#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:48:11 +0300 (Fri, 06 May 2016) $
#$Revision: 182640 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/45/7224573.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_7224573
loop_
_publ_author_name
'Chen, Chun-Hong'
'Mu, Rong'
'Zhang, Li'
'Xu, Guan-Cheng'
_publ_section_title
;
 Synthesis, crystal structure and disorder--order phase transition of a
 new diamine templated metal sulfate, (C3H12N2)2[Cu(H2O)4(SO4)2](HSO4)2
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2719
_journal_paper_doi               10.1039/C5CE02442K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C6 H34 Cu N4 O20 S4'
_chemical_formula_weight         674.15
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_audit_update_record
;
2015-12-12 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                111.230(2)
_cell_angle_beta                 107.301(2)
_cell_angle_gamma                104.268(2)
_cell_formula_units_Z            1
_cell_length_a                   8.044(2)
_cell_length_b                   9.357(2)
_cell_length_c                   9.822(2)
_cell_measurement_reflns_used    4811
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5110
_cell_measurement_theta_min      2.4615
_cell_volume                     603.6(2)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4836
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  0.7745
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             351
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2140
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.939
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0321
_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)+(0.0590P)²+0.5303P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                2103
_reflns_number_total             2140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02442k2.cif
_cod_data_source_block           qq
_cod_depositor_comments
'Adding full bibliography for 7224573--7224574.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7224573
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.5000 0.0000 0.0160(3) Uani 1 2 d S . .
S1 S 0.73704(14) 0.26460(12) -0.01734(13) 0.0204(3) Uani 1 1 d . . .
S2 S 0.28998(14) 0.25136(12) 0.36885(12) 0.0186(3) Uani 1 1 d . . .
O1 O 0.9012(5) 0.3160(5) -0.0507(5) 0.0413(9) Uani 1 1 d . . .
O2 O 0.7932(5) 0.3307(4) 0.1573(4) 0.0371(9) Uani 1 1 d . . .
O3 O 0.6460(4) 0.0796(4) -0.0979(4) 0.0267(7) Uani 1 1 d . . .
O4 O 0.5961(4) 0.3257(4) -0.0868(4) 0.0259(7) Uani 1 1 d . . .
O5 O 0.6664(4) 0.5702(4) 0.2219(4) 0.0227(7) Uani 1 1 d D . .
H5B H 0.703(9) 0.494(6) 0.230(8) 0.049(18) Uiso 1 1 d D . .
H5A H 0.630(8) 0.611(7) 0.296(5) 0.037(15) Uiso 1 1 d D . .
O6 O 0.7476(5) 0.7156(4) -0.0016(4) 0.0279(7) Uani 1 1 d D . .
H6B H 0.857(5) 0.710(8) 0.018(8) 0.049(18) Uiso 1 1 d D . .
H6A H 0.706(10) 0.708(9) -0.097(4) 0.06(2) Uiso 1 1 d D . .
O7 O 0.4163(5) 0.3235(5) 0.3110(4) 0.0345(8) Uani 1 1 d . . .
O8 O 0.3938(5) 0.2536(4) 0.5196(4) 0.0289(7) Uani 1 1 d . . .
O9 O 0.1696(5) 0.0638(4) 0.2402(4) 0.0340(8) Uani 1 1 d D . .
H9A H 0.2348 0.0258 0.1999 0.051 Uiso 1 1 calc RD . .
O10 O 0.1483(5) 0.3190(4) 0.3787(4) 0.0330(8) Uani 1 1 d . . .
N1 N 0.7571(6) 0.0306(5) 0.2076(5) 0.0268(8) Uani 1 1 d D A .
N2 N 0.8006(6) 0.4029(5) 0.6872(6) 0.0354(10) Uani 1 1 d D . .
H2WC H 0.680(3) 0.379(8) 0.656(7) 0.043(17) Uiso 1 1 d D . .
H2WB H 0.839(9) 0.402(8) 0.778(4) 0.040(17) Uiso 1 1 d D . .
H2WA H 0.855(10) 0.506(4) 0.709(9) 0.06(2) Uiso 1 1 d D . .
