#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:46:51 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230259 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/69/7056925.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_7056925
loop_
_publ_author_name
'Thakur, Neha'
'Pandey, Mrituanjay D.'
'Pandey, Rampal'
_publ_section_title
;
 A uniquely fabricated Cu(ii)-metallacycle as a reusable highly sensitive
 dual-channel and practically functional metalloreceptor for Fe3+ and Ca2+
 ions: an inorganic site of cation detection
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3582
_journal_paper_doi               10.1039/C7NJ03294C
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C10 H14 Cu N2 O7 S2'
_chemical_formula_weight         401.89
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-22 deposited with the CCDC.
2018-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.533(13)
_cell_angle_beta                 80.57(3)
_cell_angle_gamma                81.58(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2021(13)
_cell_length_b                   9.469(3)
_cell_length_c                   11.699(3)
_cell_measurement_reflns_used    340
_cell_measurement_temperature    277(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.11
_cell_volume                     719.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      277(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku ip'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1215
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_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            5282
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.7190
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1289P)²+0.2290P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                2042
_reflns_number_total             2440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj03294c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7056923--7056926.cif.'
_cod_database_code               7056925
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.77626(9) 0.05293(6) 0.16456(5) 0.0250(3) Uani 1 1 d .
S2 S 1.14149(19) -0.15716(14) 0.13232(12) 0.0254(4) Uani 1 1 d .
S1 S 0.7266(2) 0.35776(16) 0.23147(15) 0.0370(4) Uani 1 1 d .
O5 O 0.6531(6) -0.1817(5) 0.2322(4) 0.0429(11) Uani 1 1 d .
H5A H 0.7369 -0.2494 0.2262 0.052 Uiso 1 1 d R
H5B H 0.5592 -0.1710 0.1939 0.052 Uiso 1 1 d R
O1 O 1.0276(5) -0.0528(4) 0.1908(3) 0.0292(9) Uani 1 1 d .
O4 O 1.2185(6) -0.0564(4) 0.0039(4) 0.0364(10) Uani 1 1 d .
O2 O 1.2996(6) -0.2327(5) 0.2056(4) 0.0399(11) Uani 1 1 d .
O3 O 1.0246(6) -0.2680(4) 0.1298(4) 0.0395(10) Uani 1 1 d .
N1 N 0.7623(7) 0.0473(5) 0.3387(4) 0.0280(10) Uani 1 1 d .
N2 N 0.5479(6) 0.2070(5) 0.1358(4) 0.0248(9) Uani 1 1 d .
C6 C 0.5339(8) 0.3307(5) 0.1686(5) 0.0250(11) Uani 1 1 d .
C5 C 0.7413(8) 0.1780(6) 0.3617(5) 0.0304(12) Uani 1 1 d .
C7 C 0.3809(9) 0.4358(6) 0.1497(5) 0.0322(13) Uani 1 1 d .
H7 H 0.3747 0.5199 0.1727 0.039 Uiso 1 1 calc R
C4 C 0.7345(10) 0.1771(8) 0.4806(6) 0.0440(16) Uani 1 1 d .
H4 H 0.7190 0.2695 0.4928 0.053 Uiso 1 1 calc R
C9 C 0.2458(9) 0.2892(6) 0.0642(6) 0.0348(13) Uani 1 1 d .
H9 H 0.1481 0.2725 0.0292 0.042 Uiso 1 1 calc R
C2 C 0.7694(10) -0.0968(8) 0.5594(6) 0.0448(16) Uani 1 1 d .
H2 H 0.7790 -0.1925 0.6256 0.054 Uiso 1 1 calc R
C1 C 0.7740(9) -0.0894(7) 0.4376(6) 0.0383(14) Uani 1 1 d .
H1 H 0.7853 -0.1808 0.4239 0.046 Uiso 1 1 calc R
C8 C 0.2331(8) 0.4166(6) 0.0955(6) 0.0360(14) Uani 1 1 d .
H8 H 0.1278 0.4883 0.0806 0.043 Uiso 1 1 calc R
C10 C 0.4041(9) 0.1883(6) 0.0854(5) 0.0337(13) Uani 1 1 d .
H10 H 0.4124 0.1028 0.0639 0.040 Uiso 1 1 calc R
C3 C 0.7509(10) 0.0364(8) 0.5823(5) 0.0452(16) Uani 1 1 d .
H3 H 0.7493 0.0327 0.6631 0.054 Uiso 1 1 calc R
O6 O 0.3386(19) 0.4855(11) 0.4559(11) 0.173(5) Uani 1 1 d .
