#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:10:02 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179616 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/80/4508086.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_4508086
loop_
_publ_author_name
'Liu, Yi-Fu'
'Hou, Guang-Feng'
'Yu, Ying-Hui'
'Yan, Peng-Fei'
'Li, Jian-Yue'
'Li, Guang-Ming'
'Gao, Jin-Sheng'
_publ_section_title
;
 pH-Dependent Syntheses, Luminescent, and Magnetic Properties of
 Two-Dimensional Framework Lanthanide Carboxyarylphosphonate Complexes
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3816
_journal_paper_doi               10.1021/cg400877g
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C16 H17 Nd O11 P2'
_chemical_formula_sum            'C16 H17 Nd O11 P2'
_chemical_formula_weight         591.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.68(3)
_cell_angle_beta                 92.60(3)
_cell_angle_gamma                97.38(3)
_cell_formula_units_Z            2
_cell_length_a                   5.7280(11)
_cell_length_b                   9.5108(19)
_cell_length_c                   18.379(4)
_cell_measurement_reflns_used    8811
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      3.45
_cell_volume                     957.4(4)
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9414
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.940
_exptl_absorpt_correction_T_max  0.6735
_exptl_absorpt_correction_T_min  0.4858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0135P)²+0.6903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                4080
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400877g_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        957.4(3)
_cod_database_code               4508086
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.2691(4) 1.0983(3) 0.25551(13) 0.0212(5) Uani 1 1 d .
C2 C 0.4298(5) 1.0861(3) 0.31207(15) 0.0303(6) Uani 1 1 d .
H2 H 0.5854 1.1309 0.3151 0.036 Uiso 1 1 calc R
C3 C 0.3620(5) 1.0083(3) 0.36406(16) 0.0334(6) Uani 1 1 d .
H3 H 0.4717 1.0019 0.4015 0.040 Uiso 1 1 calc R
C4 C 0.1322(5) 0.9406(3) 0.36027(14) 0.0243(5) Uani 1 1 d .
C5 C -0.0303(5) 0.9496(3) 0.30334(14) 0.0274(5) Uani 1 1 d .
H5 H -0.1850 0.9030 0.2999 0.033 Uiso 1 1 calc R
C6 C 0.0389(5) 1.0283(3) 0.25160(14) 0.0266(5) Uani 1 1 d .
H6 H -0.0705 1.0340 0.2139 0.032 Uiso 1 1 calc R
C7 C 0.3494(5) 1.1929(3) 0.20398(13) 0.0230(5) Uani 1 1 d .
H7A H 0.4994 1.2510 0.2261 0.028 Uiso 1 1 calc R
H7B H 0.2367 1.2609 0.2042 0.028 Uiso 1 1 calc R
C8 C 0.0618(5) 0.8611(3) 0.41797(14) 0.0279(5) Uani 1 1 d .
C9 C 0.1834(4) 0.5773(3) 0.26143(12) 0.0205(5) Uani 1 1 d .
C10 C 0.3686(5) 0.5823(3) 0.31458(14) 0.0275(5) Uani 1 1 d .
H10 H 0.5157 0.6346 0.3123 0.033 Uiso 1 1 calc R
C11 C 0.3344(5) 0.5095(3) 0.37103(15) 0.0295(6) Uani 1 1 d .
H11 H 0.4589 0.5133 0.4061 0.035 Uiso 1 1 calc R
C12 C 0.1166(5) 0.4318(3) 0.37519(13) 0.0243(5) Uani 1 1 d .
C13 C -0.0694(5) 0.4278(3) 0.32258(15) 0.0296(6) Uani 1 1 d .
H13 H -0.2170 0.3767 0.3254 0.036 Uiso 1 1 calc R
C14 C -0.0354(5) 0.4993(3) 0.26635(14) 0.0281(6) Uani 1 1 d .
H14 H -0.1603 0.4952 0.2314 0.034 Uiso 1 1 calc R
C15 C 0.2149(5) 0.6545(3) 0.19941(13) 0.0223(5) Uani 1 1 d .
H15A H 0.3494 0.7316 0.2147 0.027 Uiso 1 1 calc R
H15B H 0.0764 0.7010 0.1940 0.027 Uiso 1 1 calc R
C16 C 0.0737(5) 0.3507(3) 0.43408(14) 0.0284(6) Uani 1 1 d .
Nd1 Nd 0.124627(19) 0.804643(12) 0.000552(6) 0.01242(4) Uani 1 1 d .
