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#$Date: 2016-03-26 03:32:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180186 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/82/7108220.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_7108220
loop_
_publ_author_name
'Arijit Mallick'
'Tanay Kundu'
'Rahul Banerjee'
_publ_section_title
;
 Correlation between coordinated water content and proton conductivity in
 Ca-BTC-based metal-organic frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              8829
_journal_paper_doi               10.1039/c2cc34006b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C22 H22 Ca3 O16 S2, 2(C H3 O S)'
_chemical_formula_sum            'C24 H28 Ca3 O18 S4'
_chemical_formula_weight         852.98
_chemical_name_common            Ca-BTC-DMSO
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.88(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.547(3)
_cell_length_b                   13.6128(19)
_cell_length_c                   18.981(4)
_cell_measurement_temperature    190(2)
_cell_volume                     3931.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.857
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10360
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760.0
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.929
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1243P)²+19.7714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2320
_refine_ls_wR_factor_ref         0.2522
_reflns_number_gt                3542
_reflns_number_total             5252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34006b.txt
_cod_data_source_block           Ca-BTC-DMSO
_cod_original_cell_volume        3931.0(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7108220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca1 Ca 0.5000 0.69807(8) 0.2500 0.0186(3) Uani 1 2 d S
S1 S 0.32437(8) 0.71107(12) 0.08782(7) 0.0450(4) Uani 1 1 d .
O2 O 0.4282(2) 0.5788(2) 0.30302(16) 0.0318(7) Uani 1 1 d .
O3 O 0.0660(2) 0.9811(3) 0.45426(17) 0.0368(8) Uani 1 1 d .
O4 O 0.4152(2) 0.6802(3) 0.12915(17) 0.0360(8) Uani 1 1 d .
O5 O 0.4089(2) 0.7677(3) 0.3921(2) 0.0440(9) Uani 1 1 d .
O6 O 0.1569(3) 0.8653(3) 0.5050(2) 0.0508(11) Uani 1 1 d .
O7 O 0.3637(2) 0.4763(3) 0.36559(17) 0.0394(8) Uani 1 1 d .
O9 O 0.4049(3) 0.8125(3) 0.2782(2) 0.0458(10) Uani 1 1 d .
C10 C 0.3777(3) 0.5067(3) 0.3065(2) 0.0279(9) Uani 1 1 d .
C11 C 0.2468(3) 0.9108(4) 0.2687(3) 0.0349(11) Uani 1 1 d .
H11 H 0.2726 0.9085 0.2286 0.042 Uiso 1 1 calc R
C12 C 0.3747(3) 0.8111(4) 0.3354(3) 0.0355(11) Uani 1 1 d .
C13 C 0.1707(3) 0.9192(4) 0.3887(3) 0.0379(12) Uani 1 1 d .
C14 C 0.2895(3) 0.8665(4) 0.3319(3) 0.0364(11) Uani 1 1 d .
C15 C 0.3331(3) 0.4586(3) 0.2368(2) 0.0326(10) Uani 1 1 d .
C16 C 0.2509(4) 0.8691(4) 0.3924(3) 0.0405(13) Uani 1 1 d .
H16 H 0.2781 0.8380 0.4348 0.049 Uiso 1 1 calc R
C17 C 0.2521(4) 0.6933(6) 0.1482(4) 0.0644(19) Uani 1 1 d .
H17A H 0.2441 0.6243 0.1548 0.097 Uiso 1 1 calc R
H17B H 0.1963 0.7232 0.1287 0.097 Uiso 1 1 calc R
H17C H 0.2769 0.7230 0.1938 0.097 Uiso 1 1 calc R
C19 C 0.1294(3) 0.9634(4) 0.3244(3) 0.0354(11) Uani 1 1 d .
H19 H 0.0764 0.9963 0.3220 0.042 Uiso 1 1 calc R
C20 C 0.1289(3) 0.9222(4) 0.4539(3) 0.0357(11) Uani 1 1 d .
C22 C 0.3289(7) 0.8404(8) 0.0877(6) 0.106(2) Uani 1 1 d .
H22A H 0.3571 0.8633 0.1347 0.158 Uiso 1 1 calc R
H22B H 0.2704 0.8665 0.0755 0.158 Uiso 1 1 calc R
H22C H 0.3618 0.8620 0.0530 0.158 Uiso 1 1 calc R
Ca2 Ca 0.46456(5) 0.61221(6) 0.43405(4) 0.0221(3) Uani 1 1 d .
O1 O 0.5632(3) 0.6858(3) 0.5366(2) 0.0447(9) Uani 1 1 d .
