#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:51:31 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179600 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/64/4506451.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_4506451
loop_
_publ_author_name
'Vakiti, Raj Kishore'
'Garabato, Brady D.'
'Schieber, Natalie P.'
'Rucks, Melinda J.'
'Cao, Yan'
'Webb, Cathleen'
'Maddox, Jeremy B.'
'Celestian, Aaron'
'Pan, Wei-Ping'
'Yan, Bangbo'
_publ_section_title
;
 Synthesis and Characterization of Two- and Three-Dimensional Calcium
 Coordination Polymers Built with Benzene-1,3,5-tricarboxylate and/or
 Pyrazine-2-carboxylate
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3937
_journal_paper_doi               10.1021/cg3003349
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C18 H30 Ca3 O24'
_chemical_formula_weight         750.66
_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                 99.5070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.72570(10)
_cell_length_b                   20.8422(4)
_cell_length_c                   20.1942(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2791.91(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Apex II CCD'
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46626
_diffrn_reflns_theta_full        36.40
_diffrn_reflns_theta_max         36.40
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.8787
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         6750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0408
_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)+(0.0238P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                5059
_reflns_number_total             6750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3003349_si_002.cif
_cod_data_source_block           c2c
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               4506451
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 0.61289(6) 0.628151(14) -0.007552(16) 0.01882(7) Uani 1 1 d .
C2 C 0.9840(2) 1.18754(6) 0.18933(8) 0.0160(2) Uani 1 1 d .
Ca2 Ca 1.0000 0.875142(19) 0.2500 0.01702(8) Uani 1 2 d S
O1 O 0.95288(19) 1.28268(5) 0.12264(6) 0.0217(2) Uani 1 1 d .
O2 O 1.0061(2) 1.19043(6) 0.07377(7) 0.0298(3) Uani 1 1 d .
O3 O 0.9926(2) 0.98527(5) 0.30377(6) 0.0251(3) Uani 1 1 d .
O4 O 0.9427(2) 0.76780(5) 0.19615(6) 0.0285(3) Uani 1 1 d .
O5 O 0.7880(2) 0.56223(6) 0.07632(6) 0.0272(3) Uani 1 1 d .
O6 O 0.91914(18) 0.47177(5) 0.12180(6) 0.0212(2) Uani 1 1 d .
C1 C 1.0000 1.22084(9) 0.2500 0.0161(4) Uani 1 2 d S
H1 H 1.0000 1.2695(12) 0.2500 0.012(6) Uiso 1 2 d S
C3 C 0.9827(3) 1.12076(6) 0.18998(9) 0.0161(3) Uani 1 1 d .
H3 H 0.974(3) 1.1006(10) 0.1494(13) 0.027(5) Uiso 1 1 d .
C4 C 1.0000 1.08697(9) 0.2500 0.0154(3) Uani 1 2 d S
C5 C 0.9798(2) 1.22251(7) 0.12378(8) 0.0173(3) Uani 1 1 d .
C6 C 1.0000 1.01510(9) 0.2500 0.0159(4) Uani 1 2 d S
C7 C 1.0000 0.66606(9) 0.2500 0.0159(3) Uani 1 2 d S
C8 C 0.9473(2) 0.63260(7) 0.19039(8) 0.0166(3) Uani 1 1 d .
H8 H 0.905(3) 0.6517(9) 0.1516(10) 0.012(4) Uiso 1 1 d .
C9 C 0.9461(2) 0.56579(6) 0.18979(7) 0.0144(2) Uani 1 1 d .
C10 C 1.0000 0.53249(9) 0.2500 0.0155(3) Uani 1 2 d S
H10 H 1.0000 0.4845(13) 0.2500 0.025(7) Uiso 1 2 d S
C11 C 1.0000 0.73798(9) 0.2500 0.0166(4) Uani 1 2 d S
C12 C 0.8784(2) 0.53146(7) 0.12481(8) 0.0166(3) Uani 1 1 d .
O1W O 0.3053(2) 0.57128(6) -0.00336(8) 0.0272(3) Uani 1 1 d .
