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#$Date: 2021-07-02 12:55:01 +0300 (Fri, 02 Jul 2021) $
#$Revision: 266907 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/38/1563898.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_1563898
loop_
_publ_author_name
'Mistry, Subhradeep'
'Natarajan, Srinivasan'
_publ_section_title
;
 Synthesis, structures and magnetic studies of new copper-azides
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              26
_journal_page_last               38
_journal_paper_doi               10.1016/j.ica.2018.08.001
_journal_volume                  483
_journal_year                    2018
_chemical_formula_moiety         'C6 H20 Cu7 N46'
_chemical_formula_sum            'C6 H20 Cu7 N46'
_chemical_formula_weight         1181.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                102.000(3)
_cell_angle_beta                 96.837(3)
_cell_angle_gamma                109.054(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4313(5)
_cell_length_b                   9.7110(6)
_cell_length_c                   11.9231(8)
_cell_measurement_reflns_used    3433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      1.783
_cell_volume                     883.93(10)
_computing_cell_refinement       'CrysAlisPro CCD (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro RED (Oxford Diffraction, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Xcalibur,Eos(Nova) CCD detector'
_diffrn_measurement_method       'fω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_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            13176
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.783
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.213
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction,2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod shaped'
_exptl_crystal_F_000             581
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0288P)²+0.6319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2755
_reflns_number_total             3433
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            CompoundsI-III.cif
_cod_data_source_block           compoundIII
_cod_database_code               1563898
_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.
;
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4699(6) 0.2572(6) -0.0671(5) 0.0439(15) Uani 1 1 d . . . . .
H1A H 0.5114 0.3667 -0.0434 0.053 Uiso 1 1 calc R U . . .
H1B H 0.4406 0.2252 -0.1519 0.053 Uiso 1 1 calc R U . . .
C2 C 0.3182(6) 0.1980(6) -0.0210(6) 0.0421(14) Uani 1 1 d . . . . .
H2 H 0.3508 0.2487 0.0629 0.050 Uiso 1 1 calc R U . . .
C3 C 0.1638(5) 0.2334(5) -0.0656(4) 0.0285(11) Uani 1 1 d . . . . .
H3A H 0.0709 0.1889 -0.0296 0.043 Uiso 1 1 calc R U . . .
H3B H 0.1928 0.3408 -0.0466 0.043 Uiso 1 1 calc R U . . .
H3C H 0.1299 0.1928 -0.1490 0.043 Uiso 1 1 calc R U . . .
N1 N 0.6055(4) 0.2066(4) -0.0265(3) 0.0177(8) Uani 1 1 d . . . . .
H1C H 0.6713 0.2715 0.0399 0.021 Uiso 1 1 calc R U . . .
H1D H 0.6707 0.2024 -0.0796 0.021 Uiso 1 1 calc R U . . .
N2 N 0.2786(4) 0.0361(4) -0.0282(3) 0.0190(8) Uani 1 1 d . . . . .
H2A H 0.2167 -0.0197 -0.0986 0.023 Uiso 1 1 calc R U . . .
H2B H 0.2180 0.0100 0.0253 0.023 Uiso 1 1 calc R U . . .
N3 N -0.1138(4) 0.2543(4) 0.5946(3) 0.0156(8) Uani 1 1 d . . . . .
N4 N -0.1627(4) 0.2122(4) 0.6778(3) 0.0148(8) Uani 1 1 d . . . . .
N5 N -0.2096(4) 0.1758(4) 0.7571(3) 0.0250(9) Uani 1 1 d . . . . .
N6 N -0.1414(4) 0.0138(4) 0.3878(3) 0.0224(9) Uani 1 1 d . . . . .
N7 N -0.2871(4) -0.0424(4) 0.3986(3) 0.0158(8) Uani 1 1 d . . . . .
N8 N -0.4280(4) -0.1045(4) 0.4037(3) 0.0192(8) Uani 1 1 d . . . . .
N9 N 0.2571(4) 0.3449(4) 0.5987(3) 0.0152(8) Uani 1 1 d . . . . .
N10 N 0.2874(4) 0.4261(4) 0.6977(3) 0.0153(8) Uani 1 1 d . . . . .
N11 N 0.3176(5) 0.5047(4) 0.7894(3) 0.0280(9) Uani 1 1 d . . . . .
