#------------------------------------------------------------------------------
#$Date: 2019-07-13 05:41:50 +0200 (Sat 13 de Jul de 2019) $
#$Revision: 217002 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/31/7233103.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_7233103
loop_
_publ_author_name
'Vušak, Darko'
'Smrečki, Neven'
'Prugovečki, Biserka'
'Đilović, Ivica'
'Kirasić, Inka'
'Žilić, Dijana'
'Muratović, Senada'
'Matković-Čalogović, Dubravka'
_publ_section_title
;
 Cobalt, nickel and copper complexes with glycinamide: structural insights
 and magnetic properties
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              21637
_journal_paper_doi               10.1039/C9RA03693H
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C4 H12 Cu1 N4 O2, Cu1 I3'
_chemical_formula_sum            'C4 H12 Cu2 I3 N4 O2'
_chemical_formula_weight         655.96
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-10 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                84.575(4)
_cell_angle_beta                 77.367(4)
_cell_angle_gamma                72.679(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0185(4)
_cell_length_b                   8.6901(4)
_cell_length_c                   11.0929(5)
_cell_measurement_reflns_used    4212
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3130
_cell_measurement_theta_min      4.7390
_cell_volume                     719.69(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7861
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         4.180
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_description       plate
_exptl_crystal_F_000             594
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0353P)²+2.0974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2548
_reflns_number_total             3084
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ra03693h2.cif
_cod_data_source_block           3c
_cod_database_code               7233103
_shelx_shelxl_version_number     2014/7
_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   0.138
_shelx_estimated_absorpt_t_max   0.705
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
C101 C 0.5338(7) -0.2278(7) 0.1056(5) 0.0407(13) Uani 1 1 d . .
C102 C 0.5425(7) -0.3440(7) 0.2163(5) 0.0455(14) Uani 1 1 d . .
H106 H 0.4259 -0.3591 0.2496 0.055 Uiso 1 1 calc R U
H105 H 0.6255 -0.4479 0.1919 0.055 Uiso 1 1 calc R U
C103 C 0.9623(7) 0.0650(6) 0.1839(5) 0.0368(12) Uani 1 1 d . .
C104 C 0.9983(8) -0.0189(6) 0.3039(5) 0.0401(12) Uani 1 1 d . .
H103 H 1.1093 -0.1050 0.2895 0.048 Uiso 1 1 calc R U
H104 H 1.0085 0.0567 0.3590 0.048 Uiso 1 1 calc R U
O11 O 0.6285(5) -0.1336(5) 0.0883(3) 0.0451(10) Uani 1 1 d . .
O21 O 0.8533(5) 0.0305(5) 0.1313(3) 0.0400(9) Uani 1 1 d . .
N11 N 0.4325(7) -0.2325(7) 0.0307(5) 0.0643(17) Uani 1 1 d . .
H11A H 0.4288 -0.1693 -0.0338 0.077 Uiso 1 1 calc R U
H11B H 0.3690 -0.2988 0.0453 0.077 Uiso 1 1 calc R U
N101 N 0.6021(6) -0.2764(6) 0.3105(4) 0.0419(11) Uani 1 1 d . .
H108 H 0.6701 -0.3554 0.3506 0.050 Uiso 1 1 calc R U
H107 H 0.5082 -0.2234 0.3650 0.050 Uiso 1 1 calc R U
N102 N 1.0513(7) 0.1652(6) 0.1351(5) 0.0541(14) Uani 1 1 d . .
H101 H 1.0376 0.2112 0.0644 0.065 Uiso 1 1 calc R U
H102 H 1.1241 0.1858 0.1734 0.065 Uiso 1 1 calc R U
N22 N 0.8490(6) -0.0856(6) 0.3600(4) 0.0405(11) Uani 1 1 d . .
H22C H 0.7680 -0.0160 0.4123 0.049 Uiso 1 1 calc R U
H22D H 0.8885 -0.1771 0.4018 0.049 Uiso 1 1 calc R U
Cu1 Cu 0.74070(9) -0.12646(9) 0.22635(6) 0.04159(18) Uani 1 1 d . .
