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_7709648
_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         'C156 H144 Cl12 Dy4 O12 P12'
_chemical_formula_sum            'C156 H144 Cl12 Dy4 O12 P12'
_chemical_formula_weight         3657.74
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   35.6799(2)
_cell_length_b                   35.6799(2)
_cell_length_c                   21.42150(10)
_cell_measurement_reflns_used    21587
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.6870
_cell_measurement_theta_min      2.4580
_cell_volume                     23617.2(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.944
_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    -48.00  20.00   0.50    0.80    --  -46.37  45.00  11.00  136
  2  \w    -72.00 -46.00   0.50    3.20    -- -102.00  45.00  11.00   52
  3  \w    -73.00 -42.00   0.50    3.20    -- -102.00  45.00  60.00   62
  4  \w   -112.00 -59.00   0.50    3.20    -- -102.00  61.00  30.00  106
  5  \w   -171.00-127.00   0.50    3.20    -- -102.00 -61.00-108.00   88
  6  \w   -118.00 -93.00   0.50    0.80    --  -46.37-125.00-180.00   50
  7  \w   -113.00 -83.00   0.50    0.80    --  -46.37-125.00  30.00   60
  8  \w   -116.00 -79.00   0.50    0.80    --  -46.37-125.00  90.00   74
  9  \w     33.00  65.00   0.50    3.20    --  107.00 -30.00 150.00   64
 10  \w     33.00  58.00   0.50    3.20    --  107.00 -30.00  90.00   50
 11  \w     37.00 100.00   0.50    3.20    --  107.00 -94.00 120.00  126
 12  \w     43.00  69.00   0.50    3.20    --  107.00 -30.00 -60.00   52
 13  \w     46.00  71.00   0.50    3.20    --  107.00 -30.00 -90.00   50
 14  \w     33.00  59.00   0.50    3.20    --  107.00 -30.00-150.00   52
 15  \w     34.00  71.00   0.50    3.20    --  107.00 -30.00-180.00   74
;
_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      -0.0353988000
_diffrn_orient_matrix_UB_12      -0.0479011000
_diffrn_orient_matrix_UB_13      0.0061632000
_diffrn_orient_matrix_UB_21      -0.0147672000
_diffrn_orient_matrix_UB_22      0.0102219000
_diffrn_orient_matrix_UB_23      0.0621611000
_diffrn_orient_matrix_UB_31      -0.0318509000
_diffrn_orient_matrix_UB_32      0.0094158000
_diffrn_orient_matrix_UB_33      -0.0356380000
_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  0.0211
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28652
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.900
_diffrn_reflns_theta_min         2.477
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44478
_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    1.543
_exptl_crystal_description       needle
_exptl_crystal_F_000             10944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.668
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         10478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+332.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10056
_reflns_number_total             10478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00334a2.cif
_cod_data_source_block           181214d3_dycl3_rf
_cod_original_cell_volume        23617.2(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7709648
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Dy P O C H Cl'
_shelx_estimated_absorpt_t_max   0.552
_shelx_estimated_absorpt_t_min   0.346
_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), C14(H14A,H14B), C39(H39A,H39B), C40(H40A,H40B)
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), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_shelx_res_checksum              57758
_shelx_hkl_checksum              64328
_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 2.071
_oxdiff_exptl_absorpt_empirical_full_min 0.679