#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179385 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/82/4328232.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_4328232
loop_
_publ_author_name
'Zu-Jin Lin'
'Zhen Yang'
'Tian-Fu Liu'
'Yuan-Biao Huang'
'Rong Cao'
_publ_contact_author_address
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China
;
_publ_contact_author_email       linzujin@fjirsm.ac.cn
_publ_contact_author_fax         +86-0591-83796710
_publ_contact_author_name        'Zujin Lin'
_publ_contact_author_phone       +86-0591-83725186
_publ_section_title
;
 Microwave-Assisted Synthesis of a Series of Lanthanide Metal-Organic
 Frameworks and Gas Sorption Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1813
_journal_page_last               1820
_journal_paper_doi               10.1021/ic202082w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C43 H25 Lu2 O16 P2'
_chemical_formula_weight         1209.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 107.052(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.4262(11)
_cell_length_b                   10.4932(5)
_cell_length_c                   23.2269(18)
_cell_measurement_reflns_used    9126
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4797
_cell_measurement_theta_min      2.1463
_cell_volume                     3361.5(4)
_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_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Mercury2 (1x1 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25992
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         8110
_exptl_absorpt_coefficient_mu    3.014
_exptl_absorpt_correction_T_max  0.6777
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
;
_refine_diff_density_max         1.158
_refine_diff_density_min         -2.089
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         7696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0384
_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)+(0.0685P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                6754
_reflns_number_total             7696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202082w_si_003_11.cif
_cod_data_source_block           Lu
_cod_database_code               4328232
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Lu1 Lu 0.153365(11) 0.066027(16) 0.227224(7) 0.02431(8) Uani 1 1 d .
C17 C 0.4820(4) 0.0602(4) 0.1723(3) 0.0462(14) Uani 1 1 d .
H17 H 0.4995 0.1458 0.1761 0.055 Uiso 1 1 calc R
P1 P 0.23118(7) -0.13845(10) 0.12253(5) 0.0244(2) Uani 1 1 d .
O7 O 0.1737(2) -0.0514(3) 0.15047(14) 0.0296(7) Uani 1 1 d .
O4 O 0.1553(2) -0.7077(3) 0.23701(15) 0.0385(8) Uani 1 1 d .
O6 O 0.7219(2) -0.0794(3) 0.21973(17) 0.0395(8) Uani 1 1 d .
O5 O 0.6801(2) 0.1160(4) 0.22931(16) 0.0426(8) Uani 1 1 d .
O2 O -0.0048(2) -0.1207(4) -0.17480(15) 0.0439(8) Uani 1 1 d .
O3 O 0.1891(3) -0.7800(3) 0.15676(16) 0.0415(8) Uani 1 1 d .
O1 O 0.1455(2) -0.0987(3) -0.17877(14) 0.0395(7) Uani 1 1 d .
C8 C 0.2176(3) -0.3020(4) 0.14105(19) 0.0285(9) Uani 1 1 d .
O8 O 0.0689(2) -0.1116(3) 0.23742(18) 0.0470(9) Uani 1 1 d .
C21 C 0.6577(3) 0.0041(5) 0.2122(2) 0.0322(9) Uani 1 1 d .
C15 C 0.3580(3) -0.1009(4) 0.14596(19) 0.0280(8) Uani 1 1 d .
C1 C 0.1905(3) -0.1283(4) 0.04190(19) 0.0285(8) Uani 1 1 d .
C11 C 0.1936(4) -0.5536(4) 0.1722(2) 0.0352(10) Uani 1 1 d .
C14 C 0.1786(3) -0.6896(4) 0.1890(2) 0.0368(10) Uani 1 1 d .
C18 C 0.5535(3) -0.0318(5) 0.1867(2) 0.0344(10) Uani 1 1 d .
C7 C 0.0847(3) -0.1111(4) -0.15074(18) 0.0283(8) Uani 1 1 d .
C19 C 0.5266(3) -0.1583(5) 0.1788(2) 0.0446(12) Uani 1 1 d .
H19 H 0.5741 -0.2212 0.1869 0.054 Uiso 1 1 calc R
C13 C 0.2018(4) -0.3319(5) 0.1957(2) 0.0485(13) Uani 1 1 d .
H13 H 0.1988 -0.2668 0.2223 0.058 Uiso 1 1 calc R
C12 C 0.1909(5) -0.4541(5) 0.2108(3) 0.0514(14) Uani 1 1 d .
H12 H 0.1814 -0.4718 0.2479 0.062 Uiso 1 1 calc R
C20 C 0.4300(3) -0.1927(5) 0.1592(2) 0.0427(11) Uani 1 1 d .
H20 H 0.4131 -0.2785 0.1547 0.051 Uiso 1 1 calc R
C16 C 0.3861(3) 0.0283(4) 0.1526(2) 0.0363(10) Uani 1 1 d .
