Two lanthanide metal‒organic frameworks constructed from tris(4-carboxyphenyl)phosphane oxide with gas adsorption and magnetic properties
Hu, Tuoping; Zhao, Qiannan; Huo, Liangqin; Gao, Lingling; Zhang, Jie; Wang, Xiaoqing; Fan, Liming; CrystEngComm 20 (2018) 4291–; doi:10.1039/C8CE00661J

data_7230977
_publ_section_title
;
 Two lanthanide metal--organic frameworks constructed from
 tris(4-carboxyphenyl)phosphane oxide with gas adsorption and magnetic
 properties
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              4291
_journal_paper_doi               10.1039/C8CE00661J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C42 H28 Dy2 O16 P2'
_chemical_formula_sum            'C42 H28 Dy2 O16 P2'
_chemical_formula_weight         1175.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-02
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-03 deposited with the CCDC.
2018-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                72.521(2)
_cell_angle_beta                 88.719(2)
_cell_angle_gamma                87.591(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4402(6)
_cell_length_b                   14.6618(8)
_cell_length_c                   23.0870(13)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.533
_cell_measurement_theta_min      3.293
_cell_volume                     3367.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60430
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.293
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1107 before and 0.0785 after correction. The Ratio of minimum to maximum transmission is 0.6078. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.411
_exptl_crystal_size_min          0.362
_platon_squeeze_details
;
TITL p         P -1         R = 0.08
CELL   10.4402   14.6618   23.0870     72.52     88.72     87.59
SPGR P-1
C101 0.397 1.000 0.249 !       5.91 eA-3
Q102 0.960 0.171 0.272 !       4.50 eA-3
Q103 1.008 0.796 0.219 !       4.03 eA-3
Q104 0.024 0.909 0.233 !       3.82 eA-3
Q105 0.098 0.844 0.226 !       3.79 eA-3
Q106 0.612 0.908 0.320 !       3.60 eA-3
Q107 0.062 0.218 0.288 !       3.36 eA-3
Q108 0.055 0.128 0.256 !       3.12 eA-3
C109 0.607 0.045 0.170 !       2.99 eA-3
Q110 0.876 0.157 0.276 !       2.49 eA-3
Q111 0.925 0.844 0.227 !       2.03 eA-3
C112 0.615 0.886 0.382 !       1.96 eA-3
C113 0.668 0.049 0.143 !       1.95 eA-3
Q114 0.835 0.845 0.219 !       1.89 eA-3
Q115 0.059 0.465 0.182 !       1.78 eA-3
C116 0.590 0.076 0.116 !       1.61 eA-3
Q117 1.012 0.437 0.320 !       1.60 eA-3
Q118 0.133 0.173 0.257 !       1.60 eA-3
Q119 0.193 0.219 0.271 !       1.58 eA-3
C120 0.678 0.934 0.397 !       1.55 eA-3
Q121 1.013 0.733 0.211 !       1.54 eA-3
Q122 0.191 0.815 0.228 !       1.53 eA-3
C123 0.724 0.236 0.141 !       1.52 eA-3
Q124 0.143 0.888 0.232 !       1.47 eA-3
Q125 0.915 0.768 0.236 !       1.46 eA-3
C126 0.594 0.950 0.405 !       1.40 eA-3
C127 0.379 0.577 0.318 !       1.34 eA-3
Q128 0.046 0.060 0.256 !       1.33 eA-3
C129 0.620 0.123 0.121 !       1.30 eA-3
Q130 0.230 0.528 0.328 !       1.30 eA-3
C131 0.735 0.125 0.085 !       1.28 eA-3
C132 0.683 0.093 0.165 !       1.27 eA-3
Q133 0.920 0.203 0.133 !       1.24 eA-3
C134 0.678 0.139 0.098 !       1.20 eA-3
C135 0.728 0.144 0.025 !       1.18 eA-3
Q136 0.056 0.591 0.193 !       1.17 eA-3
Q137 1.007 0.968 0.241 !       1.16 eA-3
C138 0.627 0.843 0.425 !       1.15 eA-3
Q139 0.837 0.188 0.377 !       1.15 eA-3
C140 0.786 0.217 0.122 !       1.15 eA-3
Q141 0.065 0.422 0.161 !       1.15 eA-3
C142 0.626 0.798 0.414 !       1.15 eA-3
C143 0.456 0.142 0.157 !       1.14 eA-3
