#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179861 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/57/7015707.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_7015707
loop_
_publ_author_name
'Türkoglu, Gazi'
'Heinemann, Frank W.'
'Burzlaff, Nicolai'
_publ_section_title
;
 Transition metal complexes bearing a
 2,2-bis(3,5-dimethylpyrazol-1-yl)propionate ligand: one methyl more
 matters.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4678
_journal_page_last               4686
_journal_paper_doi               10.1039/c1dt00022e
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H34 Cu N8 O4'
_chemical_formula_sum            'C26 H34 Cu N8 O4'
_chemical_formula_weight         586.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2010-11-10T14:42:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.446(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8389(10)
_cell_length_b                   9.665(2)
_cell_length_c                   15.970(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.942
_cell_measurement_theta_min      9.902
_cell_measurement_wavelength     0.71073
_cell_volume                     1360.2(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.110932
_diffrn_orient_matrix_UB_12      0.003089
_diffrn_orient_matrix_UB_13      0.008266
_diffrn_orient_matrix_UB_21      0.023907
_diffrn_orient_matrix_UB_22      0.014704
_diffrn_orient_matrix_UB_23      0.06156
_diffrn_orient_matrix_UB_31      -0.000082
_diffrn_orient_matrix_UB_32      0.102399
_diffrn_orient_matrix_UB_33      -0.009112
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.067
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2757
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0777P)²+0.3731P] where
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                1824
_reflns_number_total             2657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt00022e.txt
_cod_data_source_block           gtbu12
_cod_original_cell_volume        1360.1(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7015707
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5276(4) 0.2746(4) 0.0531(2) 0.0328(8) Uani 1 1 d . . .
C2 C 0.6947(4) 0.2695(4) 0.0221(2) 0.0331(8) Uani 1 1 d . . .
C3 C 0.7623(5) 0.4139(4) 0.0357(3) 0.0469(10) Uani 1 1 d . . .
H3A H 0.7018 0.4798 0.0029 0.07 Uiso 1 1 calc R . .
H3B H 0.8641 0.4148 0.0186 0.07 Uiso 1 1 calc R . .
H3C H 0.7636 0.4378 0.094 0.07 Uiso 1 1 calc R . .
C11 C 0.5979(5) -0.0556(5) -0.2110(3) 0.0490(10) Uani 1 1 d . . .
H11A H 0.6649 -0.1288 -0.1913 0.073 Uiso 1 1 calc R . .
H11B H 0.6039 -0.0437 -0.2704 0.073 Uiso 1 1 calc R . .
H11C H 0.4957 -0.0788 -0.2001 0.073 Uiso 1 1 calc R . .
C12 C 0.6429(4) 0.0746(4) -0.1669(2) 0.0366(9) Uani 1 1 d . . .
C13 C 0.7037(4) 0.1917(4) -0.2018(2) 0.0408(9) Uani 1 1 d . . .
H13 H 0.722 0.2036 -0.258 0.049 Uiso 1 1 calc R . .
C14 C 0.7320(4) 0.2860(4) -0.1390(2) 0.0362(8) Uani 1 1 d . . .
C15 C 0.7989(6) 0.4271(4) -0.1486(3) 0.0545(11) Uani 1 1 d . . .
H15A H 0.8174 0.442 -0.2064 0.082 Uiso 1 1 calc R . .
H15B H 0.8928 0.4338 -0.1144 0.082 Uiso 1 1 calc R . .
H15C H 0.7294 0.4959 -0.1313 0.082 Uiso 1 1 calc R . .
C21 C 0.7639(5) -0.1715(4) 0.1666(3) 0.0563(12) Uani 1 1 d . . .
H21A H 0.6978 -0.1543 0.2104 0.085 Uiso 1 1 calc R . .
H21B H 0.853 -0.2193 0.1895 0.085 Uiso 1 1 calc R . .
H21C H 0.7121 -0.2274 0.1238 0.085 Uiso 1 1 calc R . .
C22 C 0.8091(4) -0.0364(4) 0.1294(2) 0.0400(9) Uani 1 1 d . . .
C23 C 0.9535(4) 0.0156(4) 0.1196(3) 0.0470(10) Uani 1 1 d . . .
H23 H 1.045 -0.0271 0.1367 0.056 Uiso 1 1 calc R . .
C24 C 0.9363(4) 0.1404(4) 0.0803(3) 0.0424(9) Uani 1 1 d . . .
C25 C 1.0573(5) 0.2319(5) 0.0513(4) 0.0678(15) Uani 1 1 d . . .
H25A H 1.1544 0.1888 0.0632 0.102 Uiso 1 1 calc R . .
H25B H 1.0555 0.319 0.0801 0.102 Uiso 1 1 calc R . .
H25C H 1.04 0.2469 -0.0081 0.102 Uiso 1 1 calc R . .
