#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:51:22 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224350 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/03/7700336.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_7700336
loop_
_publ_author_name
'Rad-Yousefnia, Negar'
'Shaabani, Behrouz'
'Korabik, Maria'
'Weselski, Marek'
'Zahedi, Mansoureh'
'Englert, Ulli'
'Bikas, Rahman'
'Szeliga, Daria'
'Otręba, Marta'
'Lis, Tadeusz'
_publ_section_title
;
 Magnetic dimensionality and the crystal structure of two copper(ii)
 coordination polymers containing Cu₆ and Cu₂
 building units.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11421
_journal_page_last               11432
_journal_paper_doi               10.1039/c9dt01728c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 H24 Cu2 Fe N10 O2, H2 O'
_chemical_formula_sum            'C14 H26 Cu2 Fe N10 O3'
_chemical_formula_weight         565.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-04-13 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.125(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.895(8)
_cell_length_b                   9.354(7)
_cell_length_c                   11.045(9)
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.98
_cell_volume                     1035.2(14)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 gonimeter with APEX CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5590
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.341
_diffrn_reflns_theta_min         2.979
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1114
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0636
_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)+(0.1250P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                809
_reflns_number_total             1114
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01728c2.cif
_cod_data_source_block           u16_03
_cod_depositor_comments
'Adding full bibliography for 7700336--7700337.cif.'
_cod_database_code               7700336
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.389
_shelx_estimated_absorpt_t_max   0.922
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.12015(10) 0.000000 0.14912(10) 0.0324(5) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.000000 0.0204(5) Uani 1 4 d S T P . .
N1 N 0.2644(7) 0.000000 0.0858(7) 0.0245(15) Uani 1 2 d S T P . .
N2 N 0.6834(9) 0.000000 0.2968(8) 0.043(2) Uani 1 2 d S T P . .
N3 N 0.000000 0.1736(8) 0.000000 0.067(3) Uani 1 2 d S T P . .
N4 N -0.0294(7) 0.000000 0.2146(7) 0.0258(15) Uani 1 2 d S T P B .
H4 H -0.115623 0.000000 0.135561 0.031 Uiso 1 2 calc R U P A 1
C1 C 0.3522(8) 0.000000 0.0526(8) 0.0207(16) Uani 1 2 d S T P . .
C2 C 0.6152(9) 0.000000 0.1847(9) 0.0293(18) Uani 1 2 d S T P . .
C3 C 0.000000 0.2965(8) 0.000000 0.0301(19) Uani 1 2 d S T P . .
C4A C -0.0252(7) 0.1325(7) 0.2899(7) 0.0417(17) Uani 0.5 1 d D . P B 1
H4A H -0.088623 0.117738 0.332916 0.050 Uiso 0.5 1 calc R U P B 1
H4B H -0.063663 0.208989 0.223772 0.050 Uiso 0.5 1 calc R U P B 1
C5A C 0.0985(15) 0.1932(19) 0.3926(15) 0.042(4) Uani 0.5 1 d D U P B 1
H5A H 0.082518 0.291536 0.416368 0.050 Uiso 0.5 1 calc R U P B 1
H5B H 0.129641 0.133246 0.472920 0.050 Uiso 0.5 1 calc R U P B 1
O5A O 0.1930(11) 0.1934(12) 0.3339(11) 0.048(3) Uani 0.5 1 d D U P B 1
H5O H 0.261402 0.148197 0.382108 0.058 Uiso 0.5 1 calc R U P B 1
C4B C -0.0252(7) 0.1325(7) 0.2899(7) 0.0417(17) Uani 0.5 1 d D . P B 2
H4C H -0.074019 0.120030 0.348188 0.050 Uiso 0.5 1 calc R U P B 2
H4D H -0.064027 0.214255 0.230104 0.050 Uiso 0.5 1 calc R U P B 2
C5B C 0.1271(12) 0.1547(18) 0.3715(13) 0.031(3) Uani 0.5 1 d D U P B 2
H5C H 0.142726 0.251202 0.411586 0.038 Uiso 0.5 1 calc R U P B 2
H5D H 0.159551 0.083333 0.443313 0.038 Uiso 0.5 1 calc R U P B 2
N5B N 0.2030(12) 0.1388(13) 0.2833(11) 0.032(2) Uani 0.5 1 d D U P B 2
H5N H 0.288375 0.111687 0.332334 0.039 Uiso 0.5 1 calc R U P B 2
H5M H 0.205612 0.224558 0.245409 0.039 Uiso 0.5 1 calc R U P B 2
O1 O -0.007(3) 0.443(2) 0.544(2) 0.078(8) Uiso 0.25 1 d . . P C -1
H1O H -0.068078 0.496429 0.495870 0.094 Uiso 0.25 1 d R U P C -1
H1P H 0.066622 0.496429 0.586769 0.094 Uiso 0.25 1 d R U P C -1
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
N5B Cu1 N5B 85.7(7) 6 .
