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#$Date: 2022-01-24 11:10:22 +0200 (Mon, 24 Jan 2022) $
#$Revision: 272211 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/61/1566110.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_1566110
loop_
_publ_author_name
'Lavrenyuk, Helen'
'Mykhalichko, Borys'
'Dziuk, Błażej'
'Olijnyk, Volodymyr'
'Mykhalichko, Oleg'
_publ_section_title
;
 A new copper(II) chelate complex with polyamines as fire retardant and
 epoxy hardener: Synthesis, crystal and electronic structure, and thermal
 behavior of
 (ethylenediamine-N,N′)-(diethylenetriamine-N,N′,N″)-copper(II)
 hexafluoridosilicate
;
_journal_issue                   1
_journal_name_full               'Arabian Journal of Chemistry'
_journal_page_first              3060
_journal_page_last               3069
_journal_paper_doi               10.1016/j.arabjc.2018.08.014
_journal_volume                  13
_journal_year                    2020
_chemical_formula_sum            'C6 H21 Cu F6 N5 Si'
_chemical_formula_weight         368.91
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.460(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9945(4)
_cell_length_b                   9.6067(3)
_cell_length_c                   15.7357(8)
_cell_measurement_reflns_used    3490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      3.10
_cell_volume                     1359.24(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '1024 x 1024 with blocks 2 x 2'
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       ω--scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1888
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3490
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.8437
_exptl_absorpt_correction_T_min  0.6204
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_gt           0.0706
_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)+(0.0188P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                1897
_reflns_number_total             3490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            AJC-2020-13-3060.cif
_cod_data_source_block           76
_cod_database_code               1566110
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Cu Cu 0.97256(6) 0.77929(6) 0.78457(4) 0.01357(16) Uani 1 1 d . . .
Si Si 0.50548(14) 0.75108(12) 0.70334(9) 0.0142(3) Uani 1 1 d . . .
F3 F 0.3992(3) 0.6412(2) 0.75957(17) 0.0195(7) Uani 1 1 d . . .
F4 F 0.3521(3) 0.8390(2) 0.67197(17) 0.0208(7) Uani 1 1 d . . .
F5 F 0.4912(3) 0.6454(3) 0.61847(16) 0.0190(7) Uani 1 1 d . . .
F1 F 0.5199(3) 0.8570(2) 0.79028(17) 0.0203(7) Uani 1 1 d . . .
F2 F 0.6602(3) 0.6665(2) 0.73684(16) 0.0169(7) Uani 1 1 d . . .
F6 F 0.6109(3) 0.8644(3) 0.64816(18) 0.0229(7) Uani 1 1 d . . .
N1 N 0.9901(4) 0.6499(4) 0.8874(2) 0.0182(10) Uani 1 1 d . . .
H1 H 0.972(5) 0.559(5) 0.869(3) 0.022 Uiso 1 1 calc R . .
N2 N 1.1760(4) 0.8737(4) 0.8434(2) 0.0151(10) Uani 1 1 d . . .
H21 H 1.256(5) 0.861(5) 0.809(3) 0.018 Uiso 1 1 calc R . .
H22 H 1.162(5) 0.968(5) 0.851(3) 0.018 Uiso 1 1 calc R . .
N3 N 0.8242(4) 0.8847(4) 0.8528(2) 0.0147(10) Uani 1 1 d . . .
H32 H 0.841(5) 0.979(5) 0.848(3) 0.018 Uiso 1 1 calc R . .
H31 H 0.729(5) 0.866(5) 0.833(3) 0.018 Uiso 1 1 calc R . .
N4 N 0.9288(4) 0.8938(4) 0.6797(2) 0.0171(10) Uani 1 1 d . . .
H41 H 0.828(5) 0.895(5) 0.669(3) 0.020 Uiso 1 1 calc R . .
H42 H 0.960(5) 0.984(5) 0.689(3) 0.020 Uiso 1 1 calc R . .
N5 N 1.0669(4) 0.6459(4) 0.7028(2) 0.0169(10) Uani 1 1 d . . .
H51 H 1.168(5) 0.657(5) 0.704(3) 0.020 Uiso 1 1 calc R . .
H52 H 1.046(5) 0.555(5) 0.717(3) 0.020 Uiso 1 1 calc R . .
C1 C 0.8396(6) 0.8428(5) 0.9421(3) 0.0211(13) Uani 1 1 d . . .
