21 C22 1.409(3) .
C22 N6 1.341(3) .
C23 N6 1.328(3) .
C23 C24 1.406(3) .
C24 N5 1.332(3) .
O4 Cu1 1.8923(17) 4_565
