#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:42:47 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232910 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/84/4348426.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_4348426
loop_
_publ_author_name
'Ren, Min'
'Bao, Song-Song'
'Wang, Bing-Wu'
'Ferreira, Rute A. S.'
'Zheng, Li-Min'
'Carlos, Luis D.'
_publ_section_title
;
 Lanthanide phosphonates with pseudo-D5h local symmetry exhibiting
 magnetic and luminescence bifunctional properties
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              558
_journal_paper_doi               10.1039/C4QI00242C
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C9 H24 Ho N3 O10 P3, Cl O4, 3(H2 O)'
_chemical_formula_sum            'C9 H32 Cl Ho N3 O17 P3'
_chemical_formula_weight         747.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-26 deposited with the CCDC.
2015-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                88.2040(10)
_cell_angle_beta                 76.2920(10)
_cell_angle_gamma                75.8130(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1535(8)
_cell_length_b                   9.2424(8)
_cell_length_c                   15.2450(13)
_cell_measurement_reflns_used    5554
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.458
_cell_measurement_theta_min      2.362
_cell_volume                     1214.29(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8250
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         1.375
_exptl_absorpt_coefficient_mu    3.647
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0273P)²+1.6128P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5128
_reflns_number_total             5490
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4qi00242c2.cif
_cod_data_source_block           Ho1
_cod_database_code               4348426
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.20033(2) 0.21196(2) 0.49900(2) 0.01516(5) Uani 1 1 d . . . . .
P1 P 0.46428(9) 0.03587(9) 0.64397(5) 0.01876(15) Uani 1 1 d . . . . .
P2 P -0.04108(9) 0.00079(8) 0.63151(5) 0.01828(15) Uani 1 1 d . . . . .
P3 P 0.02961(9) 0.54451(8) 0.64162(5) 0.01911(15) Uani 1 1 d . . . . .
C1 C 0.1202(4) 0.0224(4) 0.8744(2) 0.0260(7) Uani 1 1 d . . . . .
H1A H 0.1971 -0.0517 0.8965 0.031 Uiso 1 1 calc R U . . .
H1B H 0.0734 0.1017 0.9200 0.031 Uiso 1 1 calc R U . . .
C2 C -0.0032(4) -0.0483(4) 0.8561(2) 0.0268(7) Uani 1 1 d . . . . .
H2A H 0.0451 -0.1374 0.8181 0.032 Uiso 1 1 calc R U . . .
H2B H -0.0632 -0.0764 0.9125 0.032 Uiso 1 1 calc R U . . .
C3 C -0.2186(4) 0.1740(4) 0.8713(2) 0.0298(7) Uani 1 1 d . . . . .
H3A H -0.1825 0.1859 0.9250 0.036 Uiso 1 1 calc R U . . .
H3B H -0.3153 0.1437 0.8899 0.036 Uiso 1 1 calc R U . . .
C4 C -0.2455(4) 0.3216(4) 0.8236(2) 0.0302(7) Uani 1 1 d . . . . .
H4A H -0.3138 0.3200 0.7839 0.036 Uiso 1 1 calc R U . . .
H4B H -0.2966 0.4018 0.8682 0.036 Uiso 1 1 calc R U . . .
C5 C 0.0210(4) 0.3523(4) 0.8252(2) 0.0247(6) Uani 1 1 d . . . . .
H5A H -0.0202 0.3216 0.8856 0.030 Uiso 1 1 calc R U . . .
H5B H 0.0304 0.4538 0.8303 0.030 Uiso 1 1 calc R U . . .
C6 C 0.1828(4) 0.2520(4) 0.7894(2) 0.0243(6) Uani 1 1 d . . . . .
H6A H 0.2226 0.2815 0.7285 0.029 Uiso 1 1 calc R U . . .
H6B H 0.2496 0.2711 0.8262 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3632(4) -0.0029(4) 0.7566(2) 0.0248(6) Uani 1 1 d . . . . .
H7A H 0.3652 -0.1083 0.7588 0.030 Uiso 1 1 calc R U . . .
H7B H 0.4198 0.0169 0.7993 0.030 Uiso 1 1 calc R U . . .
C8 C -0.1655(4) -0.0009(4) 0.7434(2) 0.0254(7) Uani 1 1 d . . . . .
H8A H -0.2691 0.0587 0.7444 0.030 Uiso 1 1 calc R U . . .