H1A H 0.5399 0.7409 0.5524 0.067 Uiso 1 1 d R
H1B H 0.5754 0.6439 0.5746 0.067 Uiso 1 1 d R
S8 S 0.4668(3) 0.9192(5) 0.6097(4) 0.272(5) Uani 1 1 d .
C8 C 0.3663(7) 0.8605(9) 0.6024(6) 0.106(2) Uani 1 1 d .
H8A H 0.3198 0.9080 0.5912 0.158 Uiso 1 1 calc R
H8B H 0.3640 0.8289 0.6472 0.158 Uiso 1 1 calc R
H8C H 0.3595 0.8123 0.5648 0.158 Uiso 1 1 calc R
O8 O 0.5321(6) 0.8460(8) 0.6111(6) 0.170(5) 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'
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'
Ca Ca 0.2262 0.3064 '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
O9 Ca1 O9 94.0(2) . 2_655
O9 Ca1 O2 89.05(13) . .
O9 Ca1 O2 166.63(14) 2_655 .
O9 Ca1 O2 166.62(14) . 2_655
O9 Ca1 O2 89.05(13) 2_655 2_655
O2 Ca1 O2 90.91(17) . 2_655
O9 Ca1 O4 92.18(13) . .
O9 Ca1 O4 95.72(14) 2_655 .
O2 Ca1 O4 97.16(12) . .
O2 Ca1 O4 74.55(12) 2_655 .
O9 Ca1 O4 95.72(13) . 2_655
O9 Ca1 O4 92.18(13) 2_655 2_655
O2 Ca1 O4 74.56(12) . 2_655
O2 Ca1 O4 97.16(12) 2_655 2_655
O4 Ca1 O4 168.4(2) . 2_655
O9 Ca1 C12 106.46(14) . 2_655
O9 Ca1 C12 19.32(12) 2_655 2_655
O2 Ca1 C12 164.35(13) . 2_655
O2 Ca1 C12 73.53(12) 2_655 2_655
O4 Ca1 C12 80.58(13) . 2_655
O4 Ca1 C12 105.16(13) 2_655 2_655
O9 Ca1 Ca2 130.00(10) . 2_655
O9 Ca1 Ca2 76.89(9) 2_655 2_655
O2 Ca1 Ca2 110.82(8) . 2_655
O2 Ca1 Ca2 38.41(7) 2_655 2_655
O4 Ca1 Ca2 41.80(8) . 2_655
O4 Ca1 Ca2 133.14(9) 2_655 2_655
C12 Ca1 Ca2 57.58(9) 2_655 2_655
O4 S1 C22 104.0(4) . .
O4 S1 C17 105.7(3) . .
C22 S1 C17 99.6(5) . .
C10 O2 Ca1 157.8(3) . .
C10 O2 Ca2 96.0(2) . .
Ca1 O2 Ca2 106.10(12) . .
C20 O3 Ca2 165.8(3) . 3_455
C20 O3 Ca2 88.0(3) . 7_566
Ca2 O3 Ca2 105.91(11) 3_455 7_566
S1 O4 Ca1 136.7(2) . .
S1 O4 Ca2 122.66(17) . 2_655
Ca1 O4 Ca2 99.86(11) . 2_655
C12 O5 Ca2 141.0(4) . .
C20 O6 Ca2 96.3(3) . 7_566
C10 O7 Ca2 90.8(3) . .
C12 O9 Ca1 124.1(3) . .
O7 C10 O2 121.7(4) . .
O7 C10 C15 120.4(4) . .
O2 C10 C15 117.9(4) . .
C14 C11 C15 122.1(4) . 4
O5 C12 O9 125.4(4) . .
O5 C12 C14 119.2(4) . .
O9 C12 C14 115.5(4) . .
C19 C13 C16 119.7(4) . .
C19 C13 C20 120.4(4) . .
C16 C13 C20 119.8(4) . .
C11 C14 C16 119.4(4) . .
C11 C14 C12 120.9(4) . .
C16 C14 C12 119.7(4) . .
C11 C15 C19 118.6(4) 4_545 4_545
C11 C15 C10 120.8(4) 4_545 .
C19 C15 C10 120.6(4) 4_545 .
C14 C16 C13 119.6(4) . .
C13 C19 C15 120.6(4) . 4
O6 C20 O3 122.5(4) . .
O6 C20 C13 118.6(4) . .
O3 C20 C13 118.9(4) . .
O6 C20 Ca2 57.9(2) . 7_566
O3 C20 Ca2 65.6(2) . 7_566
C13 C20 Ca2 167.7(4) . 7_566
O3 Ca2 O5 156.71(13) 3_545 .