Cu2 Cu 0.12297(10) 0.43898(9) 0.36934(7) 0.0496(2) Uani 1 1 d . .
I1 I 0.08127(4) 0.57732(4) 0.15092(3) 0.03569(11) Uani 1 1 d . .
I2 I -0.18519(4) 0.36989(4) 0.48163(3) 0.03481(11) Uani 1 1 d . .
I3 I 0.39021(5) 0.17243(4) 0.33524(4) 0.04462(12) 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 0.0000 0.0000 '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'
N N 0.0061 0.0033 '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'
I I -0.4742 1.8119 '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
O11 C101 N11 122.4(5) . .
O11 C101 C102 118.6(5) . .
N11 C101 C102 119.0(5) . .
N101 C102 C101 108.5(4) . .
N101 C102 H106 110.0 . .
C101 C102 H106 110.0 . .
N101 C102 H105 110.0 . .
C101 C102 H105 110.0 . .
H106 C102 H105 108.4 . .
O21 C103 N102 122.5(5) . .
O21 C103 C104 119.5(5) . .
N102 C103 C104 118.0(5) . .
N22 C104 C103 108.2(4) . .
N22 C104 H103 110.1 . .
C103 C104 H103 110.1 . .
N22 C104 H104 110.1 . .
C103 C104 H104 110.1 . .
H103 C104 H104 108.4 . .
C101 O11 Cu1 114.4(3) . .
C103 O21 Cu1 113.2(3) . .
C101 N11 H11A 120.0 . .
C101 N11 H11B 120.0 . .
H11A N11 H11B 120.0 . .
C102 N101 Cu1 108.6(3) . .
C102 N101 H108 110.0 . .
Cu1 N101 H108 110.0 . .
C102 N101 H107 110.0 . .
Cu1 N101 H107 110.0 . .
H108 N101 H107 108.4 . .
C103 N102 H101 120.0 . .
C103 N102 H102 120.0 . .
H101 N102 H102 120.0 . .
C104 N22 Cu1 108.6(3) . .
C104 N22 H22C 110.0 . .
Cu1 N22 H22C 110.0 . .
C104 N22 H22D 110.0 . .
Cu1 N22 H22D 110.0 . .
H22C N22 H22D 108.4 . .
O11 Cu1 O21 89.25(15) . .
O11 Cu1 N22 171.69(18) . .
O21 Cu1 N22 84.05(17) . .
O11 Cu1 N101 84.21(17) . .
O21 Cu1 N101 172.74(16) . .
N22 Cu1 N101 102.18(19) . .
I3 Cu2 I1 108.45(3) . .
I3 Cu2 I2 109.74(3) . 2_566
I1 Cu2 I2 112.86(3) . 2_566
I3 Cu2 I2 110.52(3) . .
I1 Cu2 I2 108.13(3) . .
I2 Cu2 I2 107.12(3) 2_566 .
Cu2 I2 Cu2 72.88(3) 2_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C101 O11 1.249(7) .
C101 N11 1.293(7) .
C101 C102 1.515(7) .
C102 N101 1.471(8) .
C102 H106 0.9700 .
C102 H105 0.9700 .
C103 O21 1.267(6) .
C103 N102 1.293(7) .
C103 C104 1.499(7) .
C104 N22 1.474(7) .
C104 H103 0.9700 .
C104 H104 0.9700 .
O11 Cu1 1.953(4) .
O21 Cu1 1.958(4) .
N11 H11A 0.8600 .
N11 H11B 0.8600 .
N101 Cu1 1.996(4) .
N101 H108 0.8900 .
N101 H107 0.8900 .
N102 H101 0.8600 .
N102 H102 0.8600 .
N22 Cu1 1.981(4) .
N22 H22C 0.8900 .
N22 H22D 0.8900 .
Cu2 I3 2.6374(8) .
Cu2 I1 2.6443(8) .
Cu2 I2 2.6671(9) 2_566
Cu2 I2 2.7228(9) .
I2 Cu2 2.6671(9) 2_566
