Lanthanide complexes based on the linear bifunctional ligand: Synthesis, structure regulation and magnetic properties
Lan, Hai-Ming; Yang, Ru-Xia; Yang, Li-Zhen; Zhu, Peng-Yin; Wang, Lu-Lu; Yu, Yu-Ming; Wang, Duo-Zhi; Inorganica Chimica Acta 508 (2020) 119593–; doi:10.1016/j.ica.2020.119593

data_1564573
_publ_section_title
;
 Lanthanide complexes based on the linear bifunctional ligand: Synthesis,
 structure regulation and magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119593
_journal_paper_doi               10.1016/j.ica.2020.119593
_journal_volume                  508
_journal_year                    2020
_chemical_formula_moiety         'C34 H29 N9 O10 Pr, 4(H2 O), N O3'
_chemical_formula_sum            'C34 H37 N10 O17 Pr'
_chemical_formula_weight         998.64
_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
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 101.471(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0211(9)
_cell_length_b                   11.9141(6)
_cell_length_c                   20.3289(9)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.442
_cell_measurement_theta_min      2.486
_cell_volume                     3802.8(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45156
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.146
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0818 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.3913.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.620
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7499
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0460P)^2^+8.0630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5896
_reflns_number_total             7499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            5.cif
_cod_data_source_block           222
_cod_database_code               1564573
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1_$1-H8B_$2
 2.2 with sigma of 0.02
 N8_$4-N4_$3
 3.2 with sigma of 0.02
 N8_$5-N4_$6
 3.2 with sigma of 0.02
 N4_$6-N8_$5
 3.2 with sigma of 0.02
 N8-N4_$7
 3.2 with sigma of 0.02
3.a Free rotating group:
 O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B), O11(H11A,H11B)
3.b Rotating group:
 O10(H10A,H10B), O8(H8A,H8B), O9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N1(H1), C17(H17), C24(H24), C34(H34), C11(H11), C14(H14), C7(H7),
 C31(H31), C33(H33), C15(H15), C20(H20), C13(H13), C21(H21), C16(H16), C10(H10),
  C30(H30), C28(H28), C27(H27), C32(H32), C3(H3), C4(H4)
;
_shelx_res_checksum              37341
_shelx_hkl_checksum              73462
_olex2_submission_special_instructions 'No special instructions were received'