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_4349911
_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, Cl O4'
_chemical_formula_sum            'C24 H22 Cl Dy N5 O10'
_chemical_formula_weight         738.41
_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     direct
_audit_creation_date             2018-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-05 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                62.152(14)
_cell_angle_beta                 71.245(12)
_cell_angle_gamma                81.049(11)
_cell_formula_units_Z            2
_cell_length_a                   11.0697(15)
_cell_length_b                   11.7807(16)
_cell_length_c                   12.2202(17)
_cell_measurement_reflns_used    2983
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7750
_cell_measurement_theta_min      4.2330
_cell_volume                     1334.2(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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   -109.00 -18.00   1.00   17.50    --  -39.24 -57.00 -60.00   91
  2  \w    -66.00  34.00   1.00   17.50    --  -39.24  57.00  90.00  100
  3  \w     47.00  74.00   1.00   17.50    --   39.24 -99.00 -90.00   27
  4  \w     70.00 126.00   1.00   17.50    --   39.24 178.00-150.00   56
  5  \w      3.00  46.00   1.00   17.50    --   39.24 -99.00 -90.00   43
  6  \w    -35.00  64.00   1.00   17.50    --   39.24 -37.00 150.00   99
  7  \w     37.00 126.00   1.00   50.00    --  108.77 -61.00 -60.00   89
  8  \w     29.00 109.00   1.00   50.00    --  108.77 -94.00 150.00   80
  9  \w    120.00 177.00   1.00   50.00    --  108.77  30.00  30.00   57
 10  \w     82.00 120.00   1.00   50.00    --  108.77-125.00   0.00   38
 11  \w     85.00 161.00   1.00   50.00    --  108.77  45.00   0.00   76
 12  \w     88.00 169.00   1.00   50.00    --  108.77  45.00 -90.00   81
 13  \w     36.00  63.00   1.00   50.00    --  108.77-125.00 120.00   27
 14  \w     85.00 121.00   1.00   50.00    --  108.77-125.00 120.00   36
 15  \w    122.00 147.00   1.00   50.00    --  108.77 103.00 166.00   25
 16  \w     77.00 134.00   1.00   50.00    --  108.77 -77.00-180.00   57
 17  \w     42.00  96.00   1.00   50.00    --  108.77 -45.00 150.00   54
 18  \w    100.00 170.00   1.00   50.00    --  108.77 125.00-150.00   70
 19  \w     79.00 176.00   1.00   50.00    --  108.77  77.00 -60.00   97
;
_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      0.0981320000
_diffrn_orient_matrix_UB_12      -0.0608055000
_diffrn_orient_matrix_UB_13      -0.0797968000
_diffrn_orient_matrix_UB_21      0.0711831000
_diffrn_orient_matrix_UB_22      0.1287115000
_diffrn_orient_matrix_UB_23      -0.0851550000
_diffrn_orient_matrix_UB_31      0.0830971000
_diffrn_orient_matrix_UB_32      -0.0401380000
_diffrn_orient_matrix_UB_33      0.0922271000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7893
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         4.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.492
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59608
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.004
_refine_diff_density_max         2.069
_refine_diff_density_min         -2.021
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.0082(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.1014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2851
_refine_ls_wR_factor_ref         0.3087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3861
_reflns_number_total             4734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00814k2.cif
_cod_data_source_block           20170714a
_cod_database_code               4349911
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 H10 O10 N10 Dy2 Cl2'
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.908
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O6-H6
 0.86 with sigma of 0.02
 Cl1-O7
 1.42 with sigma of 0.02
 Cl1-O8
 1.42 with sigma of 0.02
 Cl1-O9
 1.42 with sigma of 0.02
 Cl1-O10
 1.42 with sigma of 0.02
 O7-O8 \\sim O7-O9 \\sim O7-O10 \\sim O8-O9 \\sim O8-O10 \\sim O9-O10
 with sigma of 0.02
3. Rigid bond restraints
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 O6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C19(H19), C11(H11), C20(H20), C18(H18), C17(H17), C15(H15), C14(H14),
 C13(H13), C23(H23), C22(H22), C7(H7), C9(H9), C10(H10), C2(H2A), C3(H3),
 C4(H4), C5(H5)
5.c Fitted hexagon refined as free rotating group:
 N4(C18,C17,C16,C15,C14)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2017-07-14
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.680