C1 C 0.8114(8) 0.0307(7) 0.3648(6) 0.0383(12) Uani 1 1 d DU . .
H1A H 0.7652 -0.0851 0.3422 0.046 Uiso 0.688(14) 1 calc PR A 1
H1B H 0.9489 0.0740 0.4161 0.046 Uiso 0.688(14) 1 calc PR A 1
H1C H 0.9398 0.0377 0.4102 0.046 Uiso 0.312(14) 1 d PR A 2
H1D H 0.7223 -0.0623 0.3626 0.046 Uiso 0.312(14) 1 d PR A 2
C2 C 0.7524(10) 0.1209(8) 0.4862(8) 0.0260(18) Uani 0.688(14) 1 d PDU A 1
H2A H 0.7918 0.0992 0.5775 0.031 Uiso 0.688(14) 1 calc PR A 1
H2B H 0.6152 0.0826 0.4396 0.031 Uiso 0.688(14) 1 calc PR A 1
C2' C 0.789(2) 0.2071(19) 0.4505(17) 0.027(4) Uani 0.312(14) 1 d PDU A 2
H2AA H 0.8797 0.2963 0.4492 0.032 Uiso 0.312(14) 1 calc PR A 2
H2AB H 0.6623 0.1967 0.3923 0.032 Uiso 0.312(14) 1 calc PR A 2
C3 C 0.8411(10) 0.3040(9) 0.5414(9) 0.0264(19) Uani 0.688(14) 1 d PDU A 1
H3A H 0.7890 0.3275 0.4532 0.032 Uiso 0.688(14) 1 calc PR A 1
H3B H 0.9769 0.3394 0.5749 0.032 Uiso 0.688(14) 1 calc PR A 1
C3' C 0.826(2) 0.2459(16) 0.6224(16) 0.029(4) Uani 0.312(14) 1 d PDU A 2
H3AA H 0.7356 0.1580 0.6255 0.034 Uiso 0.312(14) 1 calc PR A 2
H3AB H 0.9533 0.2597 0.6828 0.034 Uiso 0.312(14) 1 calc PR A 2
H1WC H 0.637(3) 0.009(8) 0.160(7) 0.047(18) Uiso 1 1 d D . .
H1WB H 0.822(9) 0.127(5) 0.219(9) 0.07(2) Uiso 1 1 d D . .
H1WA H 0.774(9) -0.050(6) 0.141(6) 0.045(17) Uiso 1 1 d 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'
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
O5 Cu1 O5 180.00(18) 2_665 .
O5 Cu1 O4 92.25(12) 2_665 2_665
O5 Cu1 O4 87.75(12) . 2_665
O5 Cu1 O4 87.75(12) 2_665 .
O5 Cu1 O4 92.25(12) . .
O4 Cu1 O4 180.0 2_665 .
O1 S1 O2 111.2(2) . .
O1 S1 O3 109.3(2) . .
O2 S1 O3 109.3(2) . .
O1 S1 O4 108.9(2) . .
O2 S1 O4 110.07(19) . .
O3 S1 O4 107.91(19) . .
O10 S2 O7 114.6(2) . .
O10 S2 O8 111.8(2) . .
O7 S2 O8 111.9(2) . .
O10 S2 O9 103.3(2) . .
O7 S2 O9 107.6(2) . .
O8 S2 O9 106.8(2) . .
S1 O4 Cu1 136.24(19) . .
Cu1 O5 H5B 112(4) . .
Cu1 O5 H5A 118(4) . .
H5B O5 H5A 110(6) . .
H6B O6 H6A 106(6) . .
S2 O9 H9A 109.5 . .
C1 N1 H1WC 113(4) . .
C1 N1 H1WB 111(5) . .
H1WC N1 H1WB 108(7) . .
C1 N1 H1WA 110(4) . .
H1WC N1 H1WA 104(6) . .
H1WB N1 H1WA 111(7) . .
C3' N2 C3 43.5(6) . .
C3' N2 H2WC 108(4) . .
C3 N2 H2WC 110(4) . .
C3' N2 H2WB 86(4) . .
C3 N2 H2WB 124(4) . .
H2WC N2 H2WB 105(6) . .
