#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:17:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143498 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/52/7035253.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_7035253
loop_
_publ_author_name
'Bag, Partha Pratim'
'Wang, Xu-Sheng'
'Cao, Rong'
_publ_section_title
;
 Microwave-assisted large scale synthesis of lanthanide metal-organic
 frameworks (Ln-MOFs), having a preferred conformation and
 photoluminescence properties.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11954
_journal_page_last               11962
_journal_paper_doi               10.1039/c5dt01598g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C30 H27 Cl Ho N5 O14'
_chemical_formula_weight         881.95
_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
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                106.206(2)
_cell_angle_beta                 97.893(2)
_cell_angle_gamma                100.266(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4644(2)
_cell_length_b                   12.7206(3)
_cell_length_c                   18.5539(5)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5330
_cell_measurement_theta_min      4.8280
_cell_volume                     2068.88(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13861
_diffrn_reflns_theta_full        73.74
_diffrn_reflns_theta_max         73.74
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.029
_platon_squeeze_details
;
;
_refine_diff_density_max         3.520
_refine_diff_density_min         -2.596
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1578P)²+8.0145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                7675
_reflns_number_total             8012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01598g2.cif
_cod_data_source_block           ho_final
_cod_depositor_comments
'Adding full bibliography for 7035246--7035254.cif.'
_cod_database_code               7035253
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
Ho1 Ho 0.26384(3) 0.48509(3) 0.497279(17) 0.01622(18) Uani 1 1 d .
Cl1 Cl 0.0001(2) -0.3565(2) 0.17881(16) 0.0735(7) Uani 1 1 d .
O1 O 0.2840(4) 0.3333(3) 0.3943(2) 0.0253(8) Uani 1 1 d .
N1 N 0.4581(6) 0.1063(4) 0.1741(3) 0.0267(10) Uani 1 1 d .
C1 C 0.4017(6) -0.0831(4) 0.0740(3) 0.0245(11) Uani 1 1 d .
O2 O 0.5267(4) 0.3913(3) 0.4269(2) 0.0258(8) Uani 1 1 d .
N2 N 0.5041(5) -0.3506(4) 0.1808(3) 0.0234(9) Uani 1 1 d .
C2 C 0.4778(5) -0.1530(4) 0.1022(3) 0.0197(9) Uani 1 1 d .
O3 O 0.3645(4) -0.4380(3) 0.4077(2) 0.0260(8) Uani 1 1 d .
N3 N 0.0608(6) -0.3357(5) -0.1320(3) 0.0369(7) Uani 1 1 d .
C3 C 0.4186(6) -0.2694(4) 0.0781(3) 0.0211(10) Uani 1 1 d .
O4 O 0.6110(4) -0.3865(3) 0.4387(2) 0.0269(8) Uani 1 1 d .
N4 N -0.0741(6) 0.1265(5) 0.2787(3) 0.0369(7) Uani 1 1 d .
C4 C 0.2819(6) -0.3150(5) 0.0299(3) 0.0270(11) Uani 1 1 d .
O5 O 0.1796(4) -0.4762(4) -0.38683(19) 0.0287(9) Uani 1 1 d .
N5 N 0.4034(6) 0.3352(5) 0.0983(3) 0.0369(7) Uani 1 1 d .
C5 C 0.2059(6) -0.2435(5) 0.0038(3) 0.0287(12) Uani 1 1 d .
O6 O -0.0532(4) -0.4671(3) -0.41471(19) 0.0241(8) Uani 1 1 d .
C6 C 0.2660(7) -0.1279(5) 0.0235(3) 0.0311(13) Uani 1 1 d .
O11 O -0.0099(11) 0.0527(9) 0.2915(6) 0.101(3) Uani 1 1 d .
C7 C 0.4721(8) 0.0399(5) 0.0967(3) 0.0320(12) Uani 1 1 d .
H7A H 0.5774 0.0484 0.0948 0.038 Uiso 1 1 calc R
H7B H 0.4275 0.0718 0.0586 0.038 Uiso 1 1 calc R
O10 O -0.1082(10) 0.1901(8) 0.3325(6) 0.0963(13) Uani 1 1 d .
C8 C 0.5085(6) -0.3455(5) 0.1008(3) 0.0308(9) Uani 1 1 d .