H16 H 0.3392 0.0920 0.1436 0.044 Uiso 1 1 calc R
C3 C 0.2185(4) -0.1123(7) -0.0541(2) 0.0540(14) Uani 1 1 d .
H3 H 0.2619 -0.1062 -0.0767 0.065 Uiso 1 1 calc R
C10 C 0.2111(5) -0.5263(5) 0.1184(3) 0.0621(17) Uani 1 1 d .
H10 H 0.2148 -0.5923 0.0925 0.075 Uiso 1 1 calc R
C2 C 0.2542(3) -0.1188(6) 0.0079(2) 0.0514(14) Uani 1 1 d .
H2 H 0.3207 -0.1167 0.0265 0.062 Uiso 1 1 calc R
C9 C 0.2233(5) -0.4009(5) 0.1024(3) 0.0535(15) Uani 1 1 d .
H9 H 0.2353 -0.3834 0.0659 0.064 Uiso 1 1 calc R
C5 C 0.0578(3) -0.1237(6) -0.0493(2) 0.0513(14) Uani 1 1 d .
H5 H -0.0086 -0.1263 -0.0683 0.062 Uiso 1 1 calc R
C6 C 0.0918(3) -0.1289(6) 0.0128(2) 0.0516(14) Uani 1 1 d .
H6 H 0.0481 -0.1328 0.0352 0.062 Uiso 1 1 calc R
C4 C 0.1212(3) -0.1148(4) -0.08314(18) 0.0281(8) Uani 1 1 d .
C22 C 0.0000 -0.1555(8) 0.2500 0.076(3) Uani 1 2 d S
H22 H 0.0000 -0.2442 0.2500 0.091 Uiso 1 2 calc SR
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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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 Lu1 O1 100.30(13) 3 4_556
O2 Lu1 O7 92.07(13) 3 .
O1 Lu1 O7 155.10(12) 4_556 .
O2 Lu1 O8 78.91(14) 3 .
O1 Lu1 O8 80.95(13) 4_556 .
O7 Lu1 O8 80.35(12) . .
O2 Lu1 O5 150.94(15) 3 2_655
O1 Lu1 O5 83.48(13) 4_556 2_655
O7 Lu1 O5 96.13(12) . 2_655
O8 Lu1 O5 129.93(13) . 2_655
O2 Lu1 O4 77.08(13) 3 1_565
O1 Lu1 O4 75.99(12) 4_556 1_565
O7 Lu1 O4 128.22(11) . 1_565
O8 Lu1 O4 142.85(12) . 1_565
O5 Lu1 O4 75.95(12) 2_655 1_565
O2 Lu1 O6 155.07(13) 3 2_655
O1 Lu1 O6 80.93(13) 4_556 2_655
O7 Lu1 O6 78.88(12) . 2_655
O8 Lu1 O6 76.70(12) . 2_655
O5 Lu1 O6 53.91(12) 2_655 2_655
O4 Lu1 O6 126.64(11) 1_565 2_655
O2 Lu1 O3 79.71(13) 3 1_565
O1 Lu1 O3 128.82(12) 4_556 1_565
O7 Lu1 O3 74.45(11) . 1_565
O8 Lu1 O3 146.10(13) . 1_565
O5 Lu1 O3 75.78(12) 2_655 1_565
O4 Lu1 O3 53.87(11) 1_565 1_565
O6 Lu1 O3 119.10(12) 2_655 1_565
O2 Lu1 C21 176.86(13) 3 2_655
O1 Lu1 C21 82.17(13) 4_556 2_655
O7 Lu1 C21 86.37(12) . 2_655
O8 Lu1 C21 103.49(14) . 2_655
O5 Lu1 C21 26.98(14) 2_655 2_655
O4 Lu1 C21 101.76(13) 1_565 2_655
O6 Lu1 C21 26.97(12) 2_655 2_655
O3 Lu1 C21 97.23(13) 1_565 2_655
O2 Lu1 C14 77.32(14) 3 1_565
O1 Lu1 C14 102.66(14) 4_556 1_565
O7 Lu1 C14 101.10(13) . 1_565
O8 Lu1 C14 156.22(13) . 1_565
O5 Lu1 C14 73.76(13) 2_655 1_565
O4 Lu1 C14 27.20(12) 1_565 1_565
O6 Lu1 C14 127.02(12) 2_655 1_565
O3 Lu1 C14 26.67(12) 1_565 1_565
C21 Lu1 C14 100.29(14) 2_655 1_565
C16 C17 C18 121.5(4) . .
O7 P1 C15 112.25(19) . .
O7 P1 C8 111.39(19) . .
C15 P1 C8 108.13(19) . .
