Rational construction of a porous lanthanide coordination polymer featuring reversible guest-dependent magnetic relaxation behavior
Ma, Fang; Xiong, Jin; Meng, Yin-Shan; Yang, Jing; Sun, Hao-Ling; Gao, Song; Inorganic Chemistry Frontiers 5 (2018) 2875–; doi:10.1039/C8QI00814K

data_4349912
_publ_section_title
;
 Rational construction of a porous lanthanide coordination polymer
 featuring reversible guest-dependent magnetic relaxation behavior
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2875
_journal_paper_doi               10.1039/C8QI00814K
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C24 H22 Dy N5 O6, 3(C H4 O), Cl O4'
_chemical_formula_sum            'C27 H34 Cl Dy N5 O13'
_chemical_formula_weight         834.54
_chemical_name_systematic        dpbo
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                102.794(5)
_cell_angle_beta                 98.239(4)
_cell_angle_gamma                117.449(5)
_cell_formula_units_Z            2
_cell_length_a                   11.8598(6)
_cell_length_b                   12.0997(7)
_cell_length_c                   13.4297(7)
_cell_measurement_reflns_used    3312
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      26.2650
_cell_measurement_theta_min      3.6120
_cell_volume                     1599.30(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00 103.00   1.00    6.00    --   23.13  57.00 -30.00  107
  2  \w    100.00 126.00   1.00    6.00    --   23.13 178.00  90.00   26
  3  \w    -14.00 103.00   1.00    6.00    --   23.13  57.00  90.00  117
  4  \w    -20.00   6.00   1.00    6.00    --  -21.88 -99.00-150.00   26
  5  \w    -19.00 107.00   1.00    6.00    --   23.13  57.00-150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0310165000
_diffrn_orient_matrix_UB_12      0.0106723000
_diffrn_orient_matrix_UB_13      -0.0411286000
_diffrn_orient_matrix_UB_21      -0.0069470000
_diffrn_orient_matrix_UB_22      -0.0632857000
_diffrn_orient_matrix_UB_23      -0.0111196000
_diffrn_orient_matrix_UB_31      -0.0626798000
_diffrn_orient_matrix_UB_32      -0.0277208000
_diffrn_orient_matrix_UB_33      -0.0370757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.1134
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11065
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         3.244
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_preparation       'Solvent thermal method'
_exptl_crystal_recrystallization_method 'Solvent thermal method'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5531
_reflns_number_total             6717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00814k2.cif
_cod_data_source_block           20170503c
_cod_original_cell_volume        1599.30(17)
_cod_database_code               4349912
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 H7A-O7
 0.82 with sigma of 0.02
 H2-H7A
 2.5 with sigma of 0.1
 C24-H6
 1.91236 with sigma of 0.02
 Dy1-H6
 2.987004 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C14(H14), C18(H18), C15(H15), C13(H13), C23(H23), C7(H7), C12(H12),
 C17(H17), C22(H22), C2(H2A), C10(H10), C11(H11), C3(H3), C19(H19), C20(H20),
 C4(H4), C5(H5)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
4.c Idealised tetrahedral OH refined as rotating group:
 O8(H8), O9(H9)
;
_olex2_date_sample_data_collection 2017-05-03
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.794