#------------------------------------------------------------------------------
#$Date: 2019-01-06 10:04:55 +0200 (Sun, 06 Jan 2019) $
#$Revision: 212870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/82/7108222.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_7108222
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         '2(C9 H3 O6 -3) 3(Ca +2)'
_chemical_formula_sum            'C18 H6 Ca3 O12'
_chemical_formula_weight         534.48
_chemical_name_common            Ca-BTC
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   8.9636(3)
_cell_length_b                   8.9636(3)
_cell_length_c                   19.2832(11)
_cell_measurement_temperature    190(2)
_cell_volume                     1341.76(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            1049
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.000
_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    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.095
_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     51
_refine_ls_number_reflns         795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0375
_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)+(0.0322P)²+2.8251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                580
_reflns_number_total             795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34006b.txt
_cod_data_source_block           Ca-BTC
_cod_depositor_comments
;

2018-12-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H2 Ca O4'
_cod_original_formula_weight         178.16
_cod_original_formula_moiety         'C6 H2 Ca O4'
_cod_original_formula_units_Z            9
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7108222
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 -0.3333 0.3333 0.00637(4) 0.0140(3) Uani 1 3 d S
Ca2 Ca 0.3333 0.6667 0.1667 0.0135(3) Uani 1 6 d S
O1 O -0.1176(2) 0.3314(2) 0.06511(11) 0.0215(5) Uani 1 1 d .
O3 O 0.1637(2) 0.4653(2) 0.08464(9) 0.0168(4) Uani 1 1 d .
C5 C 0.1588(3) 0.1508(3) 0.08937(13) 0.0138(5) Uani 1 1 d .
H5 H 0.2651 0.2518 0.0898 0.017 Uiso 1 1 calc R
C8 C 0.0079(3) 0.1596(3) 0.08906(13) 0.0134(5) Uani 1 1 d .
C11 C 0.0162(3) 0.3300(3) 0.07955(13) 0.0141(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'
Ca Ca 0.2262 0.3064 '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'
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 Ca1 O1 96.86(7) . 2_565
O1 Ca1 O1 96.86(7) . 3_455
O1 Ca1 O1 96.86(7) 2_565 3_455
O1 Ca1 O3 89.35(6) . 12
O1 Ca1 O3 162.58(7) 2_565 12
O1 Ca1 O3 98.54(6) 3_455 12
O1 Ca1 O3 98.54(6) . 10_565
O1 Ca1 O3 89.35(6) 2_565 10_565
O1 Ca1 O3 162.58(7) 3_455 10_565
O3 Ca1 O3 73.60(7) 12 10_565
O1 Ca1 O3 162.58(7) . 11_455
O1 Ca1 O3 98.54(6) 2_565 11_455
O1 Ca1 O3 89.35(6) 3_455 11_455
O3 Ca1 O3 73.60(7) 12 11_455
O3 Ca1 O3 73.60(7) 10_565 11_455
O1 Ca1 Ca2 120.24(6) . 7_444
O1 Ca1 Ca2 120.25(6) 2_565 7_444
O1 Ca1 Ca2 120.25(6) 3_455 7_444
O3 Ca1 Ca2 43.77(4) 12 7_444
O3 Ca1 Ca2 43.77(4) 10_565 7_444
O3 Ca1 Ca2 43.77(4) 11_455 7_444
O3 Ca2 O3 78.20(7) . 3_565
O3 Ca2 O3 78.20(7) . 2_665
O3 Ca2 O3 78.20(7) 3_565 2_665
O3 Ca2 O3 101.80(7) . 15
O3 Ca2 O3 180.0 3_565 15
O3 Ca2 O3 101.80(7) 2_665 15
O3 Ca2 O3 180.00(9) . 13_565
O3 Ca2 O3 101.80(7) 3_565 13_565
O3 Ca2 O3 101.80(7) 2_665 13_565
O3 Ca2 O3 78.20(7) 15 13_565
O3 Ca2 O3 101.80(7) . 14_455
O3 Ca2 O3 101.80(7) 3_565 14_455
O3 Ca2 O3 180.0 2_665 14_455
O3 Ca2 O3 78.20(7) 15 14_455
O3 Ca2 O3 78.20(7) 13_565 14_455
O3 Ca2 Ca1 46.74(4) . 10_565
O3 Ca2 Ca1 46.74(4) 3_565 10_565
O3 Ca2 Ca1 46.74(4) 2_665 10_565
O3 Ca2 Ca1 133.26(4) 15 10_565
O3 Ca2 Ca1 133.26(4) 13_565 10_565
O3 Ca2 Ca1 133.26(4) 14_455 10_565
O3 Ca2 Ca1 133.26(4) . 4
O3 Ca2 Ca1 133.26(4) 3_565 4
O3 Ca2 Ca1 133.26(4) 2_665 4
O3 Ca2 Ca1 46.74(4) 15 4
O3 Ca2 Ca1 46.74(4) 13_565 4
O3 Ca2 Ca1 46.74(4) 14_455 4
Ca1 Ca2 Ca1 180.0 10_565 4
C11 O1 Ca1 162.77(19) . .
