#------------------------------------------------------------------------------
#$Date: 2021-07-02 12:55:01 +0300 (Fri, 02 Jul 2021) $
#$Revision: 266907 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/38/1563896.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_1563896
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         'C3 H10 Cu3 N20'
_chemical_formula_sum            'C3 H10 Cu3 N20'
_chemical_formula_weight         516.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.402(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2510(5)
_cell_length_b                   11.9939(8)
_cell_length_c                   21.6395(18)
_cell_measurement_reflns_used    3181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      1.891
_cell_volume                     1615.2(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1113
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction,2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod shaped'
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0418P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2502
_reflns_number_total             3181
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            CompoundsI-III.cif
_cod_data_source_block           compoundI
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1563896
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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 0.9349(8) 0.0969(4) 0.1445(2) 0.0381(13) Uani 1 1 d . . . . .
H1A H 0.9480 0.1542 0.1135 0.046 Uiso 1 1 calc R U . . .
H1B H 1.0620 0.0502 0.1460 0.046 Uiso 1 1 calc R U . . .
C2 C 0.7446(9) 0.0291(4) 0.1267(2) 0.0363(13) Uani 1 1 d . . . . .
H2 H 0.6291 0.0835 0.1174 0.044 Uiso 1 1 calc R U . . .
C3 C 0.7468(8) -0.0384(4) 0.0682(2) 0.0287(11) Uani 1 1 d . . . . .
H3A H 0.7906 0.0080 0.0355 0.043 Uiso 1 1 calc R U . . .
H3B H 0.8459 -0.0993 0.0752 0.043 Uiso 1 1 calc R U . . .
H3C H 0.6054 -0.0671 0.0566 0.043 Uiso 1 1 calc R U . . .
N1 N 0.9223(5) 0.1498(3) 0.20593(15) 0.0138(7) Uani 1 1 d . . . . .
H1C H 0.8553 0.2152 0.2013 0.017 Uiso 1 1 calc R U . . .
H1D H 1.0540 0.1617 0.2241 0.017 Uiso 1 1 calc R U . . .
N2 N 0.6802(5) -0.0330(3) 0.17999(16) 0.0189(8) Uani 1 1 d . . . . .
H2A H 0.7435 -0.0996 0.1816 0.023 Uiso 1 1 calc R U . . .
H2B H 0.5386 -0.0436 0.1756 0.023 Uiso 1 1 calc R U . . .
N3 N 0.7849(5) 0.1401(3) 0.33544(15) 0.0131(7) Uani 1 1 d . . . . .
N4 N 0.7699(5) 0.2409(3) 0.33861(15) 0.0134(7) Uani 1 1 d . . . . .
N5 N 0.7602(6) 0.3366(3) 0.34186(18) 0.0241(9) Uani 1 1 d . . . . .
N6 N 0.6208(5) -0.0516(3) 0.31724(16) 0.0144(8) Uani 1 1 d . . . . .
N7 N 0.5741(5) -0.1499(3) 0.30901(16) 0.0147(8) Uani 1 1 d . . . . .
N8 N 0.5285(6) -0.2418(3) 0.30132(18) 0.0236(9) Uani 1 1 d . . . . .
N9 N 0.8594(5) 0.0965(3) 0.47313(15) 0.0117(7) Uani 1 1 d . . . . .
N10 N 0.8401(5) 0.1977(3) 0.48318(16) 0.0178(8) Uani 1 1 d . . . . .
N11 N 0.8249(6) 0.2906(3) 0.49215(19) 0.0331(10) Uani 1 1 d . . . . .
N12 N 0.6274(5) -0.0833(3) 0.46023(15) 0.0133(7) Uani 1 1 d . . . . .
N13 N 0.6450(5) -0.1852(3) 0.45280(15) 0.0143(7) Uani 1 1 d . . . . .
N14 N 0.6579(6) -0.2796(3) 0.44694(18) 0.0295(9) Uani 1 1 d . . . . .
N15 N 0.8996(5) 0.0850(3) 0.60550(17) 0.0182(8) Uani 1 1 d . . . . .
N16 N 0.8953(4) 0.0691(3) 0.66014(16) 0.0105(7) Uani 1 1 d . . . . .
N17 N 0.9034(5) 0.0579(3) 0.71355(17) 0.0171(8) Uani 1 1 d . . . . .