H8A H 0.6115 -0.3188 0.0974 0.037 Uiso 1 1 calc R
H8B H 0.4721 -0.4222 0.0641 0.037 Uiso 1 1 calc R
O9 O -0.0930(10) 0.1302(8) 0.2128(6) 0.0963(13) Uani 1 1 d .
C9 C 0.0556(6) -0.2912(5) -0.0473(3) 0.0308(9) Uani 1 1 d .
H9A H -0.0008 -0.2318 -0.0400 0.037 Uiso 1 1 calc R
H9B H 0.0031 -0.3530 -0.0315 0.037 Uiso 1 1 calc R
O13 O 0.2871(9) 0.2384(8) 0.0684(5) 0.088(2) Uani 1 1 d .
C10 C 0.6207(7) -0.1037(5) 0.1578(3) 0.0318(12) Uani 1 1 d .
H10A H 0.6622 -0.1643 0.1685 0.048 Uiso 1 1 calc R
H10B H 0.6047 -0.0543 0.2055 0.048 Uiso 1 1 calc R
H10C H 0.6888 -0.0601 0.1357 0.048 Uiso 1 1 calc R
O14 O 0.3391(9) 0.3900(8) 0.0690(6) 0.0963(13) Uani 1 1 d .
C11 C 0.2168(9) -0.4393(6) 0.0045(4) 0.0486(18) Uani 1 1 d .
H11A H 0.2914 -0.4802 -0.0116 0.073 Uiso 1 1 calc R
H11B H 0.1342 -0.4583 -0.0385 0.073 Uiso 1 1 calc R
H11C H 0.1824 -0.4605 0.0470 0.073 Uiso 1 1 calc R
O12 O 0.4882(10) 0.3216(8) 0.1338(6) 0.0963(13) Uani 1 1 d .
C12 C 0.1821(9) -0.0546(7) -0.0085(4) 0.0480(18) Uani 1 1 d .
H12A H 0.1339 -0.0954 -0.0618 0.072 Uiso 1 1 calc R
H12B H 0.2500 0.0145 -0.0063 0.072 Uiso 1 1 calc R
H12C H 0.1080 -0.0356 0.0219 0.072 Uiso 1 1 calc R
C13 C 0.5776(7) 0.1669(5) 0.2274(4) 0.0313(12) Uani 1 1 d .
H13 H 0.6722 0.1625 0.2170 0.038 Uiso 1 1 calc R
C14 C 0.5641(6) 0.2354(5) 0.2972(4) 0.0306(12) Uani 1 1 d .
H14 H 0.6490 0.2760 0.3353 0.037 Uiso 1 1 calc R
C15 C 0.4274(6) 0.2446(4) 0.3114(3) 0.0256(11) Uani 1 1 d .
C16 C 0.3037(6) 0.1780(5) 0.2570(3) 0.0290(11) Uani 1 1 d .
H16 H 0.2083 0.1802 0.2671 0.035 Uiso 1 1 calc R
C17 C 0.3216(7) 0.1093(5) 0.1888(3) 0.0299(12) Uani 1 1 d .
H17 H 0.2380 0.0636 0.1516 0.036 Uiso 1 1 calc R
C18 C 0.4113(6) 0.3285(4) 0.3838(3) 0.0235(10) Uani 1 1 d .
C19 C 0.6258(6) -0.3601(5) 0.2226(4) 0.0309(12) Uani 1 1 d .
H19 H 0.7139 -0.3570 0.2033 0.037 Uiso 1 1 calc R
C20 C 0.6233(7) -0.3744(6) 0.2929(4) 0.0336(13) Uani 1 1 d .
H20 H 0.7101 -0.3795 0.3230 0.040 Uiso 1 1 calc R
C21 C 0.4940(6) -0.3812(4) 0.3202(3) 0.0231(10) Uani 1 1 d .
C22 C 0.3696(6) -0.3705(5) 0.2757(3) 0.0275(11) Uani 1 1 d .
H22 H 0.2799 -0.3741 0.2935 0.033 Uiso 1 1 calc R
C23 C 0.3773(6) -0.3547(5) 0.2068(3) 0.0273(11) Uani 1 1 d .
H23 H 0.2928 -0.3466 0.1766 0.033 Uiso 1 1 calc R
C24 C 0.4879(6) -0.4036(4) 0.3958(3) 0.0240(10) Uani 1 1 d .
