#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:48:11 +0300 (Fri, 06 May 2016) $
#$Revision: 182640 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/45/7224574.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_7224574
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
;
2016-01-20 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                94.771(4)
_cell_angle_beta                 100.757(4)
_cell_angle_gamma                95.748(4)
_cell_formula_units_Z            2
_cell_length_a                   10.649(4)
_cell_length_b                   10.677(4)
_cell_length_c                   10.799(4)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5142
_cell_measurement_theta_min      2.4661
_cell_volume                     1193.7(8)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9604
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.7724
_exptl_absorpt_correction_T_min  0.7538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.311
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0261
_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)+(0.0486P)²+0.7849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3991
_reflns_number_total             4242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02442k2.cif
_cod_data_source_block           ee
_cod_depositor_comments
'Adding full bibliography for 7224573--7224574.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7224574
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 0.5000 0.0000 0.5000 0.00713(10) Uani 1 2 d S
N1 N 0.45721(15) 0.29984(14) 0.26695(14) 0.0112(3) Uani 1 1 d .
H10 H 0.4520 0.3802 0.2529 0.013 Uiso 1 1 d R
H11 H 0.3810 0.2541 0.2391 0.013 Uiso 1 1 d R
H12 H 0.4840 0.2935 0.3493 0.013 Uiso 1 1 d R
N2 N 0.56125(15) 0.23989(14) -0.15662(14) 0.0123(3) Uani 1 1 d .
H7 H 0.4862 0.1936 -0.1833 0.015 Uiso 1 1 d R
H8 H 0.6135 0.2140 -0.2052 0.015 Uiso 1 1 d R
H9 H 0.5532 0.3202 -0.1664 0.015 Uiso 1 1 d R
N3 N -0.02366(14) 0.77968(14) 0.75525(14) 0.0102(3) Uani 1 1 d .
H4 H -0.0318 0.8560 0.7301 0.012 Uiso 1 1 d R
H5 H -0.0954 0.7280 0.7256 0.012 Uiso 1 1 d R
H6 H -0.0085 0.7866 0.8397 0.012 Uiso 1 1 d R
N4 N 0.03034(15) 0.76836(14) 0.35880(14) 0.0106(3) Uani 1 1 d .
H1 H -0.0292 0.7056 0.3277 0.013 Uiso 1 1 d R
H2 H 0.0146 0.8336 0.3191 0.013 Uiso 1 1 d R
H3 H 0.1027 0.7456 0.3444 0.013 Uiso 1 1 d R
C1 C 0.55321(18) 0.25483(17) 0.19516(17) 0.0125(4) Uani 1 1 d .
H1A H 0.5578 0.1634 0.2018 0.015 Uiso 1 1 calc R
H1B H 0.6394 0.3009 0.2313 0.015 Uiso 1 1 calc R
C2 C 0.51390(17) 0.27757(17) 0.05713(17) 0.0127(4) Uani 1 1 d .
H2A H 0.5160 0.3696 0.0503 0.015 Uiso 1 1 calc R
H2B H 0.4248 0.2375 0.0234 0.015 Uiso 1 1 calc R
C3 C 0.60440(18) 0.22274(18) -0.02064(17) 0.0144(4) Uani 1 1 d .
H3A H 0.6929 0.2658 0.0102 0.017 Uiso 1 1 calc R
H3B H 0.6056 0.1315 -0.0107 0.017 Uiso 1 1 calc R
C4 C 0.08939(17) 0.72891(17) 0.71398(17) 0.0118(4) Uani 1 1 d .
H4A H 0.1093 0.6537 0.7584 0.014 Uiso 1 1 calc R
H4B H 0.1653 0.7938 0.7384 0.014 Uiso 1 1 calc R
C5 C 0.06482(18) 0.69234(17) 0.57168(17) 0.0127(4) Uani 1 1 d .