N18 N 0.6255(5) -0.1189(3) 0.59046(16) 0.0130(7) Uani 1 1 d . . . . .
N19 N 0.6995(5) -0.1668(3) 0.63649(16) 0.0116(7) Uani 1 1 d . . . . .
N20 N 0.7585(5) -0.2166(3) 0.68095(17) 0.0203(8) Uani 1 1 d . . . . .
Cu1 Cu 0.76150(7) 0.04908(4) 0.25829(2) 0.01243(15) Uani 1 1 d . . . . .
Cu2 Cu 0.70046(7) 0.02857(4) 0.39752(2) 0.01030(15) Uani 1 1 d . . . . .
Cu3 Cu 0.76554(7) -0.01033(4) 0.53864(2) 0.01106(15) 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 111.4(4) . .
N2 C2 C1 110.7(4) . .
N2 C2 C3 114.5(4) . .
C1 C2 C3 116.8(4) . .
C1 N1 Cu1 108.8(2) . .
C2 N2 Cu1 110.7(3) . .
N4 N3 Cu1 126.4(3) . .
N4 N3 Cu2 126.9(3) . .
Cu1 N3 Cu2 101.14(14) . .
N5 N4 N3 178.6(4) . .
N7 N6 Cu2 128.6(3) . .
N7 N6 Cu1 126.6(3) . .
Cu2 N6 Cu1 99.98(14) . .
N8 N7 N6 179.4(4) . .
N10 N9 Cu2 119.4(3) . .
N10 N9 Cu3 117.0(3) . .
Cu2 N9 Cu3 99.16(13) . .
N11 N10 N9 179.1(4) . .
N13 N12 Cu2 123.2(3) . .
N13 N12 Cu3 119.9(3) . .
Cu2 N12 Cu3 99.92(14) . .
N14 N13 N12 178.4(4) . .
N16 N15 Cu3 125.8(3) . .
N17 N16 N15 175.5(4) . .
N19 N18 Cu3 128.9(2) . .
N19 N18 Cu2 113.5(2) . 3_656
Cu3 N18 Cu2 101.22(13) . 3_656
N20 N19 N18 175.6(4) . .
N2 Cu1 N3 169.14(13) . .
N2 Cu1 N1 85.29(13) . .
N3 Cu1 N1 98.24(13) . .
N2 Cu1 N6 98.69(13) . .
N3 Cu1 N6 78.44(13) . .
N1 Cu1 N6 174.88(13) . .
N12 Cu2 N3 177.98(12) . .
N12 Cu2 N9 81.12(13) . .
N3 Cu2 N9 97.72(13) . .
N12 Cu2 N6 102.30(13) . .
N3 Cu2 N6 78.39(13) . .
N9 Cu2 N6 164.67(12) . .
N12 Cu2 N18 88.76(12) . 3_656
N3 Cu2 N18 93.00(12) . 3_656
N9 Cu2 N18 95.21(12) . 3_656
N6 Cu2 N18 99.78(12) . 3_656
N15 Cu3 N18 98.41(14) . .
N15 Cu3 N12 169.64(14) . .
N18 Cu3 N12 90.80(13) . .
N15 Cu3 N9 90.90(14) . .
N18 Cu3 N9 168.86(13) . .
N12 Cu3 N9 79.46(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.462(6) .
C1 N1 1.481(5) .
C2 N2 1.461(6) .
C2 C3 1.503(6) .
N1 Cu1 1.992(3) .
N2 Cu1 1.984(3) .
N3 N4 1.214(4) .
N3 Cu1 1.989(3) .
N3 Cu2 2.002(3) .
N4 N5 1.153(5) .
N6 N7 1.224(4) .
N6 Cu2 2.007(3) .
N6 Cu1 2.017(3) .
N7 N8 1.147(4) .
N9 N10 1.241(5) .
N9 Cu2 2.005(3) .
N9 Cu3 2.038(3) .
N10 N11 1.136(5) .
N12 N13 1.239(4) .
N12 Cu2 1.992(3) .
N12 Cu3 2.029(3) .
N13 N14 1.143(5) .
N15 N16 1.200(5) .
N15 Cu3 1.968(3) .
N16 N17 1.160(5) .
N18 N19 1.204(5) .
N18 Cu3 1.976(3) .
N18 Cu2 2.344(3) 3_656
N19 N20 1.162(5) .
Cu2 N18 2.344(3) 3_656