C25 C 0.1846(5) -0.3565(5) -0.1546(3) 0.0260(11) Uani 1 1 d .
H25 H 0.2715 -0.3421 -0.1175 0.031 Uiso 1 1 calc R
C26 C 0.1859(6) -0.3983(5) -0.2310(3) 0.0232(10) Uani 1 1 d .
H26 H 0.2729 -0.4143 -0.2471 0.028 Uiso 1 1 calc R
C27 C 0.0590(5) -0.4172(4) -0.2847(3) 0.0188(9) Uani 1 1 d .
C28 C -0.0672(6) -0.3966(5) -0.2595(3) 0.0271(11) Uani 1 1 d .
H28 H -0.1560 -0.4117 -0.2954 0.032 Uiso 1 1 calc R
C29 C -0.0635(6) -0.3538(6) -0.1818(3) 0.0316(13) Uani 1 1 d .
H29 H -0.1491 -0.3375 -0.1641 0.038 Uiso 1 1 calc R
C30 C 0.0610(5) -0.4580(4) -0.3701(3) 0.0196(9) Uani 1 1 d .
O8 O 0.0910(5) 0.3143(4) 0.4931(3) 0.0373(10) Uani 1 1 d .
O7 O 0.2155(5) 0.6678(4) 0.5206(3) 0.0423(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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O6 Ho1 O2 144.72(15) 2 2_666
O6 Ho1 O4 142.45(15) 2 2_656
O2 Ho1 O4 72.74(14) 2_666 2_656
O6 Ho1 O5 99.76(13) 2 1_566
O2 Ho1 O5 82.55(14) 2_666 1_566
O4 Ho1 O5 78.56(14) 2_656 1_566
O6 Ho1 O1 80.56(13) 2 .
O2 Ho1 O1 119.08(13) 2_666 .
O4 Ho1 O1 78.64(14) 2_656 .
O5 Ho1 O1 141.50(15) 1_566 .
O6 Ho1 O3 80.78(13) 2 1_565
O2 Ho1 O3 78.44(14) 2_666 1_565
O4 Ho1 O3 121.31(13) 2_656 1_565
O5 Ho1 O3 145.86(16) 1_566 1_565
O1 Ho1 O3 72.56(14) . 1_565
O6 Ho1 O7 73.19(15) 2 .
O2 Ho1 O7 73.73(15) 2_666 .
O4 Ho1 O7 138.83(16) 2_656 .
O5 Ho1 O7 74.05(18) 1_566 .
O1 Ho1 O7 139.75(16) . .
O3 Ho1 O7 73.52(17) 1_565 .
O6 Ho1 O8 71.82(15) 2 .
O2 Ho1 O8 140.14(15) 2_666 .
O4 Ho1 O8 71.93(14) 2_656 .
O5 Ho1 O8 72.92(16) 1_566 .
O1 Ho1 O8 70.71(15) . .
O3 Ho1 O8 136.94(15) 1_565 .
O7 Ho1 O8 125.99(17) . .
C18 O1 Ho1 116.4(3) . .
C13 N1 C17 120.4(5) . .
C13 N1 C7 120.8(5) . .
C17 N1 C7 118.7(5) . .
C6 C1 C2 120.7(5) . .
C6 C1 C7 120.9(5) . .
C2 C1 C7 118.3(5) . .
C18 O2 Ho1 176.5(4) . 2_666
C19 N2 C23 121.2(5) . .
C19 N2 C8 118.2(5) . .
C23 N2 C8 120.4(5) . .
C1 C2 C3 119.5(5) . .
C1 C2 C10 120.2(5) . .
C3 C2 C10 120.4(5) . .
C24 O3 Ho1 137.9(3) . 1_545
C29 N3 C25 122.2(5) . .
C29 N3 C9 116.7(5) . .
C25 N3 C9 121.1(5) . .
C4 C3 C2 120.6(5) . .
C4 C3 C8 119.9(5) . .
C2 C3 C8 119.3(5) . .
C24 O4 Ho1 137.4(4) . 2_656
O10 N4 O9 125.3(8) . .
O10 N4 O11 118.1(8) . .
O9 N4 O11 116.6(8) . .
C3 C4 C5 119.0(5) . .
C3 C4 C11 121.1(6) . .
C5 C4 C11 120.0(6) . .