H6A H 0.2540 0.4979 0.5066 0.207 Uiso 1 1 d R
H6B H 0.4065 0.4017 0.4978 0.207 Uiso 1 1 d R
O7 O 0.035(3) 0.4823(17) 0.3806(15) 0.269(10) Uani 1 1 d .
H7A H 0.1398 0.5215 0.3497 0.323 Uiso 1 1 d R
H7B H -0.0459 0.5463 0.3231 0.323 Uiso 1 1 d 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'
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'
S S 0.1246 0.1234 '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
O1 Cu1 O4 95.45(17) . 2_755
O1 Cu1 N1 85.90(17) . .
O4 Cu1 N1 178.13(18) 2_755 .
O1 Cu1 N2 165.64(17) . .
O4 Cu1 N2 89.58(17) 2_755 .
N1 Cu1 N2 89.41(18) . .
O1 Cu1 O5 89.93(16) . .
O4 Cu1 O5 85.35(17) 2_755 .
N1 Cu1 O5 93.36(17) . .
N2 Cu1 O5 103.90(17) . .
O3 S2 O2 112.0(2) . .
O3 S2 O4 111.9(3) . .
O2 S2 O4 108.4(3) . .
O3 S2 O1 110.3(2) . .
O2 S2 O1 107.3(2) . .
O4 S2 O1 106.8(2) . .
C6 S1 C5 99.3(2) . .
Cu1 O5 H5A 110.5 . .
Cu1 O5 H5B 109.0 . .
H5A O5 H5B 114.9 . .
S2 O1 Cu1 130.1(2) . .
S2 O4 Cu1 135.3(3) . 2_755
C5 N1 C1 117.9(5) . .
C5 N1 Cu1 121.8(4) . .
C1 N1 Cu1 120.3(4) . .
C10 N2 C6 118.4(5) . .
C10 N2 Cu1 120.4(4) . .
C6 N2 Cu1 121.2(4) . .
C7 C6 N2 121.9(5) . .
C7 C6 S1 119.8(4) . .
N2 C6 S1 118.2(4) . .
N1 C5 C4 122.8(5) . .
N1 C5 S1 117.8(4) . .
C4 C5 S1 119.4(4) . .
C6 C7 C8 119.3(5) . .
C6 C7 H7 120.3 . .
C8 C7 H7 120.3 . .
C5 C4 C3 119.4(6) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C10 C9 C8 118.8(5) . .
C10 C9 H9 120.6 . .
C8 C9 H9 120.6 . .
C3 C2 C1 120.4(6) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
N1 C1 C2 121.6(6) . .
N1 C1 H1 119.2 . .
C2 C1 H1 119.2 . .
C9 C8 C7 118.8(5) . .
C9 C8 H8 120.6 . .
C7 C8 H8 120.6 . .
N2 C10 C9 122.8(5) . .
N2 C10 H10 118.6 . .
C9 C10 H10 118.6 . .
C2 C3 C4 117.9(5) . .
C2 C3 H3 121.1 . .
C4 C3 H3 121.1 . .
H6A O6 H6B 105.3 . .
H7A O7 H7B 102.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.944(4) .
Cu1 O4 1.952(4) 2_755
Cu1 N1 2.003(5) .
Cu1 N2 2.009(4) .
Cu1 O5 2.301(4) .
S2 O3 1.450(4) .
S2 O2 1.461(4) .
S2 O4 1.489(4) .
S2 O1 1.495(4) .
S1 C6 1.767(6) .
S1 C5 1.779(6) .
O5 H5A 0.8298 .
O5 H5B 0.8433 .
O4 Cu1 1.952(4) 2_755
N1 C5 1.350(7) .
N1 C1 1.352(7) .
N2 C10 1.338(7) .
N2 C6 1.356(6) .
C6 C7 1.355(8) .
C5 C4 1.380(9) .
C7 C8 1.392(8) .
C7 H7 0.9300 .
C4 C3 1.393(9) .
C4 H4 0.9300 .
C9 C10 1.364(8) .
C9 C8 1.381(8) .
C9 H9 0.9300 .
C2 C3 1.374(10) .
C2 C1 1.394(9) .
C2 H2 0.9300 .
C1 H1 0.9300 .
C8 H8 0.9300 .
C10 H10 0.9300 .
C3 H3 0.9300 .
O6 H6A 0.8086 .
O6 H6B 0.8745 .
O7 H7A 0.8500 .
O7 H7B 0.9277 .
