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_4349910
_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         'C15 H22 Dy N3 O7, C H4 O, 2(Cl)'
_chemical_formula_sum            'C16 H26 Cl2 Dy N3 O8'
_chemical_formula_weight         621.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-25
_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                90
_cell_angle_beta                 94.758(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5612(3)
_cell_length_b                   15.4837(5)
_cell_length_c                   17.4652(6)
_cell_measurement_reflns_used    3976
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      27.5650
_cell_measurement_theta_min      4.1290
_cell_volume                     2307.19(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_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 0.994
_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     17.00  86.00   1.00    1.00    --   12.45  37.00-120.00   69
  2  \w     -4.00  22.00   1.00    1.00    --  -11.20 -99.00  30.00   26
  3  \w    -13.00  13.00   1.00    1.00    --   12.45 -99.00  60.00   26
  4  \w    -16.00  88.00   1.00    1.00    --   12.45  19.00-180.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0540284000
_diffrn_orient_matrix_UB_12      0.0051604000
_diffrn_orient_matrix_UB_13      -0.0283262000
_diffrn_orient_matrix_UB_21      0.0593630000
_diffrn_orient_matrix_UB_22      -0.0197407000
_diffrn_orient_matrix_UB_23      0.0248186000
_diffrn_orient_matrix_UB_31      -0.0218244000
_diffrn_orient_matrix_UB_32      -0.0410057000
_diffrn_orient_matrix_UB_33      -0.0155332000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12761
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.729
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4874
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3799
_reflns_number_total             4874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00814k2.cif
_cod_data_source_block           20161009a
_cod_original_cell_volume        2307.17(13)
_cod_database_code               4349910
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C1 H1 N1 O1 Dy1 Cl1'
_reflns_odcompleteness_completeness 99.71
_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, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 C14-H5
 1.898303 with sigma of 0.02
 C15-H7
 1.904916 with sigma of 0.02
 Dy1-H5
 2.856867 with sigma of 0.02
 Dy1-H7
 2.966144 with sigma of 0.02
3.a Rotating group:
 O6(H6A,H6B), O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C12(H12), C11(H11), C10(H10), C13(H13), C7(H7A), C5(H5A), C4(H4),
 C3(H3), C2(H2A)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
3.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_date_sample_data_collection 2016-10-09
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.856