N12 N 0.2072(4) 0.1628(4) 0.4005(3) 0.0140(8) Uani 1 1 d . . . . .
N13 N 0.1755(4) 0.1381(4) 0.2943(3) 0.0145(8) Uani 1 1 d . . . . .
N14 N 0.1430(4) 0.1116(5) 0.1949(3) 0.0281(9) Uani 1 1 d . . . . .
N15 N 0.6438(4) 0.4601(3) 0.6051(3) 0.0113(7) Uani 1 1 d . . . . .
N16 N 0.6742(4) 0.4774(4) 0.7120(3) 0.0165(8) Uani 1 1 d . . . . .
N17 N 0.7039(5) 0.4961(5) 0.8104(4) 0.0352(11) Uani 1 1 d . . . . .
N18 N 0.5880(4) 0.2898(4) 0.3979(3) 0.0120(7) Uani 1 1 d . . . . .
N19 N 0.5635(4) 0.1923(3) 0.3088(3) 0.0112(7) Uani 1 1 d . . . . .
N20 N 0.5403(4) 0.1025(4) 0.2242(3) 0.0182(8) Uani 1 1 d . . . . .
N21 N 0.9763(4) 0.4010(4) 0.4027(3) 0.0120(7) Uani 1 1 d . . . . .
N22 N 0.9398(4) 0.3496(4) 0.2962(3) 0.0131(8) Uani 1 1 d . . . . .
N23 N 0.9076(4) 0.2997(4) 0.1970(3) 0.0247(9) Uani 1 1 d . . . . .
Cu1 Cu 0.5000 0.0000 0.0000 0.01537(19) Uani 1 2 d S . P . .
Cu2 Cu 0.03550(5) 0.18505(5) 0.50223(4) 0.01239(14) Uani 1 1 d . . . . .
Cu3 Cu 0.42628(5) 0.30497(5) 0.50440(4) 0.01199(14) Uani 1 1 d . . . . .
Cu4 Cu 0.81139(5) 0.41745(5) 0.50920(4) 0.00971(14) 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'
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'
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
C2 C1 N1 112.2(5) . .
C2 C1 H1A 109.2 . .
N1 C1 H1A 109.2 . .
C2 C1 H1B 109.2 . .
N1 C1 H1B 109.2 . .
H1A C1 H1B 107.9 . .
C1 C2 N2 110.3(4) . .
C1 C2 C3 116.5(5) . .
N2 C2 C3 113.5(4) . .
C1 C2 H2 105.1 . .
N2 C2 H2 105.1 . .
C3 C2 H2 105.1 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 N1 Cu1 109.3(3) . .
C1 N1 H1C 109.8 . .
Cu1 N1 H1C 109.8 . .
C1 N1 H1D 109.8 . .
Cu1 N1 H1D 109.8 . .
H1C N1 H1D 108.3 . .
C2 N2 Cu1 108.8(3) . .
C2 N2 H2A 109.9 . .
Cu1 N2 H2A 109.9 . .
C2 N2 H2B 109.9 . .
Cu1 N2 H2B 109.9 . .
H2A N2 H2B 108.3 . .
N4 N3 Cu2 126.6(3) . .
N4 N3 Cu4 127.1(3) . 1_455
Cu2 N3 Cu4 106.26(15) . 1_455
N5 N4 N3 178.3(4) . .
N7 N6 Cu2 124.9(3) . .
N8 N7 N6 175.7(4) . .
N7 N8 Cu3 106.2(3) . 2_556
N10 N9 Cu3 127.6(3) . .
N10 N9 Cu2 129.9(3) . .
Cu3 N9 Cu2 101.31(14) . .
N11 N10 N9 178.5(4) . .
N13 N12 Cu3 125.0(3) . .
N13 N12 Cu2 123.3(3) . .
Cu3 N12 Cu2 101.56(14) . .
N14 N13 N12 178.3(4) . .
N16 N15 Cu3 121.0(3) . .
N16 N15 Cu4 119.9(3) . .
Cu3 N15 Cu4 99.41(13) . .
N17 N16 N15 178.7(4) . .
N19 N18 Cu3 127.8(2) . .
N19 N18 Cu4 128.0(3) . .
Cu3 N18 Cu4 99.74(14) . .
N20 N19 N18 178.9(4) . .
N22 N21 Cu4 126.4(2) . .