H5D H -0.0087 0.6248 0.5480 0.015 Uiso 1 1 calc R
H5C H 0.1415 0.6578 0.5493 0.015 Uiso 1 1 calc R
C6 C 0.03577(18) 0.80361(17) 0.49606(16) 0.0117(4) Uani 1 1 d .
H6D H -0.0477 0.8307 0.5084 0.014 Uiso 1 1 calc R
H6C H 0.1034 0.8757 0.5273 0.014 Uiso 1 1 calc R
Cu2 Cu 0.0000 0.5000 0.0000 0.00763(10) Uani 1 2 d S
S1 S 0.26229(4) 0.00328(4) 0.26449(4) 0.00717(12) Uani 1 1 d .
S2 S 0.30246(4) 0.40643(4) 0.67437(4) 0.00819(12) Uani 1 1 d .
S3 S 0.22142(4) 0.51835(4) 0.25399(4) 0.00729(12) Uani 1 1 d .
S4 S 0.20695(4) 0.07815(4) 0.83765(4) 0.00771(12) Uani 1 1 d .
O1 O 0.25360(12) 0.09839(12) 0.17092(12) 0.0119(3) Uani 1 1 d .
O2 O 0.21461(12) -0.12314(12) 0.19882(12) 0.0125(3) Uani 1 1 d .
O3 O 0.18783(12) 0.03712(12) 0.36192(12) 0.0126(3) Uani 1 1 d .
O4 O 0.40170(12) 0.00550(12) 0.32427(12) 0.0116(3) Uani 1 1 d .
O5 O 0.51689(12) 0.23087(12) 0.52049(12) 0.0129(3) Uani 1 1 d .
H5B H 0.4559 0.2476 0.5564 0.019 Uiso 1 1 d R
H5A H 0.5866 0.2705 0.5626 0.019 Uiso 1 1 d R
O6 O 0.34334(12) -0.01169(12) 0.56933(12) 0.0109(3) Uani 1 1 d .
H6B H 0.3452 0.0179 0.6478 0.016 Uiso 1 1 d R
H6A H 0.2807 0.0165 0.5187 0.016 Uiso 1 1 d R
O7 O 0.17537(12) 0.43123(12) 0.69748(12) 0.0125(3) Uani 1 1 d .
O8 O 0.30113(13) 0.27782(12) 0.61703(13) 0.0164(3) Uani 1 1 d .
O9 O 0.33657(13) 0.49835(12) 0.57577(12) 0.0155(3) Uani 1 1 d .
H9A H 0.2964 0.4692 0.4964 0.023 Uiso 1 1 d R
O10 O 0.40347(13) 0.44421(12) 0.78446(13) 0.0153(3) Uani 1 1 d .
O11 O 0.22991(12) 0.41687(12) 0.34038(12) 0.0117(3) Uani 1 1 d .
O12 O 0.25407(12) 0.64240(12) 0.32920(12) 0.0125(3) Uani 1 1 d .
O13 O 0.31031(12) 0.50137(12) 0.16590(12) 0.0120(3) Uani 1 1 d .
O14 O 0.08574(12) 0.50712(12) 0.18180(12) 0.0116(3) Uani 1 1 d .
O15 O 0.01235(13) 0.73336(12) 0.01644(12) 0.0131(3) Uani 1 1 d .
H15B H -0.0565 0.7491 0.0462 0.020 Uiso 1 1 d R
H15A H 0.0813 0.7753 0.0647 0.020 Uiso 1 1 d R
O16 O 0.16304(12) 0.50816(12) -0.05779(12) 0.0110(3) Uani 1 1 d .
H16B H 0.1670 0.4725 -0.1301 0.016 Uiso 1 1 d R
H16A H 0.2247 0.4931 -0.0016 0.016 Uiso 1 1 d R
O17 O 0.20047(13) 0.20799(12) 0.88664(13) 0.0133(3) Uani 1 1 d .
O18 O 0.17492(13) -0.00921(12) 0.93999(12) 0.0145(3) Uani 1 1 d .