H8B H -0.1721 -0.1023 0.7580 0.030 Uiso 1 1 calc R U . . .
C9 C -0.1354(4) 0.4968(4) 0.7208(2) 0.0272(7) Uani 1 1 d . . . . .
H9A H -0.1820 0.5772 0.7657 0.033 Uiso 1 1 calc R U . . .
H9B H -0.2125 0.4907 0.6880 0.033 Uiso 1 1 calc R U . . .
N1 N 0.1970(3) 0.0852(3) 0.78690(17) 0.0211(5) Uani 1 1 d . . . . .
H1C H 0.1477 0.0685 0.7446 0.025 Uiso 1 1 d R U . . .
N2 N -0.1039(3) 0.0597(3) 0.81122(18) 0.0232(5) Uani 1 1 d . . . . .
N3 N -0.0958(3) 0.3527(3) 0.76873(18) 0.0220(5) Uani 1 1 d . . . . .
H3C H -0.0516 0.2783 0.7261 0.026 Uiso 1 1 d R U . . .
O1 O 0.3480(3) 0.0850(3) 0.58829(16) 0.0274(5) Uani 1 1 d . . . . .
O2 O 0.5875(3) -0.1033(3) 0.61392(15) 0.0249(5) Uani 1 1 d . . . . .
O3 O 0.5307(3) 0.1698(3) 0.66404(16) 0.0293(5) Uani 1 1 d . . . . .
H3D H 0.5665 0.2057 0.6163 0.044 Uiso 1 1 calc R U . . .
O4 O 0.0001(3) 0.1516(2) 0.61988(14) 0.0209(4) Uani 1 1 d . . . . .
O5 O 0.1140(3) -0.1168(3) 0.63375(16) 0.0268(5) Uani 1 1 d . . . . .
H5C H 0.0942 -0.1933 0.6567 0.040 Uiso 1 1 calc R U . . .
O6 O -0.1238(3) -0.0355(2) 0.56464(15) 0.0235(5) Uani 1 1 d . . . . .
O7 O 0.1380(3) 0.3980(2) 0.60422(15) 0.0226(4) Uani 1 1 d . . . . .
O8 O -0.0445(3) 0.6411(3) 0.57474(16) 0.0291(5) Uani 1 1 d . . . . .
O9 O 0.1043(3) 0.6316(2) 0.69443(16) 0.0265(5) Uani 1 1 d . . . . .
Cl1 Cl 0.68101(16) 0.72410(16) 0.98186(9) 0.0623(3) Uani 1 1 d . . . . .
O10 O 0.636(3) 0.841(3) 1.044(2) 0.115(10) Uani 0.43(4) 1 d . . P A 1
O11 O 0.830(3) 0.631(4) 0.9959(18) 0.178(15) Uani 0.43(4) 1 d . . P A 1
O12 O 0.685(5) 0.758(3) 0.8897(14) 0.153(13) Uani 0.43(4) 1 d . . P A 1
O13 O 0.588(4) 0.627(4) 0.997(2) 0.141(11) Uani 0.43(4) 1 d . . P A 1
O10' O 0.667(3) 0.859(2) 1.0210(18) 0.115(7) Uani 0.57(4) 1 d . . P A 2
O11' O 0.835(2) 0.653(2) 0.955(2) 0.153(11) Uani 0.57(4) 1 d . . P A 2
O12' O 0.631(5) 0.758(4) 0.9086(18) 0.206(14) Uani 0.57(4) 1 d . . P A 2
O13' O 0.584(2) 0.650(2) 1.040(2) 0.128(9) Uani 0.57(4) 1 d . . P A 2
O1W O 0.3676(3) 0.3859(3) 0.44694(19) 0.0394(6) Uani 1 1 d . . . . .
H1WA H 0.3367 0.4706 0.4753 0.059 Uiso 1 1 d R U . . .
H1WB H 0.4227 0.3921 0.3935 0.059 Uiso 1 1 d R U . . .
O2W O 0.5844(4) 0.4119(5) 0.2929(3) 0.0819(13) Uani 1 1 d . . . . .
H2WA H 0.6633 0.4333 0.3052 0.123 Uiso 1 1 d R U . . .
H2WB H 0.6050 0.3815 0.2376 0.123 Uiso 1 1 d R U . . .
O3W O 0.6660(5) 0.2944(4) 0.5192(2) 0.0688(11) Uani 1 1 d . . . . .
