#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179385 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/82/4328225.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_4328225
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 Gd2 O16 P2'
_chemical_formula_weight         1174.07
_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                 107.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.528(3)
_cell_length_b                   10.497(2)
_cell_length_c                   23.674(8)
_cell_measurement_reflns_used    10978
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.1397
_cell_volume                     3434.2(16)
_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 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ (2x2 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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0460
_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       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28856
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.44
_diffrn_standards_number         8269
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.7665
_exptl_absorpt_correction_T_min  0.7140
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1138
_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         1.231
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0355
_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)+(0.0324P)²+5.6848P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                7128
_reflns_number_total             7859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202082w_si_003_04.cif
_cod_data_source_block           Gd
_cod_original_cell_volume        3434.2(15)
_cod_database_code               4328225
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
Gd1 Gd 0.349541(12) -0.580023(17) -0.225912(7) 0.01637(6) Uani 1 1 d .
C1 C 0.1460(3) -0.4159(4) -0.14650(16) 0.0201(7) Uani 1 1 d .
C2 C 0.1195(3) -0.5448(4) -0.15162(17) 0.0252(8) Uani 1 1 d .
H2 H 0.1668 -0.6076 -0.1410 0.030 Uiso 1 1 calc R
C3 C 0.0235(3) -0.5779(4) -0.17240(18) 0.0250(8) Uani 1 1 d .
H3 H 0.0063 -0.6636 -0.1758 0.030 Uiso 1 1 calc R
C4 C -0.0485(3) -0.4852(4) -0.18850(16) 0.0213(7) Uani 1 1 d .
C5 C -0.0225(3) -0.3583(4) -0.18272(18) 0.0272(8) Uani 1 1 d .
H5 H -0.0704 -0.2960 -0.1930 0.033 Uiso 1 1 calc R
C6 C 0.0744(3) -0.3218(4) -0.16171(17) 0.0248(8) Uani 1 1 d .
H6 H 0.0913 -0.2360 -0.1579 0.030 Uiso 1 1 calc R
C7 C -0.1525(3) -0.5194(4) -0.21465(16) 0.0228(8) Uani 1 1 d .
C8 C 0.2863(3) -0.2129(3) -0.13794(16) 0.0198(7) Uani 1 1 d .
C9 C 0.2861(4) -0.1150(4) -0.0991(2) 0.0405(12) Uani 1 1 d .
H9 H 0.2768 -0.1326 -0.0628 0.049 Uiso 1 1 calc R
C10 C 0.2999(4) 0.0106(4) -0.1145(2) 0.0402(11) Uani 1 1 d .
H10 H 0.2997 0.0768 -0.0884 0.048 Uiso 1 1 calc R
C11 C 0.3141(3) 0.0367(4) -0.16918(18) 0.0237(8) Uani 1 1 d .
C12 C 0.3130(3) -0.0631(3) -0.20806(19) 0.0293(9) Uani 1 1 d .
H12 H 0.3215 -0.0461 -0.2447 0.035 Uiso 1 1 calc R
C13 C 0.2996(3) -0.1871(4) -0.19273(18) 0.0289(9) Uani 1 1 d .
H13 H 0.2993 -0.2533 -0.2189 0.035 Uiso 1 1 calc R
C14 C 0.3285(3) 0.1700(3) -0.18641(17) 0.0228(8) Uani 1 1 d .
C15 C 0.3090(3) -0.3855(3) -0.04110(16) 0.0197(7) Uani 1 1 d .
C16 C 0.4071(3) -0.3751(4) -0.00950(18) 0.0304(9) Uani 1 1 d .
H16 H 0.4522 -0.3685 -0.0300 0.036 Uiso 1 1 calc R
C17 C 0.4380(3) -0.3744(4) 0.05153(17) 0.0295(9) Uani 1 1 d .
H17 H 0.5036 -0.3669 0.0720 0.035 Uiso 1 1 calc R
C18 C 0.3715(3) -0.3848(3) 0.08265(15) 0.0182(7) Uani 1 1 d .
C19 C 0.2745(3) -0.3979(5) 0.05187(18) 0.0344(10) Uani 1 1 d .
H19 H 0.2299 -0.4069 0.0725 0.041 Uiso 1 1 calc R
C20 C 0.2432(3) -0.3980(5) -0.00956(18) 0.0329(10) Uani 1 1 d .
H20 H 0.1776 -0.4064 -0.0299 0.039 Uiso 1 1 calc R
C21 C 0.4039(3) -0.3800(3) 0.14942(16) 0.0204(7) Uani 1 1 d .
C22 C 0.5000 -0.3516(7) -0.2500 0.087(4) Uani 1 2 d S
H22 H 0.5000 -0.2630 -0.2500 0.104 Uiso 1 2 calc SR
O1 O -0.17597(19) -0.6341(3) -0.23152(12) 0.0264(6) Uani 1 1 d .