O1 O 0.4600(3) 0.95198(17) 0.09534(9) 0.0218(4) Uani 1 1 d .
O2 O 0.1435(3) 1.07578(17) 0.06060(9) 0.0180(3) Uani 1 1 d .
O3 O 0.5661(3) 1.21128(18) 0.08107(9) 0.0209(3) Uani 1 1 d .
O4 O 0.2202(4) 0.8625(3) 0.46859(13) 0.0546(7) Uani 1 1 d .
H4 H 0.1659 0.8147 0.4969 0.082 Uiso 1 1 calc R
O5 O -0.1472(4) 0.7965(3) 0.41403(12) 0.0453(6) Uani 1 1 d .
O6 O 0.2549(3) 0.62810(18) 0.05207(9) 0.0227(4) Uani 1 1 d .
O7 O 0.5212(3) 0.50303(19) 0.11793(10) 0.0244(4) Uani 1 1 d .
H7 H 0.5205 0.4138 0.1068 0.037 Uiso 1 1 calc R
O8 O 0.0891(3) 0.39681(17) 0.08957(9) 0.0209(3) Uani 1 1 d .
O9 O 0.2421(4) 0.3497(3) 0.48059(13) 0.0496(6) Uani 1 1 d .
H9 H 0.1936 0.3051 0.5109 0.074 Uiso 1 1 calc R
O10 O -0.1315(4) 0.2865(3) 0.43456(13) 0.0547(7) Uani 1 1 d .
O11 O -0.2036(3) 0.7733(2) 0.08108(10) 0.0269(4) Uani 1 1 d .
H111 H -0.2741 0.6894 0.0841 0.040 Uiso 1 1 d R
H112 H -0.3165 0.8256 0.0858 0.040 Uiso 1 1 d R
P1 P 0.38579(9) 1.10390(6) 0.10648(3) 0.01293(11) Uani 1 1 d .
P2 P 0.25945(10) 0.53742(6) 0.10847(3) 0.01393(11) 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'
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'
Nd Nd -0.1943 3.0179 '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
C6 C1 C2 118.2(2) . .
C6 C1 C7 123.0(2) . .
C2 C1 C7 118.7(2) . .
C3 C2 C1 121.2(3) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C4 C3 C2 120.2(2) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
C3 C4 C5 119.4(2) . .
C3 C4 C8 119.2(2) . .
C5 C4 C8 121.4(2) . .
C6 C5 C4 120.0(2) . .
C6 C5 H5 120.0 . .
C4 C5 H5 120.0 . .
C1 C6 C5 120.9(2) . .
C1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C1 C7 P1 118.57(17) . .
C1 C7 H7A 107.7 . .
P1 C7 H7A 107.7 . .
C1 C7 H7B 107.7 . .
P1 C7 H7B 107.7 . .
H7A C7 H7B 107.1 . .
O5 C8 O4 123.8(2) . .
O5 C8 C4 119.6(2) . .
O4 C8 C4 116.7(2) . .
C14 C9 C10 118.7(2) . .
C14 C9 C15 119.5(2) . .
C10 C9 C15 121.7(2) . .
C11 C10 C9 120.4(2) . .
C11 C10 H10 119.8 . .
C9 C10 H10 119.8 . .
C12 C11 C10 120.4(2) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C13 119.3(2) . .
C11 C12 C16 122.0(2) . .
C13 C12 C16 118.7(2) . .
C14 C13 C12 120.4(2) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C9 120.8(2) . .
C13 C14 H14 119.6 . .
C9 C14 H14 119.6 . .
C9 C15 P2 114.98(16) . .
C9 C15 H15A 108.5 . .
P2 C15 H15A 108.5 . .
C9 C15 H15B 108.5 . .
P2 C15 H15B 108.5 . .
H15A C15 H15B 107.5 . .
O10 C16 O9 123.3(2) . .
O10 C16 C12 117.4(2) . .
O9 C16 C12 119.3(3) . .
O6 Nd1 O8 84.52(6) . 2_565
O6 Nd1 O3 90.79(6) . 2_675
O8 Nd1 O3 87.15(6) 2_565 2_675
O6 Nd1 O2 158.67(6) . 2_575
O8 Nd1 O2 78.66(6) 2_565 2_575
O3 Nd1 O2 101.28(6) 2_675 2_575
O6 Nd1 O11 81.41(6) . .
O8 Nd1 O11 85.60(7) 2_565 .
O3 Nd1 O11 169.82(6) 2_675 .
O2 Nd1 O11 84.30(6) 2_575 .