H18A H 0.2037 0.0285 1.0183 0.022 Uiso 1 1 d R
O19 O 0.33659(12) 0.05733(12) 0.81889(12) 0.0133(3) Uani 1 1 d .
O20 O 0.10934(12) 0.03184(12) 0.72629(12) 0.0130(3) 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'
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
O6 Cu1 O6 180.0 . 2_656
O6 Cu1 O4 92.25(6) . .
O6 Cu1 O4 87.75(6) 2_656 .
O6 Cu1 O4 87.75(6) . 2_656
O6 Cu1 O4 92.25(6) 2_656 2_656
O4 Cu1 O4 180.0 . 2_656
C1 N1 H10 106.3 . .
C1 N1 H11 110.1 . .
H10 N1 H11 110.1 . .
C1 N1 H12 109.5 . .
H10 N1 H12 110.8 . .
H11 N1 H12 110.1 . .
C3 N2 H7 107.4 . .
C3 N2 H8 113.5 . .
H7 N2 H8 107.1 . .
C3 N2 H9 110.8 . .
H7 N2 H9 109.9 . .
H8 N2 H9 108.1 . .
C4 N3 H4 110.1 . .
C4 N3 H5 111.2 . .
H4 N3 H5 110.4 . .
C4 N3 H6 107.5 . .
H4 N3 H6 108.5 . .
H5 N3 H6 109.1 . .
C6 N4 H1 112.0 . .
C6 N4 H2 108.3 . .
H1 N4 H2 109.4 . .
C6 N4 H3 111.9 . .
H1 N4 H3 107.1 . .
H2 N4 H3 108.1 . .
N1 C1 C2 109.31(14) . .
N1 C1 H1A 109.8 . .
C2 C1 H1A 109.8 . .
N1 C1 H1B 109.8 . .
C2 C1 H1B 109.8 . .
H1A C1 H1B 108.3 . .
C1 C2 C3 110.43(15) . .
C1 C2 H2A 109.6 . .
C3 C2 H2A 109.6 . .
C1 C2 H2B 109.6 . .
C3 C2 H2B 109.6 . .
H2A C2 H2B 108.1 . .
N2 C3 C2 109.98(15) . .
N2 C3 H3A 109.7 . .
C2 C3 H3A 109.7 . .
N2 C3 H3B 109.7 . .
C2 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
N3 C4 C5 112.09(15) . .
N3 C4 H4A 109.2 . .
C5 C4 H4A 109.2 . .
N3 C4 H4B 109.2 . .
C5 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
C4 C5 C6 112.56(15) . .
C4 C5 H5D 109.1 . .
C6 C5 H5D 109.1 . .
C4 C5 H5C 109.1 . .
C6 C5 H5C 109.1 . .
H5D C5 H5C 107.8 . .
N4 C6 C5 110.78(14) . .
N4 C6 H6D 109.5 . .
C5 C6 H6D 109.5 . .
N4 C6 H6C 109.5 . .
C5 C6 H6C 109.5 . .
H6D C6 H6C 108.1 . .
O16 Cu2 O16 180.0 2_565 .
O16 Cu2 O14 92.87(6) 2_565 2_565
O16 Cu2 O14 87.13(6) . 2_565
O16 Cu2 O14 87.13(6) 2_565 .
O16 Cu2 O14 92.87(6) . .
O14 Cu2 O14 180.0 2_565 .
O2 S1 O3 111.31(8) . .
O2 S1 O1 109.52(8) . .
O3 S1 O1 109.40(8) . .
O2 S1 O4 108.81(8) . .
O3 S1 O4 110.05(8) . .
O1 S1 O4 107.66(7) . .
O10 S2 O8 114.50(8) . .
O10 S2 O7 112.48(8) . .
O8 S2 O7 111.95(8) . .
O10 S2 O9 103.42(8) . .
O8 S2 O9 107.11(8) . .
O7 S2 O9 106.54(8) . .
O12 S3 O13 110.75(8) . .
O12 S3 O11 109.37(8) . .