O3 Ca2 O6 125.26(12) 3_545 7_566
O5 Ca2 O6 77.32(12) . 7_566
O3 Ca2 O1 83.75(14) 3_545 .
O5 Ca2 O1 91.56(15) . .
O6 Ca2 O1 89.49(15) 7_566 .
O3 Ca2 O2 91.78(12) 3_545 .
O5 Ca2 O2 80.46(13) . .
O6 Ca2 O2 117.56(13) 7_566 .
O1 Ca2 O2 148.76(12) . .
O3 Ca2 O4 79.83(12) 3_545 2_655
O5 Ca2 O4 76.89(13) . 2_655
O6 Ca2 O4 151.80(14) 7_566 2_655
O1 Ca2 O4 80.02(12) . 2_655
O2 Ca2 O4 68.76(10) . 2_655
O3 Ca2 O7 81.77(14) 3_545 .
O5 Ca2 O7 109.20(14) . .
O6 Ca2 O7 83.10(15) 7_566 .
O1 Ca2 O7 155.67(13) . .
O2 Ca2 O7 51.44(10) . .
O4 Ca2 O7 116.23(11) 2_655 .
O3 Ca2 O3 74.10(11) 3_545 7_566
O5 Ca2 O3 126.68(11) . 7_566
O6 Ca2 O3 51.85(10) 7_566 7_566
O1 Ca2 O3 74.93(13) . 7_566
O2 Ca2 O3 133.43(12) . 7_566
O4 Ca2 O3 145.39(11) 2_655 7_566
O7 Ca2 O3 82.34(12) . 7_566
O3 Ca2 C20 100.41(12) 3_545 7_566
O5 Ca2 C20 101.02(13) . 7_566
O6 Ca2 C20 25.80(12) 7_566 7_566
O1 Ca2 C20 78.78(15) . 7_566
O2 Ca2 C20 132.31(14) . 7_566
O4 Ca2 C20 158.63(14) 2_655 7_566
O7 Ca2 C20 84.73(14) . 7_566
O3 Ca2 C20 26.34(11) 7_566 7_566
O3 Ca2 Ca2 39.13(7) 3_545 5_666
O5 Ca2 Ca2 159.94(10) . 5_666
O6 Ca2 Ca2 86.49(9) 7_566 5_666
O1 Ca2 Ca2 76.38(10) . 5_666
O2 Ca2 Ca2 118.01(9) . 5_666
O4 Ca2 Ca2 115.78(8) 2_655 5_666
O7 Ca2 Ca2 80.05(9) . 5_666
O3 Ca2 Ca2 34.97(7) 7_566 5_666
C20 Ca2 Ca2 61.29(10) 7_566 5_666
O8 S8 C8 107.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O9 2.286(3) .
Ca1 O9 2.286(3) 2_655
Ca1 O2 2.314(3) .
Ca1 O2 2.314(3) 2_655
Ca1 O4 2.411(3) .
Ca1 O4 2.411(3) 2_655
Ca1 C12 3.176(4) 2_655
Ca1 Ca2 3.8297(11) 2_655
S1 O4 1.526(3) .
S1 C22 1.762(12) .
S1 C17 1.779(7) .
O2 C10 1.267(5) .
O2 Ca2 2.477(3) .
O3 C20 1.265(5) .
O3 Ca2 2.360(3) 3_455
O3 Ca2 2.598(3) 7_566
O4 Ca2 2.591(3) 2_655
O5 C12 1.248(6) .
O5 Ca2 2.361(3) .
O6 C20 1.248(6) .
O6 Ca2 2.429(3) 7_566
O7 C10 1.256(5) .
O7 Ca2 2.594(4) .
O9 C12 1.269(6) .
C10 C15 1.511(6) .
C11 C14 1.384(7) .
C11 C15 1.387(6) 4
C12 C14 1.514(6) .
C13 C19 1.393(7) .
C13 C16 1.411(6) .
C13 C20 1.512(6) .
C14 C16 1.401(6) .
C15 C11 1.387(6) 4_545
C15 C19 1.406(6) 4_545
C19 C15 1.406(6) 4
C20 Ca2 2.850(4) 7_566
Ca2 O3 2.360(3) 3_545
Ca2 O6 2.429(3) 7_566
Ca2 O1 2.432(4) .
Ca2 O4 2.591(3) 2_655
Ca2 O3 2.598(3) 7_566
Ca2 C20 2.850(4) 7_566
Ca2 Ca2 3.9596(16) 5_666
S8 O8 1.418(8) .
S8 C8 1.735(12) .