C30 O5 Ho1 132.7(3) . 1_544
O12 N5 O14 155.4(10) . .
O12 N5 O13 111.3(8) . .
O14 N5 O13 93.1(7) . .
C4 C5 C6 121.6(5) . .
C4 C5 C9 119.8(6) . .
C6 C5 C9 118.6(5) . .
C30 O6 Ho1 179.6(4) . 2
C1 C6 C5 118.4(5) . .
C1 C6 C12 121.9(6) . .
C5 C6 C12 119.7(6) . .
N1 C7 C1 114.5(5) . .
C3 C8 N2 113.2(4) . .
C5 C9 N3 113.2(5) . .
N1 C13 C14 120.7(5) . .
C15 C14 C13 119.6(5) . .
C14 C15 C16 119.3(5) . .
C14 C15 C18 120.2(5) . .
C16 C15 C18 120.4(5) . .
C17 C16 C15 119.2(5) . .
N1 C17 C16 120.6(5) . .
O2 C18 O1 125.2(5) . .
O2 C18 C15 116.9(5) . .
O1 C18 C15 117.8(5) . .
N2 C19 C20 120.1(5) . .
C19 C20 C21 119.8(5) . .
C20 C21 C22 118.8(5) . .
C20 C21 C24 120.2(5) . .
C22 C21 C24 121.0(5) . .
C23 C22 C21 119.6(5) . .
N2 C23 C22 120.5(5) . .
O3 C24 O4 128.0(5) . .
O3 C24 C21 117.0(5) . .
O4 C24 C21 115.0(5) . .
N3 C25 C26 120.0(5) . .
C25 C26 C27 119.5(5) . .
C28 C27 C26 119.0(4) . .
C28 C27 C30 121.0(4) . .
C26 C27 C30 120.0(4) . .
C27 C28 C29 119.6(5) . .
N3 C29 C28 119.6(5) . .
O6 C30 O5 127.3(4) . .
O6 C30 C27 116.7(4) . .
O5 C30 C27 115.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O6 2.275(3) 2
Ho1 O2 2.295(4) 2_666
Ho1 O4 2.316(4) 2_656
Ho1 O5 2.350(3) 1_566
Ho1 O1 2.364(4) .
Ho1 O3 2.374(4) 1_565
Ho1 O7 2.381(4) .
Ho1 O8 2.451(4) .
O1 C18 1.257(7) .
N1 C13 1.344(8) .
N1 C17 1.362(8) .
N1 C7 1.486(7) .
C1 C6 1.400(8) .
C1 C2 1.403(7) .
C1 C7 1.502(8) .
O2 C18 1.251(6) .
O2 Ho1 2.295(4) 2_666
N2 C19 1.341(7) .
N2 C23 1.351(7) .
N2 C8 1.510(7) .
C2 C3 1.404(7) .
C2 C10 1.496(7) .
O3 C24 1.244(7) .
O3 Ho1 2.374(4) 1_545
N3 C29 1.334(8) .
N3 C25 1.342(7) .
N3 C9 1.526(7) .
C3 C4 1.391(7) .
C3 C8 1.504(8) .
O4 C24 1.263(7) .
O4 Ho1 2.316(4) 2_656
N4 O10 1.218(11) .
N4 O9 1.227(11) .
N4 O11 1.263(10) .
C4 C5 1.401(8) .
C4 C11 1.502(8) .
O5 C30 1.248(6) .
O5 Ho1 2.350(3) 1_544
N5 O12 1.037(10) .
N5 O14 1.194(10) .
N5 O13 1.415(11) .
C5 C6 1.402(9) .
C5 C9 1.514(8) .
O6 C30 1.234(6) .
O6 Ho1 2.275(3) 2
C6 C12 1.515(8) .
C13 C14 1.381(8) .
C14 C15 1.374(8) .
C15 C16 1.397(8) .
C15 C18 1.510(7) .
C16 C17 1.374(8) .
C19 C20 1.370(8) .
C20 C21 1.385(8) .
C21 C22 1.392(7) .
C21 C24 1.514(7) .
C22 C23 1.359(8) .
C25 C26 1.372(7) .
C26 C27 1.388(7) .
C27 C28 1.382(7) .
C27 C30 1.528(6) .
C28 C29 1.385(7) .
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 -0.007 0.000 0.500 561.3 157.8
