Stereoisomeric coordination polymers based on facial and meridional six-coordinate dysprosium(III)
Lin, Wei-Quan; Wang, Dan-Ru; Long, Wei-Jian; Lin, Li-Shan; Tao, Ze-Xian; Liu, Jun-Liang; Liu, Zhao-Qing; Leng, Ji-Dong; Dalton Transactions  (2022) –; doi:10.1039/D2DT00334A

data_7709649
_publ_section_title
;
 Stereoisomeric coordination polymers based on facial and meridional
 six-coordinate dysprosium(III)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00334A
_journal_year                    2022
_chemical_formula_moiety         'C39 H36 Cl3 Dy O3 P3'
_chemical_formula_sum            'C39 H36 Cl3 Dy O3 P3'
_chemical_formula_weight         914.44
_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   geom
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-30 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                96.8320(10)
_cell_angle_beta                 98.5820(10)
_cell_angle_gamma                115.4380(10)
_cell_formula_units_Z            2
_cell_length_a                   11.92540(10)
_cell_length_b                   12.06370(10)
_cell_length_c                   15.12950(10)
_cell_measurement_reflns_used    34122
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0160
_cell_measurement_theta_min      3.0510
_cell_volume                     1902.29(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_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    -39.00  22.00   0.50    0.10    --  -47.45  56.00-105.00  122
  2  \w   -116.00 -90.00   0.50    0.10    --  -47.45 -56.00 111.00   52
  3  \w    -87.00 -33.00   0.50    0.10    --  -47.45 -56.00 111.00  108
  4  \w     34.00  71.00   0.50    0.10    --   47.45  56.00-105.00   74
  5  \w   -130.00 -87.00   0.50    0.25    -- -102.00 -56.00 111.00   86
  6  \w   -172.00-136.00   0.50    0.25    -- -102.00 -56.00 111.00   72
  7  \w    -82.00 -30.00   0.50    0.25    -- -102.00  56.00-105.00  104
  8  \w    126.00 166.00   0.50    0.25    --  104.75  56.00-105.00   80
  9  \w    -93.00 -35.00   0.50    0.10    --  -47.45 -37.00-120.00  116
 10  \w     25.00  62.00   0.50    0.10    --   47.45  77.00 150.00   74
 11  \w     36.00  81.00   0.50    0.10    --   47.45  19.00  60.00   90
 12  \w     25.00  51.00   0.50    0.10    --   47.45  77.00 -90.00   52
 13  \w     35.00 111.00   0.50    0.10    --   47.45  37.00 -90.00  152
 14  \w     40.00 103.00   0.50    0.10    --   47.45  37.00 120.00  126
 15  \w     16.00  95.00   0.50    0.10    --   47.45-125.00 120.00  158
 16  \w     25.00  65.00   0.50    0.10    --   47.45  77.00  30.00   80
 17  \w     35.00  95.00   0.50    0.10    --   47.45  37.00-150.00  120
 18  \w     36.00  61.00   0.50    0.10    --   47.45  37.00  60.00   50
 19  \w     26.00  82.00   0.50    0.10    --   47.45  77.00 -60.00  112
 20  \w     26.00  70.00   0.50    0.10    --   47.45  77.00-180.00   88
 21  \w     26.00  65.00   0.50    0.10    --   47.45  77.00 -30.00   78
 22  \w     26.00  72.00   0.50    0.10    --   47.45  77.00  90.00   92
 23  \w     34.00  75.00   0.50    0.10    --   47.45  57.00 -60.00   82
 24  \w     82.00 122.00   0.50    0.10    --   47.45  19.00  60.00   80
 25  \w     39.00  95.00   0.50    0.10    --   47.45-125.00 -90.00  112
 26  \w     25.00  71.00   0.50    0.10    --   47.45  77.00-150.00   92
 27  \w    -24.00  55.00   0.50    0.10    --   47.45 -56.00 111.00  158
 28  \w   -175.00-113.00   0.50    0.25    -- -102.00 -71.00 145.85  124
 29  \w   -104.00 -77.00   0.50    0.25    -- -102.00 -82.00  60.96   54
 30  \w   -117.00 -29.00   0.50    0.25    -- -102.00  61.00  90.00  176
 31  \w   -118.00 -83.00   0.50    0.25    -- -102.00 -67.00   0.32   70
 32  \w   -110.00 -85.00   0.50    0.25    -- -102.00 -62.00-173.49   50
 33  \w   -173.00 -85.00   0.50    0.25    -- -102.00 -61.00  77.71  176
 34  \w   -168.00-142.00   0.50    0.25    -- -102.00 -76.00 175.13   52
 35  \w   -138.00 -79.00   0.50    0.25    -- -102.00 -76.00 175.13  118
 36  \w   -108.00 -81.00   0.50    0.25    -- -102.00 -72.00 -53.55   54
 37  \w   -103.00 -77.00   0.50    0.25    -- -102.00 -81.00   5.42   52
 38  \w   -175.00-125.00   0.50    0.25    -- -102.00 -61.00-150.00  100