O2 O -0.21666(18) -0.4353(2) -0.22167(12) 0.0238(6) Uani 1 1 d .
O3 O 0.3210(2) 0.2627(3) -0.15412(12) 0.0280(6) Uani 1 1 d .
O4 O 0.34888(19) 0.1899(2) -0.23436(12) 0.0231(6) Uani 1 1 d .
O5 O 0.49278(19) -0.3720(3) 0.17589(12) 0.0276(6) Uani 1 1 d .
O6 O 0.3397(2) -0.3810(3) 0.17465(12) 0.0282(6) Uani 1 1 d .
O7 O 0.33158(18) -0.4633(2) -0.14620(11) 0.0194(5) Uani 1 1 d .
O8 O 0.4273(2) -0.3971(3) -0.24313(14) 0.0325(7) Uani 1 1 d .
P1 P 0.27241(7) -0.37693(9) -0.12036(4) 0.01676(18) 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'
Gd Gd -0.1653 3.9035 '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'
H H 0.0000 0.0000 '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
O5 Gd1 O8 78.99(11) 3_645 .
O5 Gd1 O7 92.34(10) 3_645 .
O8 Gd1 O7 83.67(10) . .
O5 Gd1 O6 102.83(10) 3_645 4_545
O8 Gd1 O6 81.43(11) . 4_545
O7 Gd1 O6 156.21(10) . 4_545
O5 Gd1 O4 78.54(10) 3_645 1_545
O8 Gd1 O4 142.90(9) . 1_545
O7 Gd1 O4 126.32(9) . 1_545
O6 Gd1 O4 75.30(9) 4_545 1_545
O5 Gd1 O2 153.98(10) 3_645 2_554
O8 Gd1 O2 75.59(10) . 2_554
O7 Gd1 O2 79.51(9) . 2_554
O6 Gd1 O2 78.89(10) 4_545 2_554
O4 Gd1 O2 126.10(9) 1_545 2_554
O5 Gd1 O1 153.15(10) 3_645 2_554
O8 Gd1 O1 127.36(10) . 2_554
O7 Gd1 O1 95.49(9) . 2_554
O6 Gd1 O1 79.21(10) 4_545 2_554
O4 Gd1 O1 76.13(9) 1_545 2_554
O2 Gd1 O1 52.86(9) 2_554 2_554
O5 Gd1 O3 81.49(10) 3_645 1_545
O8 Gd1 O3 149.02(10) . 1_545
O7 Gd1 O3 73.31(9) . 1_545
O6 Gd1 O3 126.57(10) 4_545 1_545
O4 Gd1 O3 53.08(9) 1_545 1_545
O2 Gd1 O3 118.76(9) 2_554 1_545
O1 Gd1 O3 76.29(10) 2_554 1_545
O5 Gd1 C14 79.52(11) 3_645 1_545
O8 Gd1 C14 158.36(11) . 1_545
O7 Gd1 C14 99.75(10) . 1_545
O6 Gd1 C14 100.94(11) 4_545 1_545
O4 Gd1 C14 26.65(9) 1_545 1_545
O2 Gd1 C14 126.05(10) 2_554 1_545
O1 Gd1 C14 73.86(10) 2_554 1_545
O3 Gd1 C14 26.45(10) 1_545 1_545
O5 Gd1 C7 178.56(10) 3_645 2_554
O8 Gd1 C7 101.41(11) . 2_554
O7 Gd1 C7 86.33(10) . 2_554
O6 Gd1 C7 78.61(10) 4_545 2_554
O4 Gd1 C7 101.79(10) 1_545 2_554
O2 Gd1 C7 26.16(10) 2_554 2_554
O1 Gd1 C7 26.73(10) 2_554 2_554
O3 Gd1 C7 97.57(11) 1_545 2_554
C14 Gd1 C7 100.13(11) 1_545 2_554
C6 C1 C2 119.8(4) . .
C6 C1 P1 121.9(3) . .
C2 C1 P1 118.3(3) . .
C3 C2 C1 119.8(4) . .
C3 C2 H2 120.1 . .
C1 C2 H2 120.1 . .
C2 C3 C4 121.0(4) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C5 C4 C3 119.2(3) . .
C5 C4 C7 119.0(3) . .
C3 C4 C7 121.7(3) . .
C4 C5 C6 121.0(4) . .
C4 C5 H5 119.5 . .
C6 C5 H5 119.5 . .
C5 C6 C1 119.1(4) . .
C5 C6 H6 120.4 . .
C1 C6 H6 120.4 . .
O2 C7 O1 120.3(3) . .
O2 C7 C4 120.1(4) . .
O1 C7 C4 119.6(3) . .
O2 C7 Gd1 60.01(19) . 2_554
O1 C7 Gd1 60.37(19) . 2_554
C4 C7 Gd1 175.2(3) . 2_554
C9 C8 C13 120.3(4) . .
