#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:58:17 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180458 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/27/7212706.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_7212706
loop_
_publ_author_name
'Lin, Jian-Di'
'Wu, Shu-Ting'
'Li, Zhi-Hua'
'Du, Shao-Wu'
_publ_section_title
;
 A series of novel Pb(ii) or Pb(ii)/M(ii) (M = Ca and Sr) hybrid
 inorganic--organic frameworks based on polycarboxylic acids with diverse
 Pb--O--M (M = Pb, Ca and Sr) inorganic connectivities
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4252
_journal_paper_doi               10.1039/c004010j
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C18 H16 Ca O12 Pb'
_chemical_formula_weight         671.58
_chemical_name_systematic
;
?
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.1180(4)
_cell_length_b                   21.1180(4)
_cell_length_c                   9.4092(3)
_cell_measurement_reflns_used    7425
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4785
_cell_measurement_theta_min      2.3697
_cell_volume                     4196.22(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15971
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    8.350
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7373
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.863
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.060(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2386
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0558P)²+4.5513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2374
_reflns_number_total             2386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c004010j.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      I-42d
_cod_database_code               7212706
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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
Pb1 Pb 0.303998(3) 0.2500 0.1250 0.02016(1) Uani 1 2 d S
Ca1 Ca 0.2500 0.391882(17) -0.1250 0.02340(8) Uani 1 2 d S
O1 O 0.31996(5) 0.30902(6) -0.16594(12) 0.0324(3) Uani 1 1 d .
O2 O 0.39197(5) 0.28475(6) -0.00168(12) 0.0326(3) Uani 1 1 d .
O3 O 0.61617(5) 0.28545(6) -0.10578(11) 0.0337(3) Uani 1 1 d .
O4 O 0.65325(5) 0.33626(5) -0.29241(12) 0.0279(3) Uani 1 1 d .
O5 O 0.45493(5) 0.35380(7) -0.60106(11) 0.0368(3) Uani 1 1 d D
H10 H 0.4140(3) 0.361(2) -0.6525(15) 0.48(9) Uiso 1 1 d D
O6 O 0.17053(11) 0.46586(9) -0.06908(19) 0.1308(6) Uani 1 1 d D
H11 H 0.1817 0.4965 -0.0027 0.157 Uiso 1 1 calc R
C1 C 0.37677(6) 0.30273(6) -0.12520(17) 0.0230(3) Uani 1 1 d .
C2 C 0.60810(7) 0.31455(7) -0.22126(15) 0.0231(3) Uani 1 1 d .
C3 C 0.42914(6) 0.31644(7) -0.22664(15) 0.0222(3) Uani 1 1 d .
C4 C 0.49123(7) 0.31219(7) -0.18054(14) 0.0234(3) Uani 1 1 d .
H4 H 0.4997 0.3018 -0.0864 0.028 Uiso 1 1 calc R
C5 C 0.54068(6) 0.32326(7) -0.27341(15) 0.0211(3) Uani 1 1 d .
C6 C 0.52838(7) 0.33900(7) -0.41450(14) 0.0230(3) Uani 1 1 d .
H6 H 0.5615 0.3475 -0.4769 0.028 Uiso 1 1 calc R
C7 C 0.46558(7) 0.34181(7) -0.46090(15) 0.0246(4) Uani 1 1 d .
C8 C 0.41582(6) 0.33110(6) -0.36705(17) 0.0228(3) Uani 1 1 d .
H8 H 0.3741 0.3337 -0.3982 0.027 Uiso 1 1 calc R
C9 C 0.10910(17) 0.47004(19) -0.1217(5) 0.1072(13) Uani 1 1 d D
H9A H 0.0868 0.5032 -0.0730 0.161 Uiso 1 1 calc R
H9B H 0.0876 0.4305 -0.1068 0.161 Uiso 1 1 calc R
H9C H 0.1104 0.4793 -0.2215 0.161 Uiso 1 1 calc R
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'
Pb Pb -3.3944 10.1111 '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 Pb1 O2 73.99(6) . 14_454
O2 Pb1 O4 74.64(4) . 16_444
O2 Pb1 O4 81.78(4) 14_454 16_444
O2 Pb1 O4 81.78(4) . 3_565
O2 Pb1 O4 74.64(4) 14_454 3_565
O4 Pb1 O4 150.41(5) 16_444 3_565
O2 Pb1 Ca1 140.35(3) . 10
O2 Pb1 Ca1 71.83(3) 14_454 10
O4 Pb1 Ca1 81.11(2) 16_444 10
O4 Pb1 Ca1 107.52(2) 3_565 10
O2 Pb1 Ca1 71.83(3) . .
O2 Pb1 Ca1 140.35(3) 14_454 .