Cu1 Cu 0.5 0 0 0.0322(2) Uani 1 2 d S . .
N11 N 0.6326(3) 0.0939(3) -0.08503(19) 0.0338(7) Uani 1 1 d . . .
N12 N 0.6862(3) 0.2261(3) -0.06768(18) 0.0331(7) Uani 1 1 d . . .
N21 N 0.7047(3) 0.0532(3) 0.09976(19) 0.0362(7) Uani 1 1 d . . .
N22 N 0.7830(3) 0.1639(3) 0.07092(18) 0.0325(7) Uani 1 1 d . . .
O1 O 0.4314(3) 0.1849(3) 0.02429(16) 0.0391(6) Uani 1 1 d . . .
O2 O 0.5020(3) 0.3681(3) 0.1009(2) 0.0570(8) 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 0 -2
1 2 -4
-2 1 -2
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
O2 C1 O1 125.5(4) . . ?
O2 C1 C2 116.2(3) . . ?
O1 C1 C2 118.3(3) . . ?
N22 C2 N12 107.5(3) . . ?
N22 C2 C3 111.9(3) . . ?
N12 C2 C3 112.6(3) . . ?
N22 C2 C1 108.8(3) . . ?
N12 C2 C1 109.3(3) . . ?
C3 C2 C1 106.8(3) . . ?
N11 C12 C13 109.8(3) . . ?
N11 C12 C11 123.4(3) . . ?
C13 C12 C11 126.9(3) . . ?
C14 C13 C12 107.7(3) . . ?
C13 C14 N12 106.3(3) . . ?
C13 C14 C15 125.7(4) . . ?
N12 C14 C15 128.0(4) . . ?
N21 C22 C23 110.1(3) . . ?
N21 C22 C21 120.7(4) . . ?
C23 C22 C21 129.2(4) . . ?
C24 C23 C22 107.5(3) . . ?
C23 C24 N22 105.7(3) . . ?
C23 C24 C25 127.7(4) . . ?
N22 C24 C25 126.5(4) . . ?
O1 Cu1 O1 180.00(19) . 3_655 ?
O1 Cu1 N11 85.90(11) . . ?
O1 Cu1 N11 94.10(11) 3_655 . ?
O1 Cu1 N11 94.10(11) . 3_655 ?
O1 Cu1 N11 85.90(11) 3_655 3_655 ?
N11 Cu1 N11 180.0(2) . 3_655 ?
O1 Cu1 N21 84.24(11) . . ?
O1 Cu1 N21 95.76(11) 3_655 . ?
N11 Cu1 N21 84.52(11) . . ?
N11 Cu1 N21 95.48(11) 3_655 . ?
O1 Cu1 N21 95.76(11) . 3_655 ?
O1 Cu1 N21 84.24(11) 3_655 3_655 ?
N11 Cu1 N21 95.48(11) . 3_655 ?
N11 Cu1 N21 84.52(11) 3_655 3_655 ?
N21 Cu1 N21 180.00(12) . 3_655 ?
C12 N11 N12 106.2(3) . . ?
C12 N11 Cu1 131.9(2) . . ?
N12 N11 Cu1 118.4(2) . . ?
C14 N12 N11 110.1(3) . . ?
C14 N12 C2 133.4(3) . . ?
N11 N12 C2 116.3(3) . . ?
C22 N21 N22 105.9(3) . . ?
C22 N21 Cu1 124.9(3) . . ?
N22 N21 Cu1 108.8(2) . . ?
C24 N22 N21 110.7(3) . . ?
C24 N22 C2 130.7(3) . . ?
N21 N22 C2 117.2(3) . . ?
C1 O1 Cu1 119.3(2) . . ?
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
C1 O2 1.216(4) . ?
C1 O1 1.275(4) . ?
C1 C2 1.594(5) . ?
C2 N22 1.471(5) . ?
C2 N12 1.489(4) . ?
C2 C3 1.527(5) . ?
C11 C12 1.481(5) . ?
C12 N11 1.332(5) . ?
C12 C13 1.388(5) . ?
C13 C14 1.365(5) . ?
C14 N12 1.367(4) . ?
C14 C15 1.499(5) . ?
C21 C22 1.503(5) . ?
C22 N21 1.326(5) . ?
C22 C23 1.391(6) . ?
C23 C24 1.362(6) . ?
C24 N22 1.371(5) . ?
C24 C25 1.489(6) . ?
Cu1 O1 1.936(2) . ?
Cu1 O1 1.936(2) 3_655 ?
Cu1 N11 2.071(3) . ?
Cu1 N11 2.071(3) 3_655 ?
Cu1 N21 2.372(3) . ?
Cu1 N21 2.372(3) 3_655 ?
N11 N12 1.383(4) . ?
N21 N22 1.373(4) . ?