C9 C8 P1 122.4(3) . .
C13 C8 P1 117.3(3) . .
C8 C9 C10 120.0(4) . .
C8 C9 H9 120.0 . .
C10 C9 H9 120.0 . .
C9 C10 C11 119.9(4) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C12 C11 C10 119.4(4) . .
C12 C11 C14 120.0(3) . .
C10 C11 C14 120.6(4) . .
C13 C12 C11 120.6(4) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C12 C13 C8 119.9(4) . .
C12 C13 H13 120.1 . .
C8 C13 H13 120.1 . .
O3 C14 O4 120.0(3) . .
O3 C14 C11 120.8(3) . .
O4 C14 C11 119.2(3) . .
O3 C14 Gd1 61.6(2) . 1_565
O4 C14 Gd1 58.44(18) . 1_565
C11 C14 Gd1 176.7(3) . 1_565
C20 C15 C16 118.6(3) . .
C20 C15 P1 122.6(3) . .
C16 C15 P1 118.8(3) . .
C17 C16 C15 120.8(4) . .
C17 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
C16 C17 C18 120.2(4) . .
C16 C17 H17 119.9 . .
C18 C17 H17 119.9 . .
C19 C18 C17 119.5(3) . .
C19 C18 C21 119.7(3) . .
C17 C18 C21 120.8(3) . .
C18 C19 C20 120.4(4) . .
C18 C19 H19 119.8 . .
C20 C19 H19 119.8 . .
C19 C20 C15 120.5(4) . .
C19 C20 H20 119.7 . .
C15 C20 H20 119.7 . .
O6 C21 O5 124.5(4) . .
O6 C21 C18 117.6(3) . .
O5 C21 C18 117.9(3) . .
O8 C22 O8 133.6(7) . 2_654
O8 C22 H22 113.2 . .
O8 C22 H22 113.2 2_654 .
C7 O1 Gd1 92.9(2) . 2_554
C7 O2 Gd1 93.8(2) . 2_554
C14 O3 Gd1 92.0(2) . 1_565
C14 O4 Gd1 94.9(2) . 1_565
C21 O5 Gd1 163.4(3) . 3_645
C21 O6 Gd1 130.9(3) . 4_546
P1 O7 Gd1 150.15(15) . .
C22 O8 Gd1 146.9(4) . .
O7 P1 C15 112.03(16) . .
O7 P1 C1 112.03(16) . .
C15 P1 C1 106.93(17) . .
O7 P1 C8 111.34(16) . .
C15 P1 C8 105.83(17) . .
C1 P1 C8 108.36(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O5 2.287(3) 3_645
Gd1 O8 2.327(3) .
Gd1 O7 2.331(2) .
Gd1 O6 2.350(3) 4_545
Gd1 O4 2.424(3) 1_545
Gd1 O2 2.469(3) 2_554
Gd1 O1 2.476(3) 2_554
Gd1 O3 2.494(3) 1_545
Gd1 C14 2.834(4) 1_545
Gd1 C7 2.844(4) 2_554
C1 C6 1.398(5) .
C1 C2 1.401(5) .
C1 P1 1.795(4) .
C2 C3 1.372(5) .
C2 H2 0.9300 .
C3 C4 1.394(5) .
C3 H3 0.9300 .
C4 C5 1.380(6) .
C4 C7 1.490(5) .
C5 C6 1.395(5) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O2 1.257(5) .
C7 O1 1.281(5) .
C7 Gd1 2.844(4) 2_554
C8 C9 1.379(5) .
C8 C13 1.395(5) .
C8 P1 1.797(4) .
C9 C10 1.399(6) .
C9 H9 0.9300 .
C10 C11 1.400(5) .
C10 H10 0.9300 .
C11 C12 1.391(5) .
C11 C14 1.490(5) .
C12 C13 1.382(5) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 O3 1.263(4) .
C14 O4 1.276(4) .
C14 Gd1 2.834(4) 1_565
C15 C20 1.388(5) .
C15 C16 1.396(5) .
C15 P1 1.788(4) .
C16 C17 1.374(5) .
C16 H16 0.9300 .
C17 C18 1.388(5) .
C17 H17 0.9300 .
C18 C19 1.379(5) .
C18 C21 1.504(5) .
C19 C20 1.383(6) .
C19 H19 0.9300 .
C20 H20 0.9300 .
C21 O6 1.253(4) .
C21 O5 1.253(4) .
C22 O8 1.215(4) .
C22 O8 1.215(4) 2_654
C22 H22 0.9300 .
O1 Gd1 2.476(3) 2_554
O2 Gd1 2.469(3) 2_554
O3 Gd1 2.494(3) 1_565
O4 Gd1 2.424(3) 1_565
O5 Gd1 2.287(3) 3_645
O6 Gd1 2.350(3) 4_546
O7 P1 1.503(3) .
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 -0.005 -0.003 0.001 1744.1 548.1
