Coordination recognition of differential template units of lanthanide chiral chain.
Qin, Wen-Wen; Long, Bing-Fan; Zhu, Zhong-Hong; Wang, Hai-Ling; Liang, Fu-Pei; Zou, Hua-Hong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3675–3684; doi:10.1039/d3dt04028c

data_7715348
_publ_section_title
;
 Coordination recognition of differential template units of lanthanide
 chiral chain.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3675
_journal_page_last               3684
_journal_paper_doi               10.1039/d3dt04028c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C27 H30 Cl3 Dy2 N6 O9, Cl, 4(C H4 O), 1[CH3CN], 2[H2O]'
_chemical_formula_sum            'C33 H53 Cl4 Dy2 N7 O15'
_chemical_formula_weight         1254.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_update_record
;
2024-01-23 deposited with the CCDC.	2024-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.47190(10)
_cell_length_b                   14.86600(10)
_cell_length_c                   24.0640(2)
_cell_measurement_reflns_used    20721
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.0270
_cell_measurement_theta_min      3.4740
_cell_volume                     4819.38(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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    -53.00  32.00   0.50    0.60    --  -43.18  47.00 -55.00  170
  2  \w    -49.00 -23.00   0.50    2.50    --  -90.25  45.00  30.00   52
  3  \w    -53.00 -15.00   0.50    2.50    --  -90.25  47.00 -55.00   76
  4  \w   -118.00 -20.00   0.50    0.60    --  -43.18 -47.00 155.00  196
  5  \w     38.00  89.00   0.50    0.60    --   43.18-125.00   0.00  102
  6  \w     35.00  96.00   0.50    2.50    --  109.26 -74.00 -31.00  122
  7  \w     78.00 104.00   0.50    2.50    --  109.26 -77.00-120.00   52
  8  \w     63.00 100.00   0.50    2.50    --  109.26-125.00 -60.00   74
  9  \w     38.00  66.00   0.50    2.50    --  109.26 -61.00-120.00   56
 10  \w     36.00  61.00   0.50    2.50    --  109.26 -61.00 -90.00   50
 11  \w     37.00  63.00   0.50    2.50    --  109.26 -61.00-150.00   52
 12  \w     37.00  73.00   0.50    2.50    --  109.26 -77.00-120.00   72
 13  \w     37.00  67.00   0.50    2.50    --  109.26 -61.00   0.00   60
 14  \w     39.00  64.00   0.50    2.50    --  109.26 -61.00  30.00   50
 15  \w     36.00  82.00   0.50    2.50    --  109.26 -94.00  90.00   92
 16  \w     73.00 100.00   0.50    2.50    --  109.26-117.00  84.00   54
 17  \w     45.00  89.00   0.50    2.50    --  109.26 -77.00 120.00   88
 18  \w     42.00  68.00   0.50    2.50    --  109.26-117.00  84.00   52
 19  \w     38.00  69.00   0.50    2.50    --  109.26 -61.00 120.00   62
 20  \w     93.00 177.00   0.50    2.50    --  109.26  30.00  30.00  168
 21  \w     82.00 178.00   0.50    2.50    --  109.26  74.00  96.00  192
 22  \w     72.00 158.00   0.50    2.50    --  109.26 160.00 -35.00  172
 23  \w   -141.00 -50.00   0.50    2.50    --  -90.25-160.00 -67.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0789319000
_diffrn_orient_matrix_UB_12      0.0641248000
_diffrn_orient_matrix_UB_13      -0.0240582000
_diffrn_orient_matrix_UB_21      0.0510072000
_diffrn_orient_matrix_UB_22      -0.0800823000
_diffrn_orient_matrix_UB_23      -0.0289209000
_diffrn_orient_matrix_UB_31      -0.0651563000
_diffrn_orient_matrix_UB_32      0.0147716000
_diffrn_orient_matrix_UB_33      -0.0517830000
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.853
_diffrn_reflns_theta_min         3.495
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.333
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Flack x determined using 3840 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9709
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0563P)^2^+33.7099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                9410
_reflns_number_total             9709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04028c2.cif
_cod_data_source_block           lfp-lyl-072302_sq
_cod_database_code               7715348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C54 H54 N54 O54 Cl54 Dy54 '
_shelx_estimated_absorpt_t_max   0.163
_shelx_estimated_absorpt_t_min   0.123
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 H10a-H8
 2.15 with sigma of 0.01
 H11-H12a
 2.15 with sigma of 0.01
 Dy2-H8
 2.89148 with sigma of 0.02
 C27-H8
 1.893763 with sigma of 0.02
 C25-H7
 1.89841 with sigma of 0.02
 Dy1-H7
 2.945987 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) = Uanis(N4)
Uanis(C3) = Uanis(C2)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3a), N4(H4a), C15(H15), C10(H10), C18(H18), C9(H9a), C8(H8a), C22(H22),
 C4(H4b), C17(H17), C23(H23), C24(H24), C2(H2), C3(H3b)
4.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c), C26(H26a,H26b,
 H26c), C27(H27a,H27b,H27c), C01K(H01a,H01b,H01c), C28(H28a,H28b,H28c)
4.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O9(H9), O13(H13a), O10(H10a), O11(H11), O12(H12a)
;
_shelx_res_checksum              8788
_shelx_fab_checksum              81659
_platon_squeeze_special_details
;
A solvent mask was calculated and 172 electrons were 
found in a volume of 744\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH3CN], 2[H2O] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 3.261
_oxdiff_exptl_absorpt_empirical_full_min 0.594