O7 P1 C1 111.22(19) . .
C15 P1 C1 107.2(2) . .
C8 P1 C1 106.37(19) . .
P1 O7 Lu1 152.77(19) . .
C14 O4 Lu1 93.7(3) . 1_545
C21 O6 Lu1 92.2(3) . 2_655
C21 O5 Lu1 93.6(3) . 2_655
C7 O2 Lu1 158.9(3) . 3
C14 O3 Lu1 90.8(3) . 1_545
C7 O1 Lu1 140.4(3) . 4
C13 C8 C9 118.6(4) . .
C13 C8 P1 119.6(3) . .
C9 C8 P1 121.8(4) . .
C22 O8 Lu1 147.3(4) . .
O6 C21 O5 120.2(4) . .
O6 C21 C18 119.8(4) . .
O5 C21 C18 119.9(4) . .
O6 C21 Lu1 60.8(2) . 2_655
O5 C21 Lu1 59.5(2) . 2_655
C18 C21 Lu1 173.0(3) . 2_655
C20 C15 C16 118.1(4) . .
C20 C15 P1 123.2(3) . .
C16 C15 P1 118.7(3) . .
C2 C1 C6 118.8(4) . .
C2 C1 P1 122.3(3) . .
C6 C1 P1 118.9(3) . .
C10 C11 C12 118.5(4) . .
C10 C11 C14 120.6(4) . .
C12 C11 C14 120.9(5) . .
O3 C14 O4 121.6(4) . .
O3 C14 C11 120.8(4) . .
O4 C14 C11 117.5(4) . .
O3 C14 Lu1 62.5(2) . 1_545
O4 C14 Lu1 59.1(2) . 1_545
C11 C14 Lu1 176.4(4) . 1_545
C19 C18 C17 118.6(4) . .
C19 C18 C21 120.5(4) . .
C17 C18 C21 120.9(4) . .
O1 C7 O2 124.7(4) . .
O1 C7 C4 117.7(4) . .
O2 C7 C4 117.6(4) . .
C18 C19 C20 120.9(4) . .
C12 C13 C8 120.9(5) . .
C13 C12 C11 121.5(5) . .
C19 C20 C15 120.7(4) . .
C17 C16 C15 120.2(4) . .
C4 C3 C2 121.9(5) . .
C11 C10 C9 120.8(5) . .
C1 C2 C3 119.6(4) . .
C8 C9 C10 119.7(5) . .
C4 C5 C6 120.5(4) . .
C5 C6 C1 120.6(5) . .
C3 C4 C5 118.6(4) . .
C3 C4 C7 120.6(4) . .
C5 C4 C7 120.8(4) . .
O8 C22 O8 135.1(8) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 O2 2.208(3) 3
Lu1 O1 2.246(3) 4_556
Lu1 O7 2.256(3) .
Lu1 O8 2.277(3) .
Lu1 O5 2.376(3) 2_655
Lu1 O4 2.384(3) 1_565
Lu1 O6 2.405(3) 2_655
Lu1 O3 2.460(3) 1_565
Lu1 C21 2.754(4) 2_655
Lu1 C14 2.773(5) 1_565
C17 C16 1.365(7) .
C17 C18 1.381(7) .
P1 O7 1.503(3) .
P1 C15 1.792(4) .
P1 C8 1.794(4) .
P1 C1 1.794(4) .
O4 C14 1.270(6) .
O4 Lu1 2.384(3) 1_545
O6 C21 1.250(5) .
O6 Lu1 2.405(3) 2_655
O5 C21 1.252(6) .
O5 Lu1 2.376(3) 2_655
O2 C7 1.252(5) .
O2 Lu1 2.208(3) 3
O3 C14 1.245(6) .
O3 Lu1 2.460(3) 1_545
O1 C7 1.242(5) .
O1 Lu1 2.246(3) 4
C8 C13 1.390(6) .
C8 C9 1.391(6) .
O8 C22 1.206(4) .
C21 C18 1.493(6) .
C21 Lu1 2.754(4) 2_655
C15 C20 1.384(6) .
C15 C16 1.411(6) .
C1 C2 1.380(6) .
C1 C6 1.386(6) .
C11 C10 1.375(8) .
C11 C12 1.383(7) .
C11 C14 1.511(6) .
C14 Lu1 2.773(5) 1_545
C18 C19 1.380(7) .
C7 C4 1.503(5) .
C19 C20 1.381(6) .
C13 C12 1.351(7) .
C3 C4 1.368(6) .
C3 C2 1.380(7) .
C10 C9 1.393(7) .
C5 C4 1.374(6) .
C5 C6 1.381(7) .
C22 O8 1.206(4) 2
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.419 -0.084 0.431 1770.2 233.0
