Structural cutting and recombining in a layered sodium dysprosium phosphonate: key roles of flexible pyrazinyl hydrazone molecular tools
Sun, Xiao; Chen, Peiqiong; Liu, Yanan; Liu, Hou-Ting; Tian, Haiquan; CrystEngComm  (2022) –; doi:10.1039/D2CE01161A

data_7245544
_publ_section_title
;
 Structural cutting and recombining in a layered sodium dysprosium
 phosphonate: key roles of flexible pyrazinyl hydrazone molecular tools
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01161A
_journal_year                    2022
_chemical_formula_moiety
'C138 H114 Dy8 N16 Na4 O49 P8, 1.5(C H4 O), 5.5(H2 O)'
_chemical_formula_sum            'C139.5 H131 Dy8 N16 Na4 O56 P8'
_chemical_formula_weight         4420.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.814(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.922(2)
_cell_length_b                   16.3477(6)
_cell_length_c                   34.0768(19)
_cell_measurement_reflns_used    29607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.020
_cell_measurement_theta_min      2.028
_cell_volume                     16778.6(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1171
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            133386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       block
_exptl_crystal_F_000             8552
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.738
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2016
_refine_ls_number_reflns         29591
_refine_ls_number_restraints     7764
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0957
_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^)+(0.1152P)^2^+364.0410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16927
_reflns_number_total             29591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01161a2.cif
_cod_data_source_block           2
_cod_original_cell_volume        16778.8(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7245544
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.687
_shelx_res_checksum              73154
_shelx_hkl_checksum              62086
_shelx_fab_checksum              90572