O4 Pb1 Ca1 107.52(2) 16_444 .
O4 Pb1 Ca1 81.11(2) 3_565 .
Ca1 Pb1 Ca1 146.669(3) 10 .
O3 Ca1 O3 171.53(6) 7_564 3_565
O3 Ca1 O1 83.91(4) 7_564 5_554
O3 Ca1 O1 89.70(4) 3_565 5_554
O3 Ca1 O1 89.70(4) 7_564 .
O3 Ca1 O1 83.91(4) 3_565 .
O1 Ca1 O1 82.21(6) 5_554 .
O3 Ca1 O6 94.02(5) 7_564 5_554
O3 Ca1 O6 91.61(5) 3_565 5_554
O1 Ca1 O6 172.46(6) 5_554 5_554
O1 Ca1 O6 90.54(6) . 5_554
O3 Ca1 O6 91.61(5) 7_564 .
O3 Ca1 O6 94.02(5) 3_565 .
O1 Ca1 O6 90.54(6) 5_554 .
O1 Ca1 O6 172.46(6) . .
O6 Ca1 O6 96.78(10) 5_554 .
O3 Ca1 Pb1 45.04(3) 7_564 10_554
O3 Ca1 Pb1 126.53(3) 3_565 10_554
O1 Ca1 Pb1 49.30(3) 5_554 10_554
O1 Ca1 Pb1 61.09(3) . 10_554
O6 Ca1 Pb1 124.94(5) 5_554 10_554
O6 Ca1 Pb1 115.35(5) . 10_554
O3 Ca1 Pb1 126.53(3) 7_564 .
O3 Ca1 Pb1 45.04(3) 3_565 .
O1 Ca1 Pb1 61.09(3) 5_554 .
O1 Ca1 Pb1 49.30(3) . .
O6 Ca1 Pb1 115.35(5) 5_554 .
O6 Ca1 Pb1 124.94(5) . .
Pb1 Ca1 Pb1 82.207(7) 10_554 .
C1 O1 Ca1 129.16(10) . .
C1 O2 Pb1 111.29(9) . .
C2 O3 Ca1 164.08(10) . 4_655
C2 O4 Pb1 100.01(9) . 4_655
C7 O5 H10 129.6(8) . .
C9 O6 Ca1 128.9(2) . .
C9 O6 H11 115.6 . .
Ca1 O6 H11 115.6 . .
O2 C1 O1 123.39(13) . .
O2 C1 C3 117.33(12) . .
O1 C1 C3 119.28(13) . .
O4 C2 O3 122.46(13) . .
O4 C2 C5 119.82(13) . .
O3 C2 C5 117.71(13) . .
C4 C3 C8 120.37(13) . .
C4 C3 C1 119.34(13) . .
C8 C3 C1 120.25(12) . .
C5 C4 C3 120.46(13) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C6 120.15(13) . .
C4 C5 C2 118.97(12) . .
C6 C5 C2 120.80(12) . .
C5 C6 C7 119.00(13) . .
C5 C6 H6 120.5 . .
C7 C6 H6 120.5 . .
O5 C7 C8 121.35(13) . .
O5 C7 C6 117.86(13) . .
C8 C7 C6 120.77(13) . .
C3 C8 C7 119.22(12) . .
C3 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
O6 C9 H9A 109.5 . .
O6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O2 2.3260(11) .
Pb1 O2 2.3260(11) 14_454
Pb1 O4 2.6684(11) 16_444
Pb1 O4 2.6684(11) 3_565
Pb1 Ca1 3.9763(3) 10
Pb1 Ca1 3.9763(3) .
Ca1 O3 2.3032(11) 7_564
Ca1 O3 2.3032(11) 3_565
Ca1 O1 2.3223(12) 5_554
Ca1 O1 2.3223(12) .
Ca1 O6 2.352(2) 5_554
Ca1 O6 2.352(2) .
Ca1 Pb1 3.9763(3) 10_554
O1 C1 1.2664(17) .
O2 C1 1.2642(19) .
O3 C2 1.2599(18) .
O3 Ca1 2.3032(11) 4_655
O4 C2 1.2520(18) .
O4 Pb1 2.6684(11) 4_655
O5 C7 1.3616(17) .
O5 H10 1.002(10) .
O6 C9 1.391(4) .
O6 H11 0.9300 .
C1 C3 1.489(2) .
C2 C5 1.517(2) .
C3 C4 1.3840(19) .
C3 C8 1.386(2) .
C4 C5 1.381(2) .
C4 H4 0.9300 .
C5 C6 1.3930(19) .
C6 C7 1.397(2) .
C6 H6 0.9300 .
C7 C8 1.391(2) .
C8 H8 0.9300 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
