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_7245543
_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
'C128 H103 Dy6 N24 Na5 O37 P5, 2(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C130 H112 Dy6 N24 Na5 O39.5 P5'
_chemical_formula_weight         3814.14
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                85.737(3)
_cell_angle_beta                 78.930(3)
_cell_angle_gamma                83.347(3)
_cell_formula_units_Z            2
_cell_length_a                   15.4587(4)
_cell_length_b                   18.4285(6)
_cell_length_c                   26.0855(9)
_cell_measurement_reflns_used    10635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8740
_cell_measurement_theta_min      3.5900
_cell_volume                     7233.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.1180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59355
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.250
_diffrn_reflns_theta_max         67.250
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    17.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             3722
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.455
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1888
_refine_ls_number_reflns         25878
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+33.7580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15329
_reflns_number_total             25878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01161a2.cif
_cod_data_source_block           1
_cod_database_code               7245543
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.333
_shelx_estimated_absorpt_t_max   0.371
_shelx_res_checksum              94158
_shelx_hkl_checksum              69424