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_7715350
_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 ad
_chemical_formula_moiety
'C26 H25 Cl3 Dy2 N6 O8, Cl, 2(C H4 O), 3[CH3OH]'
_chemical_formula_sum            'C31 H45 Cl4 Dy2 N6 O13'
_chemical_formula_weight         1176.53
_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_creation_date             2024-01-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_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                   13.07500(10)
_cell_length_b                   17.6728(2)
_cell_length_c                   18.0533(2)
_cell_measurement_reflns_used    17826
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1930
_cell_measurement_theta_min      3.4780
_cell_volume                     4171.61(7)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -74.00  36.00   0.50    1.20    --  -39.95  75.00-179.00  220
  2  \w     63.00 119.00   0.50    1.20    --   39.95 178.00-150.00  112
  3  \w     89.00 176.00   0.50    7.50    --  110.12  75.00-179.00  174
  4  \w    117.00 155.00   0.50    7.50    --  110.12  77.00 -30.00   76
  5  \w    116.00 173.00   0.50    7.50    --  110.12  45.00   0.00  114
  6  \w     82.00 108.00   0.50    7.50    --  110.12  45.00   0.00   52
  7  \w     78.00 104.00   0.50    7.50    --  110.12  77.00 -30.00   52
  8  \w     84.00 177.00   0.50    7.50    --  110.12  45.00 120.00  186
  9  \w     72.00 115.00   0.50    1.20    --   39.95 178.00 150.00   86
 10  \w    -51.00 -15.00   0.50    7.50    --  -94.50  45.00 -30.00   72
 11  \w    -50.00 -19.00   0.50    7.50    --  -94.50  61.00 -90.00   62
 12  \w    -89.00 -19.00   0.50    7.50    --  -94.50  71.00 -57.00  140
 13  \w    -96.00 -19.00   0.50    7.50    --  -94.50  74.00  62.00  154
 14  \w    -50.00 -25.00   0.50    7.50    --  -94.50  45.00 120.00   50
 15  \w   -113.00 -16.00   0.50    1.20    --  -39.95 -74.00 -65.00  194
 16  \w     35.00  89.00   0.50    7.50    --  110.12 -71.00 172.00  108
 17  \w     43.00  71.00   0.50    7.50    --  110.12 -61.00  90.00   56
 18  \w     43.00  69.00   0.50    7.50    --  110.12 -61.00  60.00   52
 19  \w     35.00 112.00   0.50    7.50    --  110.12-125.00  30.00  154
 20  \w     45.00  71.00   0.50    7.50    --  110.12 -61.00 -30.00   52
 21  \w     35.00  96.00   0.50    7.50    --  110.12 -74.00 -65.00  122
 22  \w     36.00  62.00   0.50    7.50    --  110.12 -61.00 -60.00   52
 23  \w     36.00  71.00   0.50    7.50    --  110.12 -61.00-180.00   70
 24  \w     36.00  95.00   0.50    7.50    --  110.12 -77.00 150.00  118
;
_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      -0.0507434000
_diffrn_orient_matrix_UB_12      -0.0329955000
_diffrn_orient_matrix_UB_13      0.0699330000
_diffrn_orient_matrix_UB_21      -0.0796937000
_diffrn_orient_matrix_UB_22      0.0642198000
_diffrn_orient_matrix_UB_23      -0.0012689000
_diffrn_orient_matrix_UB_31      -0.0704517000
_diffrn_orient_matrix_UB_32      -0.0488746000
_diffrn_orient_matrix_UB_33      -0.0488209000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17095
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       block
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.593
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 2966 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7375
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0657P)^2^+7.5595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7103
_reflns_number_total             7375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04028c2.cif
_cod_data_source_block           lfp-lbf-120410_sq
_cod_database_code               7715350
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H52 Cl16 Dy8 N60 O28 '
_shelx_estimated_absorpt_t_max   0.150
_shelx_estimated_absorpt_t_min   0.103
_reflns_odcompleteness_completeness 100.00
_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
 O7-H7
 0.85 with sigma of 0.01
 H9A-H4
 2.15 with sigma of 0.01
 Dy2-H7
 2.872743 with sigma of 0.02
 C26-H7
 1.862333 with sigma of 0.02
3. Rigid bond restraints
 C26, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O6, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C26) = Uanis(C25)
Uanis(O8) = Uanis(O7)
Uanis(C25) = Uanis(C21)
Uanis(C17) = Uanis(C21) = Uanis(C19)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C13(H13)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3A), N4(H4A), C2(H2), C8(H8), C4(H4B), C10(H10), C24(H24), C17(H17),
 C3(H3B), C22(H22), C18(H18), C9(H9), C15(H15), C23(H23)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C25(H25A,H25B,
 H25C)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O9(H9A), O10(H10A)
;
_shelx_res_checksum              1949
_shelx_fab_checksum              54104
_platon_squeeze_special_details
;
A solvent mask was calculated and 230 electrons were 
found in a volume of 752\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[CH3OH] per Asymmetric Unit 
which account for 216 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 3.745
_oxdiff_exptl_absorpt_empirical_full_min 0.519