O6 Nd1 O2 128.43(6) . .
O8 Nd1 O2 143.85(5) 2_565 .
O3 Nd1 O2 104.53(6) 2_675 .
O2 Nd1 O2 65.62(6) 2_575 .
O11 Nd1 O2 85.50(6) . .
O6 Nd1 O1 77.47(6) . .
O8 Nd1 O1 158.51(6) 2_565 .
O3 Nd1 O1 81.54(6) 2_675 .
O2 Nd1 O1 121.39(5) 2_575 .
O11 Nd1 O1 102.96(6) . .
O2 Nd1 O1 57.37(5) . .
O6 Nd1 P1 103.92(5) . .
O8 Nd1 P1 171.50(4) 2_565 .
O3 Nd1 P1 91.67(5) 2_675 .
O2 Nd1 P1 93.34(4) 2_575 .
O11 Nd1 P1 96.53(5) . .
O2 Nd1 P1 28.95(4) . .
O1 Nd1 P1 28.52(4) . .
P1 O1 Nd1 98.77(8) . .
P1 O2 Nd1 142.32(9) . 2_575
P1 O2 Nd1 98.97(8) . .
Nd1 O2 Nd1 114.38(6) 2_575 .
P1 O3 Nd1 136.80(10) . 2_675
C8 O4 H4 109.5 . .
P2 O6 Nd1 154.66(11) . .
P2 O7 H7 109.5 . .
P2 O8 Nd1 150.03(10) . 2_565
C16 O9 H9 109.5 . .
Nd1 O11 H111 124.3 . .
Nd1 O11 H112 123.0 . .
H111 O11 H112 102.3 . .
O1 P1 O3 112.80(10) . .
O1 P1 O2 104.55(9) . .
O3 P1 O2 112.31(9) . .
O1 P1 C7 113.46(11) . .
O3 P1 C7 105.15(11) . .
O2 P1 C7 108.67(11) . .
O1 P1 Nd1 52.71(6) . .
O3 P1 Nd1 124.59(7) . .
O2 P1 Nd1 52.09(6) . .
C7 P1 Nd1 130.14(9) . .
O8 P2 O6 115.77(10) . .
O8 P2 O7 109.80(10) . .
O6 P2 O7 107.56(10) . .
O8 P2 C15 111.38(11) . .
O6 P2 C15 107.43(10) . .
O7 P2 C15 104.21(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.389(4) .
C1 C2 1.394(3) .
C1 C7 1.511(3) .
C2 C3 1.389(4) .
C2 H2 0.9300 .
C3 C4 1.380(4) .
C3 H3 0.9300 .
C4 C5 1.395(3) .
C4 C8 1.491(3) .
C5 C6 1.393(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 P1 1.812(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 O5 1.263(3) .
C8 O4 1.266(3) .
C9 C14 1.391(4) .
C9 C10 1.397(3) .
C9 C15 1.510(3) .
C10 C11 1.393(4) .
C10 H10 0.9300 .
C11 C12 1.382(4) .
C11 H11 0.9300 .
C12 C13 1.396(3) .
C12 C16 1.491(3) .
C13 C14 1.381(4) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 P2 1.807(2) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 O10 1.254(4) .
C16 O9 1.262(3) .
Nd1 O6 2.3099(16) .
Nd1 O8 2.3492(18) 2_565
Nd1 O3 2.3677(18) 2_675
Nd1 O2 2.4198(16) 2_575
Nd1 O11 2.4792(19) .
Nd1 O2 2.5209(17) .
Nd1 O1 2.5407(19) .
Nd1 P1 3.1563(14) .
O1 P1 1.5251(16) .
O2 P1 1.5467(16) .
O2 Nd1 2.4198(16) 2_575
O3 P1 1.5306(18) .
O3 Nd1 2.3677(18) 2_675
O4 H4 0.8200 .
O6 P2 1.5085(16) .
O7 P2 1.5860(17) .
O7 H7 0.8200 .
O8 P2 1.5031(17) .
O8 Nd1 2.3492(18) 2_565
O9 H9 0.8200 .
O11 H111 0.8622 .
O11 H112 0.8602 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O10 0.82 1.77 2.572(3) 164.3 2_566
O7 H7 O3 0.82 1.92 2.733(2) 171.9 1_545
O9 H9 O5 0.82 1.88 2.692(3) 168.5 2_566
O11 H111 O7 0.86 2.24 3.080(3) 166.5 1_455
O11 H112 O1 0.86 1.85 2.708(2) 175.0 1_455
