Synthesis, structure and slow magnetic relaxation of lanthanoid coordination polymers based on ethynyl-bridged picolinate ligands.
Jornet-Mollá, Verónica; Gómez-García, Carlos J; Dolz-Lozano, Miquel J; Giménez-Saiz, Carlos; Romero, Francisco M.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13143–13154; doi:10.1039/d5dt01330e

data_7719248
_publ_section_title
;
 Synthesis, structure and slow magnetic relaxation of lanthanoid
 coordination polymers based on ethynyl-bridged picolinate ligands.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13143
_journal_page_last               13154
_journal_paper_doi               10.1039/d5dt01330e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H18 Ho N2 O10, C2 H8 N'
_chemical_formula_sum            'C32 H26 Ho N3 O10'
_chemical_formula_weight         777.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-05-14 deposited with the CCDC.	2025-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.763(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9306(2)
_cell_length_b                   10.7799(2)
_cell_length_c                   24.3559(4)
_cell_measurement_reflns_used    12521
_cell_measurement_temperature    119.9(3)
_cell_measurement_theta_max      26.8440
_cell_measurement_theta_min      3.9030
_cell_volume                     3095.86(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  26.20   0.70   15.00    --  -17.61 -99.00  60.00   66
  2  \w    -20.00  26.20   0.70   15.00    --  -17.61 -99.00-180.00   66
  3  \w    -56.00  91.70   0.70   15.00    --   18.47   0.00   0.00  211
  4  \w    -52.00  41.10   0.70   15.00    --   18.47 -57.00 150.00  133
  5  \w     -5.00  88.10   0.70   15.00    --   18.47  57.00  60.00  133
  6  \w    -52.00  41.10   0.70   15.00    --   18.47 -57.00 -90.00  133
  7  \w    -20.00  26.20   0.70   15.00    --  -17.61 -99.00 120.00   66
  8  \w    -20.00  26.20   0.70   15.00    --  -17.61 -99.00 -90.00   66
  9  \w   -100.00 -34.90   0.70   15.00    --  -17.61 178.00 -30.00   93
 10  \w    -88.00   5.10   0.70   15.00    --  -17.61 -57.00 120.00  133
 11  \w    -62.00  19.20   0.70   15.00    --  -17.61  99.00 175.00  116
 12  \w    -52.00  41.10   0.70   15.00    --   18.47 -57.00 -30.00  133
 13  \w    -20.00  26.20   0.70   15.00    --  -17.61 -99.00-150.00   66
 14  \w    -20.00  62.60   0.70   15.00    --   18.47 -99.00  60.00  118
;
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0550947000
_diffrn_orient_matrix_UB_12      -0.0114558000
_diffrn_orient_matrix_UB_13      0.0146561000
_diffrn_orient_matrix_UB_21      0.0239463000
_diffrn_orient_matrix_UB_22      0.0181011000
_diffrn_orient_matrix_UB_23      -0.0237040000
_diffrn_orient_matrix_UB_31      0.0031441000
_diffrn_orient_matrix_UB_32      0.0622052000
_diffrn_orient_matrix_UB_33      0.0095779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.737
_diffrn_reflns_theta_min         3.385
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.619
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       spearhead
_exptl_crystal_F_000             1544
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    hetero
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0206P)^2^+2.7710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3118
_reflns_number_total             3413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01330e2.cif
_cod_data_source_block           picCOOHo-c5
_cod_depositor_comments
'Adding full bibliography for 7719245--7719249.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7719248
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.812
_shelx_res_checksum              13623
_shelx_hkl_checksum              48704