#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:06:29 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229979.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_7229979
loop_
_publ_author_name
'Dankhoff, Katja'
'Weber, Birgit'
_publ_section_title
;
 Novel Cu(ii) complexes with NNO-Schiff base-like ligands -- structures
 and magnetic properties
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              818
_journal_paper_doi               10.1039/C7CE02007D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C32 H40 Cu2 N4 O12, 2(H2 O)'
_chemical_formula_sum            'C32 H44 Cu2 N4 O14'
_chemical_formula_weight         835.78
_chemical_name_common            '[CuL30cOAc]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-27
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-11 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                94.241(5)
_cell_angle_beta                 104.942(5)
_cell_angle_gamma                108.277(5)
_cell_formula_units_Z            1
_cell_length_a                   8.8660(6)
_cell_length_b                   8.8511(6)
_cell_length_c                   12.7620(8)
_cell_measurement_reflns_used    9512
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      1.68
_cell_volume                     905.63(11)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       omega-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10553
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.601
_diffrn_reflns_theta_min         1.676
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0612P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                3604
_reflns_number_total             4267
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce02007d2.cif
_cod_data_source_block           cl123
_cod_depositor_comments
'Adding full bibliography for 7229962--7229987.cif.'
_cod_database_code               7229979
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.5640(3) 0.2467(3) 0.32765(18) 0.0188(4) Uani 1 1 d . .
H1 H 0.6403 0.3544 0.3461 0.023 Uiso 1 1 calc R U
C2 C 0.5538(3) 0.1500(3) 0.23402(19) 0.0215(5) Uani 1 1 d . .
H2 H 0.6216 0.1902 0.1885 0.026 Uiso 1 1 calc R U
C3 C 0.4421(3) -0.0072(3) 0.20825(19) 0.0213(5) Uani 1 1 d . .
H3 H 0.4332 -0.0764 0.1447 0.026 Uiso 1 1 calc R U
C4 C 0.3436(3) -0.0630(3) 0.27527(18) 0.0188(4) Uani 1 1 d . .
H4 H 0.2664 -0.1702 0.2583 0.023 Uiso 1 1 calc R U
C5 C 0.3601(3) 0.0412(3) 0.36804(17) 0.0150(4) Uani 1 1 d . .
C6 C 0.2551(3) -0.0096(3) 0.44354(18) 0.0176(4) Uani 1 1 d . .
H6A H 0.1371 -0.0292 0.4041 0.021 Uiso 1 1 calc R U
H6B H 0.2639 -0.1112 0.4675 0.021 Uiso 1 1 calc R U
C7 C 0.2411(3) 0.0879(3) 0.61675(17) 0.0145(4) Uani 1 1 d . .
H7 H 0.1552 -0.0139 0.6042 0.017 Uiso 1 1 calc R U
C8 C 0.2770(3) 0.1897(3) 0.71691(17) 0.0164(4) Uani 1 1 d . .
C9 C 0.4175(3) 0.3360(3) 0.74861(17) 0.0160(4) Uani 1 1 d . .
C10 C 0.6209(3) 0.5407(3) 0.89372(18) 0.0208(5) Uani 1 1 d . .
H10A H 0.6225 0.6057 0.9609 0.025 Uiso 1 1 calc R U
H10B H 0.6321 0.6113 0.8374 0.025 Uiso 1 1 calc R U
C11 C 0.7641(4) 0.4795(3) 0.9196(2) 0.0338(6) Uani 1 1 d . .
H11A H 0.7434 0.3957 0.9654 0.051 Uiso 1 1 calc R U
H11B H 0.8667 0.5688 0.9592 0.051 Uiso 1 1 calc R U
H11C H 0.7758 0.4340 0.8510 0.051 Uiso 1 1 calc R U
C12 C 0.1775(3) 0.1349(3) 0.79120(18) 0.0173(4) Uani 1 1 d . .
C13 C 0.0003(4) -0.0961(3) 0.8388(2) 0.0264(5) Uani 1 1 d . .
H13A H -0.0852 -0.2012 0.8002 0.032 Uiso 1 1 calc R U
H13B H -0.0572 -0.0232 0.8576 0.032 Uiso 1 1 calc R U
C14 C 0.1111(4) -0.1195(4) 0.9420(2) 0.0355(7) Uani 1 1 d . .
