Ring-forming transformation associated with hydrazone changes of hexadecanuclear dysprosium phosphonates.
Tian, Haiquan; Huang, Fu-Ping; Li, Yongfei; Chen, Peiqiong; Chai, Keyu; Lu, Jing; Liu, Hou-Ting; Zeng, Suyuan; Li, Dacheng; Dou, Jianmin; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1119–1125; doi:10.1039/d0dt03536j

data_7706031
_publ_section_title
;
 Ring-forming transformation associated with hydrazone changes of
 hexadecanuclear dysprosium phosphonates.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1119
_journal_page_last               1125
_journal_paper_doi               10.1039/d0dt03536j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C108 H91 Dy8 N17 O37 P5, 0.5(C H4 O), 4.5(H2 O)'
_chemical_formula_sum            'C108.5 H102 Dy8 N17 O42 P5'
_chemical_formula_weight         3770.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-11-27 deposited with the CCDC.	2020-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.1885(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   28.62469(19)
_cell_length_c                   27.8172(2)
_cell_measurement_reflns_used    38944
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0410
_cell_measurement_theta_min      2.5410
_cell_volume                     13835.0(2)
_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    '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      100.00(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            110052
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.249
_diffrn_reflns_theta_max         67.249
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    23.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       block
_exptl_crystal_F_000             7028
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1771
_refine_ls_number_reflns         24735
_refine_ls_number_restraints     1272
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1351P)^2^+19.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19450
_reflns_number_total             24735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03536j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7706031--7706032.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7706031
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.223
_shelx_estimated_absorpt_t_max   0.251
_shelx_res_checksum              80552
_shelx_fab_checksum              74709