Photoluminescent lanthanide(iii) coordination polymers based on 2-{[(4-methylphenyl)amino]methylene}-5,5-dimethylcyclohexane-1,3-dione
Smirnova, Ksenia S.; Sanzhenakova, Elizaveta A.; Eltsov, Ilia V.; Pozdnyakov, Ivan P.; Russkikh, Alena A.; Dotsenko, Victor V.; Lider, Elizaveta V.; New Journal of Chemistry 48 (2024) 18536–18545; doi:10.1039/D4NJ03444A

data_7063502
_publ_section_title
;
 Photoluminescent lanthanide(iii) coordination polymers based on
 2-{[(4-methylphenyl)amino]methylene}-5,5-dimethylcyclohexane-1,3-dione
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18536
_journal_page_last               18545
_journal_paper_doi               10.1039/D4NJ03444A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C32 H38 Gd N5 O13'
_chemical_formula_sum            'C32 H38 Gd N5 O13'
_chemical_formula_weight         857.92
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-09-30 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.279(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5319(5)
_cell_length_b                   11.6177(5)
_cell_length_c                   20.4408(7)
_cell_measurement_reflns_used    4839
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      28.6490
_cell_measurement_theta_min      2.4730
_cell_volume                     3445.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.15
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.884
_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    -38.00  -5.00   0.25   80.00    --  -19.00 -77.00 150.00  132
  2  \w    -56.00  61.00   0.25   80.00    --  -19.00  57.00 120.00  468
  3  \w    -24.00  38.00   0.25   80.00    --  -19.00  77.00   0.00  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7383
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.848
_diffrn_reflns_theta_min         2.246
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0153P)^2^+10.3649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3804
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03444a2.cif
_cod_data_source_block           gd20ypp-13_auto
_cod_depositor_comments
'Adding full bibliography for 7063497--7063502.cif.'
_cod_database_code               7063502
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C15(H15), C11(H11), C12(H12), C16(H16), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              88778
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;