N5B Cu1 N1 94.4(3) 6 .
N5B Cu1 N1 94.4(3) . .
N5B Cu1 N4 85.7(3) 6 .
N5B Cu1 N4 85.7(3) . .
N1 Cu1 N4 179.9(3) . .
N1 Cu1 N3 93.14(15) . 5
N4 Cu1 N3 86.82(16) . 5
N5B Cu1 N3 172.3(3) 6 .
N5B Cu1 N3 92.2(4) . .
N1 Cu1 N3 93.14(15) . .
N4 Cu1 N3 86.82(16) . .
N3 Cu1 N3 89.0(3) 5 .
C3 Fe1 C3 180.0 7 3_545
C3 Fe1 C1 90.0 7 5_655
C3 Fe1 C1 90.0 3_545 5_655
C3 Fe1 C1 90.0 7 .
C3 Fe1 C1 90.0 3_545 .
C1 Fe1 C1 180.0 5_655 .
C3 Fe1 C2 90.0 7 .
C3 Fe1 C2 90.0 3_545 .
C1 Fe1 C2 92.6(3) 5_655 .
C1 Fe1 C2 87.4(3) . .
C3 Fe1 C2 90.0 7 5_655
C3 Fe1 C2 90.0 3_545 5_655
C1 Fe1 C2 87.4(3) 5_655 5_655
C1 Fe1 C2 92.6(3) . 5_655
C2 Fe1 C2 180.0 . 5_655
C1 N1 Cu1 177.8(8) . .
C3 N3 Cu1 134.49(13) . .
C3 N3 Cu1 134.49(13) . 5
Cu1 N3 Cu1 91.0(3) . 5
C4A N4 C4A 113.3(7) 6 .
C4A N4 Cu1 110.4(4) 6 .
C4B N4 Cu1 110.4(4) . .
C4A N4 Cu1 110.4(4) . .
C4A N4 H4 107.5 6 .
C4A N4 H4 107.5 . .
Cu1 N4 H4 107.5 . .
N1 C1 Fe1 179.2(8) . .
N2 C2 Fe1 179.1(7) . .
N3 C3 Fe1 180.0 . 3_455
N4 C4A C5A 124.4(9) . .
N4 C4A H4A 106.2 . .
C5A C4A H4A 106.2 . .
N4 C4A H4B 106.2 . .
C5A C4A H4B 106.2 . .
H4A C4A H4B 106.4 . .
O5A C5A C4A 104.7(10) . .
O5A C5A H5A 110.8 . .
C4A C5A H5A 110.8 . .
O5A C5A H5B 110.8 . .
C4A C5A H5B 110.8 . .
H5A C5A H5B 108.9 . .
C5A O5A H5O 109.5 . .
N4 C4B C5B 103.1(7) . .
N4 C4B H4C 111.1 . .
C5B C4B H4C 111.1 . .
N4 C4B H4D 111.1 . .
C5B C4B H4D 111.1 . .
H4C C4B H4D 109.1 . .
N5B C5B C4B 109.9(9) . .
N5B C5B H5C 109.7 . .
C4B C5B H5C 109.7 . .
N5B C5B H5D 109.7 . .
C4B C5B H5D 109.7 . .
H5C C5B H5D 108.2 . .
C5B N5B Cu1 110.8(7) . .
C5B N5B H5N 109.5 . .
Cu1 N5B H5N 109.5 . .
C5B N5B H5M 109.5 . .
Cu1 N5B H5M 109.5 . .
H5N N5B H5M 108.1 . .
H1O O1 H1P 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N5B 1.909(12) 6
Cu1 N5B 1.909(12) .
Cu1 N1 1.956(7) .
Cu1 N4 2.025(6) .
Cu1 N3 2.317(5) 5
Cu1 N3 2.317(5) .
Fe1 C3 1.903(8) 7
Fe1 C3 1.903(8) 3_545
Fe1 C1 1.914(8) 5_655
Fe1 C1 1.914(8) .
Fe1 C2 1.930(10) .
Fe1 C2 1.930(10) 5_655
N1 C1 1.151(11) .
N2 C2 1.167(11) .
N3 C3 1.150(11) .
N4 C4A 1.483(7) 6
N4 C4B 1.483(7) .
N4 C4A 1.483(7) .
N4 H4 1.0000 .
C4A C5A 1.492(14) .
C4A H4A 0.9900 .
C4A H4B 0.9900 .
C5A O5A 1.416(13) .
C5A H5A 0.9900 .
C5A H5B 0.9900 .
O5A H5O 0.8400 .
C4B C5B 1.561(14) .
C4B H4C 0.9900 .
C4B H4D 0.9900 .
C5B N5B 1.512(12) .
C5B H5C 0.9900 .
C5B H5D 0.9900 .
N5B H5N 0.9100 .
N5B H5M 0.9100 .
O1 H1O 0.8336 .
O1 H1P 0.9106 .