H1WA H 0.309(5) 0.5398(15) 0.0248(17) 0.066(10) Uiso 1 1 d .
H1WB H 0.233(6) 0.5586(14) -0.0427(17) 0.062(9) Uiso 1 1 d .
O2W O 0.7005(2) 0.53757(7) -0.07484(7) 0.0264(3) Uani 1 1 d .
H2WA H 0.624(5) 0.5271(12) -0.1112(15) 0.041(7) Uiso 1 1 d .
H2WB H 0.805(7) 0.5318(18) -0.0820(19) 0.084(12) Uiso 1 1 d .
O3W O 0.9600(2) 0.65928(6) -0.01123(7) 0.0275(3) Uani 1 1 d .
H3WA H 0.999(4) 0.6802(13) -0.0464(13) 0.040(7) Uiso 1 1 d .
H3WB H 1.057(5) 0.6367(12) 0.0016(13) 0.041(7) Uiso 1 1 d .
O4W O 0.5679(3) 0.72605(6) -0.06372(8) 0.0332(3) Uani 1 1 d .
H4WA H 0.555(4) 0.7331(11) -0.1058(15) 0.038(7) Uiso 1 1 d .
H4WB H 0.532(5) 0.7552(14) -0.0466(14) 0.054(9) Uiso 1 1 d .
O5W O 1.1453(2) 0.87274(6) 0.14172(9) 0.0328(3) Uani 1 1 d .
H5WA H 1.210(5) 0.9010(14) 0.1414(14) 0.042(8) Uiso 1 1 d .
H5WB H 1.220(5) 0.8398(13) 0.1384(13) 0.046(8) Uiso 1 1 d .
O6W O 0.6658(2) 0.87908(7) 0.19549(9) 0.0335(3) Uani 1 1 d .
H6WA H 0.597(4) 0.9052(14) 0.1756(13) 0.041(7) Uiso 1 1 d .
H6WB H 0.617(4) 0.8485(12) 0.1752(13) 0.029(6) Uiso 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'
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
O2 Ca1 O4W 79.78(5) 3_445 .
O2 Ca1 O5 89.64(5) 3_445 .
O4W Ca1 O5 151.08(5) . .
O2 Ca1 O1W 83.15(5) 3_445 .
O4W Ca1 O1W 114.00(6) . .
O5 Ca1 O1W 91.04(5) . .
O2 Ca1 O3W 106.58(5) 3_445 .
O4W Ca1 O3W 78.45(5) . .
O5 Ca1 O3W 78.96(5) . .
O1W Ca1 O3W 165.82(5) . .
O2 Ca1 O2W 164.08(5) 3_445 .
O4W Ca1 O2W 115.33(5) . .
O5 Ca1 O2W 79.11(5) . .
O1W Ca1 O2W 85.80(5) . .
O3W Ca1 O2W 82.47(5) . .
O2 Ca1 O5W 116.81(5) 3_445 7_665
O4W Ca1 O5W 63.36(5) . 7_665
O5 Ca1 O5W 143.64(4) . 7_665
O1W Ca1 O5W 69.57(5) . 7_665
O3W Ca1 O5W 113.15(5) . 7_665
O2W Ca1 O5W 69.35(4) . 7_665
O2 Ca1 H4WB 66.2(6) 3_445 .
O4W Ca1 H4WB 13.6(6) . .
O5 Ca1 H4WB 144.3(6) . .
O1W Ca1 H4WB 110.5(7) . .
O3W Ca1 H4WB 83.2(7) . .
O2W Ca1 H4WB 128.8(6) . .
O5W Ca1 H4WB 72.0(6) 7_665 .
C3 C2 C1 119.23(15) . .
C3 C2 C5 119.51(14) . .
C1 C2 C5 121.17(12) . .
O6W Ca2 O6W 175.97(7) 2_755 .
O6W Ca2 O4 76.01(5) 2_755 2_755
O6W Ca2 O4 107.76(5) . 2_755
O6W Ca2 O4 107.76(5) 2_755 .
