Structural diversity of four lanthanide metal‒organic frameworks based on 2,6-naphthalenedicarboxylate: synthesis, structures and photoluminescent properties
Chatenever, Ana R. K.; Ehlke, Beatriz; Le Maguerès, Pierre; Reinheimer, Eric W.; Song, Xueling; Fei, Honghan; Oliver, Scott R. J.; CrystEngComm 23 (2021) 1388–1397; doi:10.1039/D0CE01448F

data_7241989
_publ_section_title
;
 Structural diversity of four lanthanide metal--organic frameworks based
 on 2,6-naphthalenedicarboxylate: synthesis, structures and
 photoluminescent properties
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1388
_journal_page_last               1397
_journal_paper_doi               10.1039/D0CE01448F
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C21 H16 N Nd O7.5'
_chemical_formula_sum            'C21 H16 N Nd O7.5'
_chemical_formula_weight         546.59
_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             2017-11-23
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.03.02 svn.r3394 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.907(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4204(5)
_cell_length_b                   21.5953(7)
_cell_length_c                   16.3081(6)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2240
_cell_measurement_theta_min      3.6280
_cell_volume                     4263.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -30.00   6.00   0.50   65.80    --   -3.94 -37.00 -30.00   72
  2  \w    -23.00  31.00   0.50   65.80    --    2.69 -99.00 -30.00  108
  3  \w    -14.00  24.00   0.50   65.80    --   -3.94 -99.00  30.00   76
  4  \w    -18.00  14.00   0.50   65.80    --   -3.94 -99.00  90.00   64
  5  \w    -10.00  56.00   0.50   65.80    --   -3.94  37.00-180.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0390498000
_diffrn_orient_matrix_UB_12      -0.0233173000
_diffrn_orient_matrix_UB_13      -0.0165951000
_diffrn_orient_matrix_UB_21      0.0429744000
_diffrn_orient_matrix_UB_22      -0.0187126000
_diffrn_orient_matrix_UB_23      -0.0088030000
_diffrn_orient_matrix_UB_31      0.0078153000
_diffrn_orient_matrix_UB_32      -0.0136632000
_diffrn_orient_matrix_UB_33      0.0404427000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4360
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33b (Rigaku Oxford Diffraction, 2017)
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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4360
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0360P)^2^+15.6013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3954
_reflns_number_total             4360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01448f2.cif
_cod_data_source_block           ucsc_3
_cod_depositor_comments
'Adding full bibliography for 7241989--7241992.cif.'
_cod_original_formula_sum        'C21 H16 N Nd O7.50'
_cod_database_code               7241989
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C21 H16 N Nd O7.5'
_diffrn_oxdiff_ac3_digest_frames
;
01ab2f8ef0af72a7dc7008153afe7eb18400452a25c
;
_diffrn_oxdiff_ac3_digest_hkl
;
01f349a3c689c5660206b53f7d83f14f6b5f58
;
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19A-C21A \\sim C21A-C20A
 with sigma of 0.001
 C19B-C20B \\sim C20B-C21B
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 C19A, N1A, C21A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21B, C19B, N1B, C20B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C19B(0.7) H19B(0.7) N1B(0.7) C20B(0.7) H20A(0.7) H20B(0.7)
 H20C(0.7) C20A(0.3) H20D(0.3) H20E(0.3) H20F(0.3) C21B(0.7) H21A(0.7)
 H21B(0.7) H21C(0.7) N1A(0.3) C19A(0.3) H19A(0.3) C21A(0.3) H21D(0.3) H21E(0.3)
 H21F(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C12(H12), C6(H6), C15(H15), C3(H3), C16(H16), C9(H9), C5(H5),
 C10(H10), C19B(H19B), C19A(H19A)
5.b Idealised Me refined as rotating group:
 C20B(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C21B(H21A,H21B,H21C), C21A(H21D,
 H21E,H21F)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.871
_oxdiff_exptl_absorpt_empirical_full_min 0.635