H3WB H 0.7404 0.2297 0.4857 0.103 Uiso 1 1 d R U . . .
H3WA H 0.5957 0.3277 0.4904 0.103 Uiso 1 1 d R U . . .
O4W O 0.3394(9) 0.6644(6) 0.8966(4) 0.145(3) Uani 1 1 d . . . . .
H4WA H 0.4319 0.6744 0.8889 0.217 Uiso 1 1 d R U . . .
H4WB H 0.3394 0.5811 0.9225 0.217 Uiso 1 1 d R U . . .
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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O8 Ho1 O1 172.64(9) 2_566 .
O8 Ho1 O6 81.38(8) 2_566 2_556
O1 Ho1 O6 104.47(9) . 2_556
O8 Ho1 O7 88.02(8) 2_566 .
O1 Ho1 O7 84.66(8) . .
O6 Ho1 O7 147.53(8) 2_556 .
O8 Ho1 O2 103.37(9) 2_566 2_656
O1 Ho1 O2 82.63(8) . 2_656
O6 Ho1 O2 75.48(8) 2_556 2_656
O7 Ho1 O2 136.97(8) . 2_656
O8 Ho1 O4 97.14(9) 2_566 .
O1 Ho1 O4 80.14(8) . .
O6 Ho1 O4 76.56(7) 2_556 .
O7 Ho1 O4 74.43(7) . .
O2 Ho1 O4 142.11(8) 2_656 .
O8 Ho1 O1W 83.58(9) 2_566 .
O1 Ho1 O1W 94.83(9) . .
O6 Ho1 O1W 136.54(9) 2_556 .
O7 Ho1 O1W 71.59(8) . .
O2 Ho1 O1W 68.78(9) 2_656 .
O4 Ho1 O1W 145.97(8) . .
O2 P1 O1 117.28(14) . .
O2 P1 O3 112.87(13) . .
O1 P1 O3 110.63(14) . .
O2 P1 C7 104.59(14) . .
O1 P1 C7 108.44(14) . .
O3 P1 C7 101.53(15) . .
O6 P2 O4 115.00(13) . .
O6 P2 O5 114.54(13) . .
O4 P2 O5 105.76(13) . .
O6 P2 C8 107.67(14) . .
O4 P2 C8 108.28(14) . .
O5 P2 C8 105.01(15) . .
O7 P3 O8 115.58(13) . .
O7 P3 O9 111.78(13) . .
O8 P3 O9 111.62(13) . .
O7 P3 C9 105.80(14) . .
O8 P3 C9 103.36(15) . .
O9 P3 C9 107.88(15) . .
C2 C1 N1 108.8(3) . .
C2 C1 H1A 109.9 . .
N1 C1 H1A 109.9 . .
C2 C1 H1B 109.9 . .
N1 C1 H1B 109.9 . .
H1A C1 H1B 108.3 . .
N2 C2 C1 108.5(3) . .
N2 C2 H2A 110.0 . .
C1 C2 H2A 110.0 . .
N2 C2 H2B 110.0 . .
C1 C2 H2B 110.0 . .
H2A C2 H2B 108.4 . .
N2 C3 C4 110.1(3) . .
N2 C3 H3A 109.6 . .
C4 C3 H3A 109.6 . .
N2 C3 H3B 109.6 . .
C4 C3 H3B 109.6 . .
H3A C3 H3B 108.2 . .
N3 C4 C3 112.3(3) . .
N3 C4 H4A 109.1 . .
C3 C4 H4A 109.1 . .
N3 C4 H4B 109.1 . .
C3 C4 H4B 109.1 . .
H4A C4 H4B 107.9 . .
N3 C5 C6 115.8(3) . .
N3 C5 H5A 108.3 . .
C6 C5 H5A 108.3 . .
N3 C5 H5B 108.3 . .
C6 C5 H5B 108.3 . .
H5A C5 H5B 107.4 . .
N1 C6 C5 117.0(3) . .
N1 C6 H6A 108.0 . .
C5 C6 H6A 108.0 . .
N1 C6 H6B 108.0 . .
C5 C6 H6B 108.0 . .
H6A C6 H6B 107.3 . .
N1 C7 P1 115.4(2) . .
N1 C7 H7A 108.4 . .
P1 C7 H7A 108.4 . .
N1 C7 H7B 108.4 . .
P1 C7 H7B 108.4 . .
H7A C7 H7B 107.5 . .
N2 C8 P2 110.4(2) . .