O6W Ca2 O4 76.01(5) . .
O4 Ca2 O4 52.04(6) 2_755 .
O6W Ca2 O5W 94.13(6) 2_755 2_755
O6W Ca2 O5W 85.95(6) . 2_755
O4 Ca2 O5W 70.12(4) 2_755 2_755
O4 Ca2 O5W 107.74(5) . 2_755
O6W Ca2 O5W 85.95(6) 2_755 .
O6W Ca2 O5W 94.13(6) . .
O4 Ca2 O5W 107.74(5) 2_755 .
O4 Ca2 O5W 70.12(4) . .
O5W Ca2 O5W 177.74(6) 2_755 .
O6W Ca2 O3 94.84(5) 2_755 2_755
O6W Ca2 O3 81.49(5) . 2_755
O4 Ca2 O3 170.08(5) 2_755 2_755
O4 Ca2 O3 129.57(4) . 2_755
O5W Ca2 O3 115.02(4) 2_755 2_755
O5W Ca2 O3 67.21(4) . 2_755
O6W Ca2 O3 81.49(5) 2_755 .
O6W Ca2 O3 94.84(5) . .
O4 Ca2 O3 129.57(4) 2_755 .
O4 Ca2 O3 170.08(5) . .
O5W Ca2 O3 67.21(4) 2_755 .
O5W Ca2 O3 115.02(4) . .
O3 Ca2 O3 51.01(6) 2_755 .
O6W Ca2 C11 92.02(3) 2_755 .
O6W Ca2 C11 92.02(3) . .
O4 Ca2 C11 26.02(3) 2_755 .
O4 Ca2 C11 26.02(3) . .
O5W Ca2 C11 88.87(3) 2_755 .
O5W Ca2 C11 88.87(3) . .
O3 Ca2 C11 154.49(3) 2_755 .
O3 Ca2 C11 154.49(3) . .
O6W Ca2 C6 87.98(3) 2_755 .
O6W Ca2 C6 87.98(3) . .
O4 Ca2 C6 153.98(3) 2_755 .
O4 Ca2 C6 153.98(3) . .
O5W Ca2 C6 91.13(3) 2_755 .
O5W Ca2 C6 91.13(3) . .
O3 Ca2 C6 25.51(3) 2_755 .
O3 Ca2 C6 25.51(3) . .
C11 Ca2 C6 180.0 . .
C5 O2 Ca1 169.47(13) . 3
C6 O3 Ca2 94.07(10) . .
C11 O4 Ca2 93.62(10) . .
C12 O5 Ca1 174.37(11) . .
C2 C1 C2 120.41(18) 2_755 .
C2 C1 H1 119.79(9) 2_755 .
C2 C1 H1 119.80(9) . .
C4 C3 C2 121.00(15) . .
C4 C3 H3 122.2(14) . .
C2 C3 H3 116.8(14) . .
C3 C4 C3 119.12(17) . 2_755
C3 C4 C6 120.44(9) . .
C3 C4 C6 120.44(9) 2_755 .
O2 C5 O1 123.69(15) . .
O2 C5 C2 117.85(13) . .
O1 C5 C2 118.46(13) . .
O3 C6 O3 120.84(18) . 2_755
O3 C6 C4 119.58(9) . .
O3 C6 C4 119.58(9) 2_755 .
O3 C6 Ca2 60.42(9) . .
O3 C6 Ca2 60.42(9) 2_755 .
C4 C6 Ca2 180.0 . .
C8 C7 C8 119.56(18) . 2_755
C8 C7 C11 120.22(9) . .
C8 C7 C11 120.22(9) 2_755 .
C7 C8 C9 120.74(14) . .
C7 C8 H8 122.9(12) . .
C9 C8 H8 116.2(12) . .
C8 C9 C10 119.31(14) . .
C8 C9 C12 119.06(13) . .
C10 C9 C12 121.57(12) . .
C9 C10 C9 120.33(17) . 2_755
C9 C10 H10 119.84(9) . .