C11 O3 Ca2 139.54(16) . .
C11 O3 Ca1 128.10(16) . 10_565
Ca2 O3 Ca1 89.49(6) . 10_565
C8 C5 C8 120.6(2) 3 .
C8 C5 H5 119.7 3 .
C8 C5 H5 119.7 . .
C5 C8 C5 119.4(2) 2 .
C5 C8 C11 120.0(2) 2 .
C5 C8 C11 120.1(2) . .
O1 C11 O3 123.9(2) . .
O1 C11 C8 118.8(2) . .
O3 C11 C8 117.2(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.2489(18) .
Ca1 O1 2.2489(18) 2_565
Ca1 O1 2.2489(18) 3_455
Ca1 O3 2.4300(19) 12
Ca1 O3 2.4300(19) 10_565
Ca1 O3 2.4300(19) 11_455
Ca1 Ca2 3.3367(9) 7_444
Ca2 O3 2.3081(17) .
Ca2 O3 2.3081(17) 3_565
Ca2 O3 2.3081(17) 2_665
Ca2 O3 2.3081(17) 15
Ca2 O3 2.3082(17) 13_565
Ca2 O3 2.3082(17) 14_455
Ca2 Ca1 3.3366(9) 10_565
Ca2 Ca1 3.3367(9) 4
O1 C11 1.237(3) .
O3 C11 1.275(3) .
O3 Ca1 2.4300(19) 10_565
C5 C8 1.392(3) 3
C5 C8 1.394(3) .
C5 H5 0.9300 .
C8 C5 1.392(3) 2
C8 C11 1.503(3) .
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
_geom_torsion_site_symmetry_4
O1 Ca1 O1 C11 -131.3(6) 2_565 .
O1 Ca1 O1 C11 130.9(6) 3_455 .
O3 Ca1 O1 C11 32.4(6) 12 .
O3 Ca1 O1 C11 -40.9(6) 10_565 .
O3 Ca1 O1 C11 20.7(7) 11_455 .
Ca2 Ca1 O1 C11 -0.2(6) 7_444 .
O3 Ca2 O3 C11 -120.0(3) 3_565 .
O3 Ca2 O3 C11 159.7(3) 2_665 .
O3 Ca2 O3 C11 60.0(3) 15 .
O3 Ca2 O3 C11 26.4(15) 13_565 .
O3 Ca2 O3 C11 -20.3(3) 14_455 .
Ca1 Ca2 O3 C11 -160.1(3) 10_565 .
Ca1 Ca2 O3 C11 19.8(3) 4 .
O3 Ca2 O3 Ca1 40.11(2) 3_565 10_565
O3 Ca2 O3 Ca1 -40.11(2) 2_665 10_565
O3 Ca2 O3 Ca1 -139.89(2) 15 10_565
O3 Ca2 O3 Ca1 -173.4(15) 13_565 10_565
O3 Ca2 O3 Ca1 139.89(2) 14_455 10_565
Ca1 Ca2 O3 Ca1 180.0 4 10_565
C8 C5 C8 C5 0.9(5) 3 2
C8 C5 C8 C11 -171.61(16) 3 .
Ca1 O1 C11 O3 86.7(6) . .
Ca1 O1 C11 C8 -90.7(6) . .
Ca2 O3 C11 O1 88.4(3) . .
Ca1 O3 C11 O1 -66.1(3) 10_565 .
Ca2 O3 C11 C8 -94.2(3) . .
Ca1 O3 C11 C8 111.4(2) 10_565 .
C5 C8 C11 O1 -7.3(4) 2 .
C5 C8 C11 O1 165.2(2) . .
C5 C8 C11 O3 175.1(2) 2 .
C5 C8 C11 O3 -12.4(4) . .