H14A H 0.1699 -0.1896 0.9232 0.053 Uiso 1 1 calc R U
H14B H 0.0437 -0.1696 0.9885 0.053 Uiso 1 1 calc R U
H14C H 0.1921 -0.0146 0.9820 0.053 Uiso 1 1 calc R U
C21 C 0.8075(3) 0.5119(3) 0.57705(17) 0.0159(4) Uani 1 1 d . .
C22 C 0.9444(3) 0.6577(3) 0.5679(2) 0.0223(5) Uani 1 1 d . .
H22A H 1.0492 0.6668 0.6219 0.034 Uiso 1 1 calc R U
H22B H 0.9172 0.7549 0.5821 0.034 Uiso 1 1 calc R U
H22C H 0.9558 0.6464 0.4936 0.034 Uiso 1 1 calc R U
N1 N 0.4687(2) 0.1925(2) 0.39374(15) 0.0154(4) Uani 1 1 d . .
N2 N 0.3122(2) 0.1174(2) 0.53937(14) 0.0147(4) Uani 1 1 d . .
O1 O 0.5028(2) 0.39710(19) 0.68798(12) 0.0176(3) Uani 1 1 d . .
O2 O 0.4631(2) 0.4061(2) 0.85303(13) 0.0212(4) Uani 1 1 d . .
O3 O 0.1631(2) 0.2185(2) 0.86502(14) 0.0221(4) Uani 1 1 d . .
O4 O 0.0968(2) -0.0276(2) 0.76716(14) 0.0236(4) Uani 1 1 d . .
O21 O 0.6579(2) 0.50775(18) 0.53106(12) 0.0158(3) Uani 1 1 d . .
O22 O 0.8364(2) 0.4017(2) 0.62347(15) 0.0243(4) Uani 1 1 d . .
O31 O 1.1560(3) 0.5247(3) 0.7843(2) 0.0362(5) Uani 1 1 d . .
Cu1 Cu 0.47975(3) 0.31535(3) 0.53591(2) 0.01314(10) Uani 1 1 d . .
H31A H 1.067(6) 0.485(6) 0.749(4) 0.054(13) Uiso 1 1 d . .
H31B H 1.170(6) 0.459(6) 0.816(4) 0.058(14) 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'
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'
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
N1 C1 C2 122.0(2) .
N1 C1 H1 119.0 .
C2 C1 H1 119.0 .
C1 C2 C3 118.4(2) .
C1 C2 H2 120.8 .
C3 C2 H2 120.8 .
C4 C3 C2 119.9(2) .
C4 C3 H3 120.1 .
C2 C3 H3 120.1 .
C3 C4 C5 118.7(2) .
C3 C4 H4 120.7 .
C5 C4 H4 120.7 .
N1 C5 C4 121.7(2) .
N1 C5 C6 116.58(18) .
C4 C5 C6 121.7(2) .
N2 C6 C5 109.39(18) .
N2 C6 H6A 109.8 .
C5 C6 H6A 109.8 .
N2 C6 H6B 109.8 .
C5 C6 H6B 109.8 .
H6A C6 H6B 108.2 .
N2 C7 C8 127.4(2) .
N2 C7 H7 116.3 .
C8 C7 H7 116.3 .
C7 C8 C9 119.9(2) .
C7 C8 C12 118.6(2) .
C9 C8 C12 121.23(19) .
O1 C9 O2 118.8(2) .
O1 C9 C8 125.45(19) .
O2 C9 C8 115.7(2) .
O2 C10 C11 110.5(2) .
O2 C10 H10A 109.6 .
C11 C10 H10A 109.6 .
O2 C10 H10B 109.6 .
C11 C10 H10B 109.6 .
H10A C10 H10B 108.1 .
C10 C11 H11A 109.5 .
C10 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C10 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
O3 C12 O4 121.9(2) .
O3 C12 C8 126.6(2) .
O4 C12 C8 111.41(19) .
O4 C13 C14 110.3(2) .
O4 C13 H13A 109.6 .
C14 C13 H13A 109.6 .
O4 C13 H13B 109.6 .
C14 C13 H13B 109.6 .
H13A C13 H13B 108.1 .
C13 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C13 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
O22 C21 O21 122.3(2) .
O22 C21 C22 122.2(2) .
O21 C21 C22 115.5(2) .
C21 C22 H22A 109.5 .
C21 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
C21 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
C5 N1 C1 119.44(19) .
C5 N1 Cu1 114.42(15) .