 39  \w   -174.00-147.00   0.50    0.25    -- -102.00 -62.00-173.49   54
 40  \w   -174.00 -80.00   0.50    0.25    -- -102.00 -74.00-103.45  188
 41  \w   -105.00 -79.00   0.50    0.25    -- -102.00 -76.00 -19.58   52
 42  \w   -104.00 -79.00   0.50    0.25    -- -102.00 -77.00  90.00   50
 43  \w   -165.00-138.00   0.50    0.25    -- -102.00 -76.00 -19.58   54
 44  \w   -104.00 -79.00   0.50    0.25    -- -102.00 -77.00 120.00   50
 45  \w   -106.00 -79.00   0.50    0.25    -- -102.00 -76.00 -63.43   54
 46  \w   -108.00 -79.00   0.50    0.25    -- -102.00 -77.00 -90.00   58
 47  \w   -171.00-131.00   0.50    0.25    -- -102.00 -77.00 120.00   80
 48  \w   -105.00 -77.00   0.50    0.25    -- -102.00 -81.00  47.04   56
 49  \w   -106.00 -81.00   0.50    0.25    -- -102.00 -73.00 101.49   50
 50  \w   -131.00 -79.00   0.50    0.25    -- -102.00 -77.00 164.04  104
 51  \w   -158.00-132.00   0.50    0.25    -- -102.00 -81.00  47.04   52
 52  \w   -172.00 -79.00   0.50    0.25    -- -102.00 -77.00  30.00  186
 53  \w   -110.00 -85.00   0.50    0.25    -- -102.00 -61.00 125.14   50
 54  \w   -104.00 -79.00   0.50    0.25    -- -102.00 -76.00-170.60   50
 55  \w   -105.00 -80.00   0.50    0.25    -- -102.00 -74.00 -82.49   50
 56  \w   -125.00 -80.00   0.50    0.25    -- -102.00 -74.00 -36.54   90
 57  \w   -106.00 -80.00   0.50    0.25    -- -102.00 -75.00-119.12   52
 58  \w   -170.00-144.00   0.50    0.25    -- -102.00 -74.00 -36.54   52
 59  \w   -121.00 -84.00   0.50    0.25    -- -102.00 -64.00  59.29   74
 60  \w   -110.00 -85.00   0.50    0.25    -- -102.00 -61.00-150.00   50
 61  \w   -170.00 -90.00   0.50    0.25    -- -102.00 -57.00 -87.93  160
 62  \w   -155.00-124.00   0.50    0.25    -- -102.00 -61.00 -30.00   62
 63  \w   -123.00 -86.00   0.50    0.25    -- -102.00 -61.00 -30.00   74
 64  \w   -110.00 -85.00   0.50    0.25    -- -102.00 -62.00   5.78   50
 65  \w   -170.00 -85.00   0.50    0.25    -- -102.00 -65.00 -55.42  170
 66  \w   -107.00 -82.00   0.50    0.25    -- -102.00 -71.00  72.61   50
 67  \w   -173.00 -81.00   0.50    0.25    -- -102.00 -72.00  57.32  184
 68  \w   -107.00 -82.00   0.50    0.25    -- -102.00 -71.00 145.85   50
 69  \w   -145.00 -90.00   0.50    0.25    -- -102.00 -45.00-180.00  110
 70  \w     45.00 107.00   0.50    0.25    --  104.75 -94.00 120.00  124
 71  \w     38.00 109.00   0.50    0.25    --  104.75 -94.00 -30.00  142
 72  \w     41.00 126.00   0.50    0.25    --  104.75 -77.00 120.00  170
 73  \w     79.00 104.00   0.50    0.25    --  104.75 -94.00-150.00   50
 74  \w     89.00 115.00   0.50    0.25    --  104.75-125.00  90.00   52
 75  \w     54.00  79.00   0.50    0.25    --  104.75-125.00  90.00   50
 76  \w     89.00 114.00   0.50    0.25    --  104.75  61.00-150.00   50
 77  \w     34.00 106.00   0.50    0.25    --  104.75 -94.00 -60.00  144
 78  \w     52.00  77.00   0.50    0.25    --  104.75 -56.00 111.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1269580000
_diffrn_orient_matrix_UB_12      0.0798478000
_diffrn_orient_matrix_UB_13      0.0702603000
_diffrn_orient_matrix_UB_21      -0.0265380000
_diffrn_orient_matrix_UB_22      0.1144897000
_diffrn_orient_matrix_UB_23      0.0037014000
_diffrn_orient_matrix_UB_31      -0.0686751000
_diffrn_orient_matrix_UB_32      -0.0372970000
_diffrn_orient_matrix_UB_33      0.0782267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46309
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.455
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.047
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+1.5449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7450
_reflns_number_total             7672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00334a2.cif
_cod_data_source_block           wdr139-s6
_cod_database_code               7709649
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H Dy P O Cl'
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.336
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C26(H26A,H26B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              96723
_shelx_hkl_checksum              66451
_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 2.723
_oxdiff_exptl_absorpt_empirical_full_min 0.555