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_7709647
_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, 1.75(C H4 O)'
_chemical_formula_sum            'C40.75 H43 Cl3 Dy O4.75 P3'
_chemical_formula_weight         970.51
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-20
_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                105.698(3)
_cell_angle_beta                 97.442(3)
_cell_angle_gamma                115.579(4)
_cell_formula_units_Z            2
_cell_length_a                   12.7559(5)
_cell_length_b                   13.5242(6)
_cell_length_c                   14.6360(4)
_cell_measurement_reflns_used    11689
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.6720
_cell_measurement_theta_min      2.6800
_cell_volume                     2102.42(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_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  59.00   1.00    3.00    --  -11.59  57.00 120.00   98
  2  \w     36.00  66.00   1.00    3.00    --   11.74 178.00 -30.00   30
  3  \w    -56.00 -29.00   1.00    3.00    --   11.74 -37.00 -30.00   27
  4  \w    -18.00  17.00   1.00    3.00    --  -11.59 -99.00-120.00   35
  5  \w    -20.00  53.00   1.00    3.00    --   11.74 -99.00-120.00   73
  6  \w    -82.00  15.00   1.00    3.00    --  -11.59 -57.00 -30.00   97
  7  \w    -68.00 -23.00   1.00    3.00    --  -11.59 125.00 -26.43   45
  8  \w    -85.00  11.00   1.00    3.00    --  -11.59 -37.00  90.00   96
  9  \w     15.00  52.00   1.00    3.00    --  -11.59  37.00 -90.00   37
 10  \w    -92.00  -7.00   1.00    3.00    --  -11.59 -19.00-180.00   85
 11  \w     -3.00  53.00   1.00    3.00    --   11.74 -99.00   0.00   56
;
_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      -0.0583609000
_diffrn_orient_matrix_UB_12      -0.0327273000
_diffrn_orient_matrix_UB_13      0.0050630000
_diffrn_orient_matrix_UB_21      -0.0051294000
_diffrn_orient_matrix_UB_22      -0.0525627000
_diffrn_orient_matrix_UB_23      -0.0323042000
_diffrn_orient_matrix_UB_31      0.0264718000
_diffrn_orient_matrix_UB_32      -0.0081680000
_diffrn_orient_matrix_UB_33      0.0410698000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.589
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             975
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.834
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0499P)^2^+1.8852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8528
_reflns_number_total             10482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00334a2.cif
_cod_data_source_block           125-w7
_cod_original_cell_volume        2102.43(15)
_cod_database_code               7709647
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O5(0.5) H5A(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) O7(0.25)
 H7(0.25) C40(0.25) H40A(0.25) H40B(0.25) H40C(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C20(H20A,H20B), C39(H39A,H39B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), 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)
3.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O5(H5A), O7(H7)
;
_shelx_res_checksum              99198
_shelx_hkl_checksum              72399
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.728