C9 C10 H10 119.84(9) 2_755 .
O4 C11 O4 120.71(18) . 2_755
O4 C11 C7 119.64(9) . .
O4 C11 C7 119.65(9) 2_755 .
O4 C11 Ca2 60.36(9) . .
O4 C11 Ca2 60.35(9) 2_755 .
C7 C11 Ca2 180.0 . .
O5 C12 O6 123.10(14) . .
O5 C12 C9 118.84(13) . .
O6 C12 C9 118.06(13) . .
Ca1 O1W H1WA 118(2) . .
Ca1 O1W H1WB 117(2) . .
H1WA O1W H1WB 108(3) . .
Ca1 O2W H2WA 120.6(18) . .
Ca1 O2W H2WB 123(3) . .
H2WA O2W H2WB 104(4) . .
Ca1 O3W H3WA 123.8(18) . .
Ca1 O3W H3WB 124.1(19) . .
H3WA O3W H3WB 102(2) . .
Ca1 O4W H4WA 128.2(16) . .
Ca1 O4W H4WB 120(2) . .
H4WA O4W H4WB 109(3) . .
Ca2 O5W Ca1 122.43(6) . 7_665
Ca2 O5W H5WA 108(2) . .
Ca1 O5W H5WA 105(2) 7_665 .
Ca2 O5W H5WB 113.4(18) . .
Ca1 O5W H5WB 100.7(18) 7_665 .
H5WA O5W H5WB 107(3) . .
Ca2 O6W H6WA 135(2) . .
Ca2 O6W H6WB 119.9(18) . .
H6WA O6W H6WB 98(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.2993(13) 3_445
Ca1 O4W 2.3299(14) .
Ca1 O5 2.3417(12) .
Ca1 O1W 2.3980(13) .
Ca1 O3W 2.4360(14) .
Ca1 O2W 2.4540(14) .
Ca1 O5W 2.9667(19) 7_665
Ca1 H4WB 2.79(3) .
C2 C3 1.3920(18) .
C2 C1 1.3967(18) .
C2 C5 1.507(2) .
Ca2 O6W 2.3354(15) 2_755
Ca2 O6W 2.3354(15) .
Ca2 O4 2.4895(12) 2_755
Ca2 O4 2.4896(12) .
Ca2 O5W 2.5386(16) 2_755
Ca2 O5W 2.5386(16) .
Ca2 O3 2.5432(12) 2_755
Ca2 O3 2.5432(12) .
Ca2 C11 2.8588(19) .
Ca2 C6 2.9170(19) .
O1 C5 1.2669(18) .
O2 C5 1.2479(19) .
O2 Ca1 2.2994(13) 3
O3 C6 1.2592(15) .
O4 C11 1.2567(15) .
O5 C12 1.2424(19) .
O6 C12 1.2776(18) .
C1 C2 1.3967(18) 2_755
C1 H1 1.01(3) .
C3 C4 1.3899(19) .
C3 H3 0.91(2) .
C4 C3 1.3899(19) 2_755
C4 C6 1.498(3) .
C6 O3 1.2593(15) 2_755
C7 C8 1.3857(18) .
C7 C8 1.3857(18) 2_755
C7 C11 1.499(3) .
C8 C9 1.3925(19) .
C8 H8 0.88(2) .
C9 C10 1.3949(17) .
C9 C12 1.498(2) .
C10 C9 1.3949(17) 2_755
C10 H10 1.00(3) .
C11 O4 1.2567(15) 2_755
O1W H1WA 0.87(3) .
O1W H1WB 0.90(4) .
O2W H2WA 0.85(3) .
O2W H2WB 0.75(5) .
O3W H3WA 0.91(3) .
O3W H3WB 0.81(3) .
O4W H4WA 0.85(3) .
O4W H4WB 0.76(3) .
O5W Ca1 2.9667(19) 7_665
O5W H5WA 0.73(3) .
O5W H5WB 0.86(3) .
O6W H6WA 0.78(3) .
O6W H6WB 0.80(3) .