C1 N1 Cu1 126.07(16) .
C7 N2 C6 117.18(19) .
C7 N2 Cu1 126.38(15) .
C6 N2 Cu1 116.39(14) .
C9 O1 Cu1 128.80(14) .
C9 O2 C10 117.53(18) .
C12 O4 C13 116.13(18) .
C21 O21 Cu1 116.07(14) .
C21 O21 Cu1 138.86(14) 2_666
Cu1 O21 Cu1 104.06(7) 2_666
H31A O31 H31B 102(5) .
N2 Cu1 O21 176.39(8) .
N2 Cu1 O1 90.70(7) .
O21 Cu1 O1 90.92(7) .
N2 Cu1 N1 82.78(8) .
O21 Cu1 N1 95.03(7) .
O1 Cu1 N1 167.67(7) .
N2 Cu1 O21 107.23(7) 2_666
O21 Cu1 O21 75.94(7) 2_666
O1 Cu1 O21 91.51(6) 2_666
N1 Cu1 O21 100.39(7) 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.352(3) .
C1 C2 1.383(3) .
C1 H1 0.9500 .
C2 C3 1.388(4) .
C2 H2 0.9500 .
C3 C4 1.384(3) .
C3 H3 0.9500 .
C4 C5 1.392(3) .
C4 H4 0.9500 .
C5 N1 1.338(3) .
C5 C6 1.504(3) .
C6 N2 1.462(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 N2 1.303(3) .
C7 C8 1.410(3) .
C7 H7 0.9500 .
C8 C9 1.430(3) .
C8 C12 1.464(3) .
C9 O1 1.253(3) .
C9 O2 1.329(3) .
C10 O2 1.461(3) .
C10 C11 1.503(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 O3 1.213(3) .
C12 O4 1.360(3) .
C13 O4 1.447(3) .
C13 C14 1.498(4) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C21 O22 1.238(3) .
C21 O21 1.292(3) .
C21 C22 1.505(3) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
N1 Cu1 2.0085(18) .
N2 Cu1 1.9211(19) .
O1 Cu1 1.9563(15) .
O21 Cu1 1.9438(16) .
O21 Cu1 2.3518(16) 2_666
O31 H31A 0.75(5) .
O31 H31B 0.75(5) .
Cu1 O21 2.3518(16) 2_666
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 -0.1(4) .
C1 C2 C3 C4 0.5(4) .
C2 C3 C4 C5 -0.3(4) .
C3 C4 C5 N1 -0.3(3) .
C3 C4 C5 C6 178.8(2) .
N1 C5 C6 N2 -7.0(3) .
C4 C5 C6 N2 173.8(2) .
N2 C7 C8 C9 -7.8(4) .
N2 C7 C8 C12 177.9(2) .
C7 C8 C9 O1 10.7(4) .
C12 C8 C9 O1 -175.1(2) .
C7 C8 C9 O2 -166.0(2) .
C12 C8 C9 O2 8.1(3) .
C7 C8 C12 O3 -160.7(2) .
C9 C8 C12 O3 25.1(4) .
C7 C8 C12 O4 18.4(3) .
C9 C8 C12 O4 -155.8(2) .
C4 C5 N1 C1 0.7(3) .
C6 C5 N1 C1 -178.5(2) .
C4 C5 N1 Cu1 -176.53(17) .
C6 C5 N1 Cu1 4.3(3) .
C2 C1 N1 C5 -0.4(3) .
C2 C1 N1 Cu1 176.39(17) .
C8 C7 N2 C6 178.7(2) .
C8 C7 N2 Cu1 -3.8(3) .
C5 C6 N2 C7 -175.61(19) .
C5 C6 N2 Cu1 6.7(2) .
O2 C9 O1 Cu1 174.80(15) .
C8 C9 O1 Cu1 -1.8(3) .
O1 C9 O2 C10 -6.6(3) .
C8 C9 O2 C10 170.4(2) .
C11 C10 O2 C9 -79.0(3) .
O3 C12 O4 C13 -3.5(3) .
C8 C12 O4 C13 177.3(2) .
C14 C13 O4 C12 -81.0(3) .
O22 C21 O21 Cu1 -1.3(3) .
C22 C21 O21 Cu1 177.09(15) .
O22 C21 O21 Cu1 164.82(16) 2_666
C22 C21 O21 Cu1 -16.8(3) 2_666