N22 N21 Cu4 124.6(3) . 2_766
Cu4 N21 Cu4 100.72(13) . 2_766
N23 N22 N21 178.6(4) . .
N2 Cu1 N2 180.0 2_655 .
N2 Cu1 N1 84.37(13) 2_655 2_655
N2 Cu1 N1 95.63(13) . 2_655
N2 Cu1 N1 95.63(13) 2_655 .
N2 Cu1 N1 84.37(13) . .
N1 Cu1 N1 180.0 2_655 .
N6 Cu2 N3 98.09(14) . .
N6 Cu2 N9 166.06(13) . .
N3 Cu2 N9 95.85(13) . .
N6 Cu2 N12 88.92(13) . .
N3 Cu2 N12 166.46(14) . .
N9 Cu2 N12 77.52(12) . .
N12 Cu3 N18 100.16(13) . .
N12 Cu3 N15 175.91(14) . .
N18 Cu3 N15 80.02(12) . .
N12 Cu3 N9 79.03(13) . .
N18 Cu3 N9 170.68(15) . .
N15 Cu3 N9 100.12(13) . .
N12 Cu3 N8 87.72(13) . 2_556
N18 Cu3 N8 100.44(13) . 2_556
N15 Cu3 N8 96.27(13) . 2_556
N9 Cu3 N8 88.82(13) . 2_556
N12 Cu3 Cu4 140.28(9) . .
N18 Cu3 Cu4 40.39(9) . .
N15 Cu3 Cu4 40.44(9) . .
N9 Cu3 Cu4 140.56(9) . .
N8 Cu3 Cu4 94.70(8) 2_556 .
N18 Cu4 N15 79.23(12) . .
N18 Cu4 N21 100.08(12) . .
N15 Cu4 N21 171.10(14) . .
N18 Cu4 N21 161.01(14) . 2_766
N15 Cu4 N21 98.46(12) . 2_766
N21 Cu4 N21 79.28(13) . 2_766
N18 Cu4 N3 104.55(13) . 1_655
N15 Cu4 N3 100.44(13) . 1_655
N21 Cu4 N3 88.34(13) . 1_655
N21 Cu4 N3 94.42(13) 2_766 1_655
N18 Cu4 Cu3 39.87(9) . .
N15 Cu4 Cu3 40.15(8) . .
N21 Cu4 Cu3 139.95(9) . .
N21 Cu4 Cu3 137.85(9) 2_766 .
N3 Cu4 Cu3 100.16(8) 1_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.445(7) .
C1 N1 1.455(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.478(6) .
C2 C3 1.516(6) .
C2 H2 0.9800 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
N1 Cu1 2.020(3) .
N1 H1C 0.8900 .
N1 H1D 0.8900 .
N2 Cu1 2.012(3) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N3 N4 1.216(5) .
N3 Cu2 1.956(3) .
N3 Cu4 2.262(4) 1_455
N4 N5 1.145(5) .
N6 N7 1.205(4) .
N6 Cu2 1.950(3) .
N7 N8 1.159(4) .
N8 Cu3 2.428(4) 2_556
N9 N10 1.220(5) .
N9 Cu3 2.003(3) .
N9 Cu2 2.019(3) .
N10 N11 1.141(5) .
N12 N13 1.218(5) .
N12 Cu3 1.983(3) .
N12 Cu2 2.032(3) .
N13 N14 1.138(5) .
N15 N16 1.234(5) .
N15 Cu3 1.999(3) .
N15 Cu4 2.011(3) .
N16 N17 1.133(5) .
N18 N19 1.212(4) .
N18 Cu3 1.989(3) .
N18 Cu4 2.011(3) .
N19 N20 1.137(4) .
N21 N22 1.223(4) .
N21 Cu4 2.014(3) .
N21 Cu4 2.034(3) 2_766
N22 N23 1.143(4) .
Cu1 N2 2.012(3) 2_655
Cu1 N1 2.020(3) 2_655
Cu3 N8 2.428(4) 2_556
Cu3 Cu4 3.0583(6) .
Cu4 N21 2.034(3) 2_766
Cu4 N3 2.262(4) 1_655
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N1 C1 C2 N2 -43.9(6) . . . .
N1 C1 C2 C3 -175.2(4) . . . .
C2 C1 N1 Cu1 30.6(5) . . . .
C1 C2 N2 Cu1 35.0(5) . . . .
C3 C2 N2 Cu1 167.8(4) . . . .
