Quick and robust PDF data acquisition using a laboratory single-crystal X-ray diffractometer for study of polynuclear lanthanide complexes in solid form and in solution
Tsymbarenko, Dmitry; Grebenyuk, Dimitry; Burlakova, Maria; Zobel, Mirijam; Journal of Applied Crystallography 55 (2022) 890–900; doi:10.1107/S1600576722005878

data_2300692
_publ_section_title
;
 Quick and robust PDF data acquisition using a laboratory single-crystal
 X-ray diffractometer for study of polynuclear lanthanide complexes in
 solid form and in solution
;
_journal_coeditor_code           XX5001
_journal_issue                   4
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              890
_journal_page_last               900
_journal_paper_doi               10.1107/S1600576722005878
_journal_volume                  55
_journal_year                    2022
_chemical_formula_moiety
'C34 H80 F9 N18 O18 Pr4, 3(C2 F3 O2), C2 H F3 O2, 6(H2 O)'
_chemical_formula_sum            'C42 H93 F21 N18 O32 Pr4'
_chemical_formula_weight         2324.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 98.4791(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6254(9)
_cell_length_b                   12.7853(4)
_cell_length_c                   23.5496(8)
_cell_measurement_reflns_used    9066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.75
_cell_measurement_theta_min      2.55
_cell_volume                     8226.8(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.914
_diffrn_source                   'Micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.6742
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.139
_refine_diff_density_max         2.116
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0695P)^2^+112.3975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7970
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xx5001sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2300692.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2300692
_cod_database_fobs_code          2300692
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.601
_shelx_estimated_absorpt_t_max   0.726
_shelx_res_checksum              12569
_shelx_hkl_checksum              90686