C144 0.355 0.517 0.240 !       1.13 eA-3
C145 0.351 0.423 0.218 !       1.12 eA-3
C146 0.412 0.499 0.124 !       1.12 eA-3
C147 0.736 0.220 0.069 !       1.12 eA-3
C148 0.735 0.268 0.094 !       1.10 eA-3
C149 0.371 0.486 0.289 !       1.08 eA-3
Q150 0.933 0.809 0.125 !       1.08 eA-3
C151 0.366 0.469 0.061 !       1.08 eA-3
C152 0.746 0.206 0.032 !       1.07 eA-3
Q153 1.008 0.375 0.314 !       1.07 eA-3
Q154 0.097 0.342 0.110 !       1.07 eA-3
C155 0.382 0.485 0.211 !       1.06 eA-3
C156 0.601 0.906 0.420 !       1.06 eA-3
C157 0.795 0.310 0.048 !       1.06 eA-3
Q158 0.141 0.749 0.369 !       1.02 eA-3
C159 0.470 0.434 0.095 !       1.01 eA-3
C160 0.467 0.108 0.123 !       1.00 eA-3
C161 0.310 0.626 0.353 !       0.98 eA-3
C162 0.576 0.138 0.137 !       0.98 eA-3
Q163 0.813 0.826 0.132 !       0.98 eA-3
Q164 0.884 0.047 0.257 !       0.97 eA-3
Q165 0.970 0.939 0.204 !       0.95 eA-3
C166 0.413 0.609 0.349 !       0.95 eA-3
Q167 0.168 0.231 0.384 !       0.94 eA-3
Q168 0.879 0.813 0.126 !       0.94 eA-3
Q169 0.030 0.301 0.281 !       0.94 eA-3
C170 0.472 0.970 0.359 !       0.94 eA-3
Q171 0.706 0.155 0.178 !       0.94 eA-3
Q172 0.651 0.986 0.196 !       0.93 eA-3
Q173 0.789 0.204 0.377 !       0.93 eA-3
Q174 0.905 0.515 0.181 !       0.93 eA-3
C175 0.512 0.173 0.099 !       0.92 eA-3
Q176 0.706 0.453 0.087 !       0.92 eA-3
C177 0.693 0.999 0.404 !       0.91 eA-3
C178 0.351 0.560 0.258 !       0.91 eA-3
C179 0.372 0.533 0.383 !       0.91 eA-3
Q180 0.051 0.029 0.148 !       0.91 eA-3
C181 0.378 0.548 0.212 !       0.91 eA-3
C182 0.617 0.902 0.447 !       0.90 eA-3
C183 0.484 0.574 0.342 !       0.90 eA-3
C184 0.500 0.486 0.109 !       0.90 eA-3
C185 0.399 0.840 0.392 !       0.90 eA-3
Q186 0.856 0.500 0.312 !       0.90 eA-3
C187 0.708 0.080 0.077 !       0.90 eA-3
C188 0.504 0.125 0.048 !       0.90 eA-3
C189 0.052 0.501 0.501 !       0.89 eA-3
Q190 0.917 0.504 0.072 !       0.89 eA-3
C191 0.327 0.306 0.156 !       0.89 eA-3
Q192 0.981 0.283 0.384 !       0.89 eA-3
Q193 0.136 0.639 0.438 !       0.89 eA-3
C194 0.315 0.580 0.241 !       0.88 eA-3
C195 0.470 0.909 0.354 !       0.88 eA-3
C196 0.232 0.470 0.486 !       0.88 eA-3
Q197 0.079 0.875 0.305 !       0.88 eA-3
C198 0.493 1.004 0.235 !       0.87 eA-3
Q199 0.913 0.829 0.479 !       0.87 eA-3
;
_refine_diff_density_max         3.510
_refine_diff_density_min         -3.158
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         12745
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+31.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11607
_reflns_number_total             12745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00661j2.cif
_cod_data_source_block           p_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7230976--7230977.cif.'
_cod_database_code               7230977
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.396
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C23-C42 = C41-C26 = C25-C24
 1.45 with sigma of 0.02
 C23-C24 = C25-C26 = C41-C42
 1.45 with sigma of 0.02
 C27-C33 = C32-C30 = C29-C28
 1.45 with sigma of 0.02
 C27-C28 = C29-C30 = C32-C33
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C3, C4, C5, C6, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Dy1, Dy2, O1, O2, O3, O4, O3A, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O3(0.5) O3A(0.5)
6.a Riding coordinates:
 O10(H10A,H10B), O16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C29(H29),
  C32(H32), C33(H33), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C42(H42)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'