#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/44/2214461.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214461
loop_
_publ_author_name
'Wen-Li Zhang'
'Jian-Fang Ma'
'Hui Jiang'
_publ_section_title
;
 Tetraamminediaquacopper(II) 4-amino-2,5-dichlorobenzenesulfonate
;
_journal_coeditor_code           XU2281
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2001
_journal_page_last               m2001
_journal_paper_doi               10.1107/S1600536807030711
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (H2 O)2 (N H3)4] (C6 H4 Cl2 N O3 S)2'
_chemical_formula_moiety         'Cu H16 N4 O2 2+ , 2C6 H4 Cl2 N O3 S -'
_chemical_formula_sum            'C12 H24 Cl4 Cu N6 O8 S2'
_chemical_formula_weight         649.83
_chemical_name_systematic
;
Tetraamminediaquacopper(II) 4-amino-2,5-dichlorobenzenesulfonate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL97
_cell_angle_alpha                96.22(4)
_cell_angle_beta                 94.62(4)
_cell_angle_gamma                118.33(3)
_cell_formula_units_Z            1
_cell_length_a                   7.367(6)
_cell_length_b                   7.380(5)
_cell_length_c                   12.689(10)
_cell_measurement_reflns_used    5673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     596.8(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotor target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5849
_diffrn_reflns_theta_full        25.2
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             331
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0461P)²+0.1532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.076
_refine_ls_wR_factor_ref         0.076
_reflns_number_gt                2518
_reflns_number_total             2715
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2281.cif
_cod_data_source_block           I
_cod_database_code               2214461
_cod_database_fobs_code          2214461
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu1 1.0000 0.0000 1.0000 0.02605(10) Uani d S 1
Cl Cl1 0.12744(6) 0.22744(8) 0.68358(3) 0.03803(12) Uani d . 1
Cl Cl2 0.80402(7) 0.27818(7) 0.40904(3) 0.03640(12) Uani d . 1
S S1 0.57643(6) 0.30274(6) 0.80181(3) 0.02445(11) Uani d . 1
C C1 0.5153(2) 0.2819(2) 0.66165(12) 0.0231(3) Uani d . 1
C C2 0.3236(2) 0.2471(2) 0.61119(13) 0.0248(3) Uani d . 1
C C3 0.2789(2) 0.2209(3) 0.50137(13) 0.0279(3) Uani d . 1
H H3 0.1496 0.1983 0.4704 0.033 Uiso calc R 1
C C4 0.4238(3) 0.2275(3) 0.43586(12) 0.0270(3) Uani d . 1
C C5 0.6171(2) 0.2647(2) 0.48716(13) 0.0256(3) Uani d . 1
C C6 0.6623(2) 0.2912(2) 0.59713(12) 0.0246(3) Uani d . 1
H H6 0.7921 0.3155 0.6284 0.030 Uiso calc R 1
N N1 0.3790(3) 0.1971(3) 0.32678(12) 0.0384(4) Uani d . 1
H H1N 0.2620 0.1798 0.2962 0.058 Uiso d R 1
H H2N 0.4689 0.2039 0.2910 0.058 Uiso d R 1
O O1 0.4554(2) 0.0939(2) 0.82788(10) 0.0357(3) Uani d . 1
O O2 0.79984(18) 0.3761(2) 0.82209(10) 0.0357(3) Uani d . 1
O O1W 1.0063(2) -0.1798(2) 0.81528(12) 0.0445(3) Uani d . 1
H H1A 0.9705 -0.3136 0.8054 0.067 Uiso d R 1
H H1B 1.1262 -0.1150 0.8014 0.067 Uiso d R 1
N N2 0.6962(2) -0.0932(2) 0.95054(12) 0.0317(3) Uani d . 1
H H2A 0.6650 -0.0215 0.9104 0.048 Uiso d R 1