C3' N2 H2WA 138(5) . .
C3 N2 H2WA 103(5) . .
H2WC N2 H2WA 107(7) . .
H2WB N2 H2WA 106(7) . .
C2 C1 N1 121.5(5) . .
C2 C1 C2' 37.2(6) . .
N1 C1 C2' 92.2(6) . .
C2 C1 H1A 106.9 . .
N1 C1 H1A 106.9 . .
C2' C1 H1A 142.4 . .
C2 C1 H1B 106.9 . .
N1 C1 H1B 106.9 . .
C2' C1 H1B 97.7 . .
H1A C1 H1B 106.7 . .
C2 C1 H1C 113.9 . .
N1 C1 H1C 113.2 . .
C2' C1 H1C 113.7 . .
H1A C1 H1C 88.4 . .
H1B C1 H1C 18.3 . .
C2 C1 H1D 79.5 . .
N1 C1 H1D 113.3 . .
C2' C1 H1D 112.8 . .
H1A C1 H1D 29.9 . .
H1B C1 H1D 127.4 . .
H1C C1 H1D 110.6 . .
C1 C2 C3 109.2(5) . .
C1 C2 H2A 109.8 . .
C3 C2 H2A 109.8 . .
C1 C2 H2B 109.8 . .
C3 C2 H2B 109.8 . .
H2A C2 H2B 108.3 . .
C3' C2' C1 107.9(9) . .
C3' C2' H2AA 110.1 . .
C1 C2' H2AA 110.1 . .
C3' C2' H2AB 110.1 . .
C1 C2' H2AB 110.1 . .
H2AA C2' H2AB 108.4 . .
C2 C3 N2 109.4(5) . .
C2 C3 H3A 109.8 . .
N2 C3 H3A 109.8 . .
C2 C3 H3B 109.8 . .
N2 C3 H3B 109.8 . .
H3A C3 H3B 108.2 . .
N2 C3' C2' 103.7(10) . .
N2 C3' H3AA 111.0 . .
C2' C3' H3AA 111.0 . .
N2 C3' H3AB 111.0 . .
C2' C3' H3AB 111.0 . .
H3AA C3' H3AB 109.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.941(3) 2_665
Cu1 O5 1.941(3) .
Cu1 O4 1.997(3) 2_665
Cu1 O4 1.997(3) .
S1 O1 1.463(4) .
S1 O2 1.471(4) .
S1 O3 1.482(3) .
S1 O4 1.490(3) .
S2 O10 1.444(3) .
S2 O7 1.447(3) .
S2 O8 1.458(3) .
S2 O9 1.563(3) .
O5 H5B 0.862(18) .
O5 H5A 0.864(18) .
O6 H6B 0.862(18) .
O6 H6A 0.863(18) .
O9 H9A 0.8200 .
N1 C1 1.474(7) .
N1 H1WC 0.872(18) .
N1 H1WB 0.869(18) .
N1 H1WA 0.872(18) .
N2 C3' 1.465(12) .
N2 C3 1.574(8) .
N2 H2WC 0.869(18) .
N2 H2WB 0.858(18) .
N2 H2WA 0.866(19) .
C1 C2 1.471(8) .
C1 C2' 1.641(13) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 C3 1.494(9) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2' C3' 1.509(14) .
C2' H2AA 0.9700 .
C2' H2AB 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3' H3AA 0.9700 .
C3' H3AB 0.9700 .
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
O1 S1 O4 Cu1 -109.4(3) .
O2 S1 O4 Cu1 12.7(4) .
O3 S1 O4 Cu1 132.0(3) .
O5 Cu1 O4 S1 -179.3(3) 2_665
O5 Cu1 O4 S1 0.7(3) .
O4 Cu1 O4 S1 2(100) 2_665
N1 C1 C2 C3 -64.3(7) .
C2' C1 C2 C3 -21.4(9) .
C2 C1 C2' C3' 32.3(9) .
N1 C1 C2' C3' 176.8(10) .
C1 C2 C3 N2 -172.6(5) .
C3' N2 C3 C2 30.1(10) .
C3 N2 C3' C2' -19.8(7) .
C1 C2' C3' N2 -179.4(9) .