O13 S3 O11 109.21(8) . .
O12 S3 O14 109.53(7) . .
O13 S3 O14 110.12(8) . .
O11 S3 O14 107.80(7) . .
O20 S4 O17 114.10(8) . .
O20 S4 O19 111.97(8) . .
O17 S4 O19 112.27(8) . .
O20 S4 O18 103.68(8) . .
O17 S4 O18 107.41(8) . .
O19 S4 O18 106.64(8) . .
S1 O4 Cu1 135.30(8) . .
H5B O5 H5A 109.3 . .
Cu1 O6 H6B 120.5 . .
Cu1 O6 H6A 110.8 . .
H6B O6 H6A 109.9 . .
S2 O9 H9A 111.6 . .
S3 O14 Cu2 136.03(8) . .
H15B O15 H15A 110.3 . .
Cu2 O16 H16B 120.3 . .
Cu2 O16 H16A 112.8 . .
H16B O16 H16A 111.2 . .
S4 O18 H18A 111.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O6 1.9492(14) .
Cu1 O6 1.9492(14) 2_656
Cu1 O4 1.9974(14) .
Cu1 O4 1.9974(14) 2_656
N1 C1 1.486(2) .
N1 H10 0.8886 .
N1 H11 0.8903 .
N1 H12 0.8923 .
N2 C3 1.487(2) .
N2 H7 0.8820 .
N2 H8 0.8812 .
N2 H9 0.8839 .
N3 C4 1.494(2) .
N3 H4 0.8873 .
N3 H5 0.8868 .
N3 H6 0.8913 .
N4 C6 1.488(2) .
N4 H1 0.8729 .
N4 H2 0.8620 .
N4 H3 0.8676 .
C1 C2 1.518(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.520(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.521(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.521(2) .
C5 H5D 0.9900 .
C5 H5C 0.9900 .
C6 H6D 0.9900 .
C6 H6C 0.9900 .
Cu2 O16 1.9480(14) 2_565
Cu2 O16 1.9480(14) .
Cu2 O14 1.9965(14) 2_565
Cu2 O14 1.9965(14) .
S1 O2 1.4669(13) .
S1 O3 1.4738(14) .
S1 O1 1.4884(13) .
S1 O4 1.5012(14) .
S2 O10 1.4454(14) .
S2 O8 1.4562(14) .
S2 O7 1.4666(14) .
S2 O9 1.5734(14) .
S3 O12 1.4691(13) .
S3 O13 1.4751(14) .
S3 O11 1.4862(13) .
S3 O14 1.4963(14) .
S4 O20 1.4500(14) .
S4 O17 1.4550(14) .
S4 O19 1.4679(14) .
S4 O18 1.5672(14) .
O5 H5B 0.8426 .
O5 H5A 0.8457 .
O6 H6B 0.8757 .
O6 H6A 0.8747 .
O9 H9A 0.8983 .
O15 H15B 0.8789 .
O15 H15A 0.8739 .
O16 H16B 0.8503 .
O16 H16A 0.8445 .
O18 H18A 0.8904 .
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
N1 C1 C2 C3 -175.41(14) .
C1 C2 C3 N2 177.21(15) .
N3 C4 C5 C6 59.9(2) .
C4 C5 C6 N4 172.15(15) .
O2 S1 O4 Cu1 -103.63(12) .
O3 S1 O4 Cu1 18.58(14) .
O1 S1 O4 Cu1 137.75(11) .
O6 Cu1 O4 S1 0.61(12) .
O6 Cu1 O4 S1 -179.39(12) 2_656
O4 Cu1 O4 S1 119(100) 2_656
O12 S3 O14 Cu2 111.26(12) .
O13 S3 O14 Cu2 -10.77(14) .
O11 S3 O14 Cu2 -129.83(11) .
O16 Cu2 O14 S3 -178.33(12) 2_565
O16 Cu2 O14 S3 1.67(12) .
O14 Cu2 O14 S3 45(100) 2_565