H H2B 0.6300 -0.1033 1.0089 0.048 Uiso d R 1
H H2C 0.6394 -0.2209 0.9211 0.048 Uiso d R 1
O O3 0.5222(2) 0.4502(2) 0.85509(10) 0.0362(3) Uani d . 1
N N3 1.0992(2) 0.2790(2) 0.95026(11) 0.0314(3) Uani d . 1
H H3A 1.0038 0.2791 0.9115 0.047 Uiso d R 1
H H3B 1.1447 0.3759 1.0025 0.047 Uiso d R 1
H H3C 1.1979 0.3035 0.9140 0.047 Uiso d R 1
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'
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Cu1 N2 . 2_757 180.0000(10)
N2 Cu1 N3 . . 92.99(7)
N2 Cu1 N3 2_757 . 87.01(7)
N2 Cu1 N3 . 2_757 87.01(7)
N2 Cu1 N3 2_757 2_757 92.99(7)
N3 Cu1 N3 . 2_757 180.0000(10)
O3 S1 O2 . . 112.05(9)
O3 S1 O1 . . 112.11(10)
O2 S1 O1 . . 111.67(9)
O3 S1 C1 . . 108.15(8)
O2 S1 C1 . . 105.56(8)
O1 S1 C1 . . 106.89(9)
C6 C1 C2 . . 117.67(15)
C6 C1 S1 . . 118.57(12)
C2 C1 S1 . . 123.70(12)
C3 C2 C1 . . 121.70(15)
C3 C2 Cl1 . . 116.75(13)
C1 C2 Cl1 . . 121.53(13)
C2 C3 C4 . . 121.18(15)
C2 C3 H3 . . 119.4
C4 C3 H3 . . 119.4
N1 C4 C3 . . 121.51(16)
N1 C4 C5 . . 121.65(16)
C3 C4 C5 . . 116.84(15)
C6 C5 C4 . . 122.08(15)
C6 C5 Cl2 . . 119.39(13)
C4 C5 Cl2 . . 118.53(14)
C5 C6 C1 . . 120.52(15)
C5 C6 H6 . . 119.7
C1 C6 H6 . . 119.7
C4 N1 H1N . . 120.9
C4 N1 H2N . . 118.6
H1N N1 H2N . . 120.3
H1A O1W H1B . . 107.3
Cu1 N2 H2A . . 119.1
Cu1 N2 H2B . . 109.0
H2A N2 H2B . . 108.1
Cu1 N2 H2C . . 106.8
H2A N2 H2C . . 111.0
H2B N2 H2C . . 101.4
Cu1 N3 H3A . . 110.6
Cu1 N3 H3B . . 110.9
H3A N3 H3B . . 109.9
Cu1 N3 H3C . . 110.4
H3A N3 H3C . . 107.6
H3B N3 H3C . . 107.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N2 . 2.024(2) y
Cu1 N2 2_757 2.024(2) ?
Cu1 N3 . 2.025(2) y
Cu1 N3 2_757 2.025(2) ?
Cu1 O1W . 2.580(2) y
Cl1 C2 . 1.731(2) ?
Cl2 C5 . 1.732(2) ?
S1 O3 . 1.4482(15) ?
S1 O2 . 1.4574(17) ?
S1 O1 . 1.4608(17) ?
S1 C1 . 1.771(2) ?
C1 C6 . 1.390(2) ?
C1 C2 . 1.395(2) ?
C2 C3 . 1.377(2) ?
C3 C4 . 1.391(3) ?
C3 H3 . 0.9300 ?
C4 N1 . 1.365(2) ?
C4 C5 . 1.403(3) ?
C5 C6 . 1.379(2) ?
C6 H6 . 0.9300 ?
N1 H1N . 0.8605 ?
N1 H2N . 0.8179 ?
O1W H1A . 0.8836 ?
O1W H1B . 0.8260 ?
N2 H2A . 0.8642 ?
N2 H2B . 0.9089 ?
N2 H2C . 0.8531 ?
N3 H3A . 0.8251 ?
N3 H3B . 0.8346 ?
N3 H3C . 0.8488 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1A O2 1_545 0.88 2.07 2.900(3) 156
O1W H1B O1 1_655 0.83 2.14 2.925(3) 159
N1 H1N O1W 2_656 0.86 2.34 3.179(4) 166
N1 H2N Cl2 . 0.82 2.56 2.967(3) 112
N2 H2A O1 . 0.86 2.32 3.134(3) 157
N2 H2B O1 2_657 0.91 2.22 3.108(3) 166
N2 H2C O3 1_545 0.85 2.19 3.038(3) 174
N3 H3A O2 . 0.82 2.23 3.033(3) 164
N3 H3B O2 2_767 0.84 2.59 3.412(3) 166
N3 H3B O3 2_767 0.84 2.59 3.226(3) 133
N3 H3C O3 1_655 0.85 2.33 3.157(3) 164
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
O3 S1 C1 C6 133.25(13)
O2 S1 C1 C6 13.16(15)
O1 S1 C1 C6 -105.86(14)
O3 S1 C1 C2 -49.74(16)
O2 S1 C1 C2 -169.83(14)
O1 S1 C1 C2 71.15(16)
C6 C1 C2 C3 0.6(2)
S1 C1 C2 C3 -176.48(13)
C6 C1 C2 Cl1 178.68(12)
S1 C1 C2 Cl1 1.6(2)
C1 C2 C3 C4 0.2(3)
Cl1 C2 C3 C4 -178.05(13)
C2 C3 C4 N1 178.56(16)
C2 C3 C4 C5 -0.8(2)
N1 C4 C5 C6 -178.61(16)
C3 C4 C5 C6 0.7(2)
N1 C4 C5 Cl2 1.6(2)
C3 C4 C5 Cl2 -179.06(12)
C4 C5 C6 C1 0.0(3)
Cl2 C5 C6 C1 179.77(12)
C2 C1 C6 C5 -0.6(2)
S1 C1 C6 C5 176.58(13)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139072590
