Multifunctional chiral metal hydrogen-bonded organic frameworks constructed from lanthanide ions with a trigonal prismatic coordination environment.
Peng, Guo; Zhou, Guo-Xing; Dong, Xiang-Tao; Peng, Yong-Bo; Zhang, Rong-Yan; Ma, Ying-Zhao; Ren, Xiao-Ming; Dalton transactions (Cambridge, England : 2003) 54 (2024) 152–158; doi:10.1039/d4dt02131b

data_7717405
_publ_section_title
;
 Multifunctional chiral metal hydrogen-bonded organic frameworks
 constructed from lanthanide ions with a trigonal prismatic coordination
 environment.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              152
_journal_page_last               158
_journal_paper_doi               10.1039/d4dt02131b
_journal_volume                  54
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H33 Dy N3 O15 P3, 2(H2 O)'
_chemical_formula_sum            'C18 H37 Dy N3 O17 P3'
_chemical_formula_weight         822.91
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-23 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4345(3)
_cell_length_b                   12.4345(3)
_cell_length_c                   18.7179(11)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      33.12
_cell_measurement_theta_min      2.56
_cell_volume                     2894.1(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19262
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.724
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       plate
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.075(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0239P)^2^+0.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                4840
_reflns_number_total             4953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02131b2.cif
_cod_data_source_block           D-1
_cod_depositor_comments
'Adding full bibliography for 7717405--7717407.cif.'
_cod_database_code               7717405
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.925(11)
 0.075(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 H16C-H17B
 2.4 with sigma of 0.02
4.a Free rotating group:
 O16(H16C,H16D), O17(H17A,H17B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3A), C5(H5), C11(H11), C17(H17)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3B,H3C), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B)
4.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O13(H13)
;
_shelx_res_checksum              85510
_shelx_hkl_checksum              84136
_olex2_submission_special_instructions 'No special instructions were received'