H1A H 0.747(5) 0.864(5) 0.972(3) 0.025 Uiso 1 1 calc R . .
H1B H 0.922(5) 0.895(5) 0.970(3) 0.025 Uiso 1 1 calc R . .
C2 C 0.8706(5) 0.6883(5) 0.9469(3) 0.0189(12) Uani 1 1 d . . .
H2A H 0.902(5) 0.663(5) 1.006(3) 0.023 Uiso 1 1 calc R . .
H2B H 0.779(5) 0.636(5) 0.932(3) 0.023 Uiso 1 1 calc R . .
C3 C 1.2045(5) 0.8057(5) 0.9255(3) 0.0205(12) Uani 1 1 d . . .
H3A H 1.156(5) 0.859(5) 0.971(3) 0.025 Uiso 1 1 calc R . .
H3B H 1.313(5) 0.804(5) 0.938(3) 0.025 Uiso 1 1 calc R . .
C4 C 1.1439(5) 0.6568(5) 0.9226(3) 0.0209(13) Uani 1 1 d . . .
H4A H 1.209(5) 0.599(5) 0.887(3) 0.025 Uiso 1 1 calc R . .
H4B H 1.146(5) 0.618(5) 0.981(3) 0.025 Uiso 1 1 calc R . .
C5 C 1.0043(5) 0.6781(5) 0.6170(3) 0.0181(13) Uani 1 1 d . . .
H5A H 0.902(5) 0.641(5) 0.611(3) 0.022 Uiso 1 1 calc R . .
H5B H 1.065(5) 0.634(5) 0.573(3) 0.022 Uiso 1 1 calc R . .
C6 C 1.0040(5) 0.8359(5) 0.6063(3) 0.0178(12) Uani 1 1 d . . .
H6A H 1.107(5) 0.871(5) 0.604(3) 0.021 Uiso 1 1 calc R . .
H6B H 0.950(5) 0.862(5) 0.553(3) 0.021 Uiso 1 1 calc R . .
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'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 '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
N3 Cu N4 92.53(16) . .
N3 Cu N5 163.13(15) . .
N4 Cu N5 84.30(16) . .
N3 Cu N1 85.54(16) . .
N4 Cu N1 172.22(16) . .
N5 Cu N1 95.37(15) . .
N3 Cu N2 97.07(14) . .
N4 Cu N2 105.06(14) . .
N5 Cu N2 99.76(14) . .
N1 Cu N2 82.68(14) . .
F5 Si F4 91.42(14) . .
F5 Si F2 90.18(13) . .
F4 Si F2 178.37(15) . .
F5 Si F3 90.35(14) . .
F4 Si F3 89.82(14) . .
F2 Si F3 90.50(13) . .
F5 Si F6 90.75(15) . .
F4 Si F6 89.57(13) . .
F2 Si F6 90.08(14) . .
F3 Si F6 178.75(16) . .
F5 Si F1 179.42(15) . .
F4 Si F1 88.91(13) . .
F2 Si F1 89.50(13) . .
F3 Si F1 89.17(15) . .
F6 Si F1 89.73(14) . .
C4 N1 C2 115.9(4) . .
C4 N1 Cu 108.8(3) . .
C2 N1 Cu 107.8(3) . .
C3 N2 Cu 108.0(3) . .
C1 N3 Cu 109.0(3) . .
C6 N4 Cu 110.8(3) . .
C5 N5 Cu 107.0(3) . .
N3 C1 C2 109.3(4) . .
N1 C2 C1 110.3(4) . .
N2 C3 C4 109.7(4) . .
N1 C4 C3 112.4(4) . .
N5 C5 C6 107.9(4) . .
N4 C6 C5 106.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N3 2.008(4) .
Cu N4 2.014(4) .
Cu N5 2.018(4) .
Cu N1 2.043(4) .
Cu N2 2.223(3) .
Si F5 1.679(3) .
Si F4 1.681(3) .
Si F2 1.684(3) .
Si F3 1.690(3) .
Si F6 1.697(3) .
Si F1 1.708(3) .
N1 C4 1.479(5) .
N1 C2 1.489(6) .
N2 C3 1.465(5) .
N3 C1 1.465(6) .
N4 C6 1.463(6) .
N5 C5 1.482(5) .
C1 C2 1.512(6) .
C3 C4 1.531(6) .
C5 C6 1.526(6) .