N2 C8 H8A 109.6 . .
P2 C8 H8A 109.6 . .
N2 C8 H8B 109.6 . .
P2 C8 H8B 109.6 . .
H8A C8 H8B 108.1 . .
N3 C9 P3 114.8(2) . .
N3 C9 H9A 108.6 . .
P3 C9 H9A 108.6 . .
N3 C9 H9B 108.6 . .
P3 C9 H9B 108.6 . .
H9A C9 H9B 107.5 . .
C7 N1 C6 112.2(2) . .
C7 N1 C1 109.3(2) . .
C6 N1 C1 115.3(2) . .
C7 N1 H1C 106.7 . .
C6 N1 H1C 106.3 . .
C1 N1 H1C 106.5 . .
C2 N2 C3 114.4(3) . .
C2 N2 C8 116.5(3) . .
C3 N2 C8 113.8(3) . .
C9 N3 C4 108.2(2) . .
C9 N3 C5 112.9(2) . .
C4 N3 C5 112.8(3) . .
C9 N3 H3C 107.9 . .
C4 N3 H3C 107.7 . .
C5 N3 H3C 107.0 . .
P1 O1 Ho1 164.73(16) . .
P1 O2 Ho1 144.50(14) . 2_656
P1 O3 H3D 109.5 . .
P2 O4 Ho1 125.41(12) . .
P2 O5 H5C 109.5 . .
P2 O6 Ho1 147.24(14) . 2_556
P3 O7 Ho1 146.76(13) . .
P3 O8 Ho1 167.21(17) . 2_566
O12' Cl1 O10' 104.2(17) . .
O13 Cl1 O10 114.0(17) . .
O12' Cl1 O11' 106.7(17) . .
O10' Cl1 O11' 109.4(13) . .
O12' Cl1 O13' 110.0(16) . .
O10' Cl1 O13' 108.0(13) . .
O11' Cl1 O13' 117.6(12) . .
O13 Cl1 O12 101.4(19) . .
O10 Cl1 O12 118.3(18) . .
O13 Cl1 O11 103(2) . .
O10 Cl1 O11 106.0(14) . .
O12 Cl1 O11 113(2) . .
Ho1 O1W H1WA 114.5 . .
Ho1 O1W H1WB 127.7 . .
H1WA O1W H1WB 111.5 . .
H2WA O2W H2WB 110.8 . .
H3WB O3W H3WA 109.3 . .
H4WA O4W H4WB 105.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O8 2.204(2) 2_566
Ho1 O1 2.247(2) .
Ho1 O6 2.252(2) 2_556
Ho1 O7 2.261(2) .
Ho1 O2 2.305(2) 2_656
Ho1 O4 2.429(2) .
Ho1 O1W 2.472(2) .
P1 O2 1.489(2) .
P1 O1 1.492(2) .
P1 O3 1.574(2) .
P1 C7 1.817(3) .
P2 O6 1.495(2) .
P2 O4 1.526(2) .
P2 O5 1.569(2) .
P2 C8 1.815(3) .
P3 O7 1.505(2) .
P3 O8 1.507(2) .
P3 O9 1.528(2) .
P3 C9 1.833(3) .
C1 C2 1.517(5) .
C1 N1 1.522(4) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.456(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N2 1.456(4) .
C3 C4 1.520(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 N3 1.514(4) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N3 1.523(4) .
C5 C6 1.526(4) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 N1 1.515(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N1 1.508(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 N2 1.472(4) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 N3 1.506(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
N1 H1C 0.9059 .
N3 H3C 0.9090 .
O2 Ho1 2.305(2) 2_656
O3 H3D 0.8200 .
O5 H5C 0.8200 .
O6 Ho1 2.252(2) 2_556
O8 Ho1 2.204(2) 2_566
Cl1 O12' 1.31(2) .
Cl1 O13 1.36(3) .
Cl1 O10' 1.359(16) .
Cl1 O10 1.38(2) .
Cl1 O11' 1.371(18) .
Cl1 O13' 1.394(19) .
Cl1 O12 1.42(2) .
Cl1 O11 1.48(2) .
O1W H1WA 0.8570 .
O1W H1WB 0.8591 .
O2W H2WA 0.8556 .
O2W H2WB 0.8590 .
O3W H3WB 0.8586 .
O3W H3WA 0.8539 .
O4W H4WA 0.8550 .
O4W H4WB 0.8543 .
