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_7241992
_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         '2(C66 H57 La3 N4 O23), C3 H7 N O'
_chemical_formula_sum            'C135 H121 La6 N9 O47'
_chemical_formula_weight         3454.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                70.927(5)
_cell_angle_beta                 74.630(5)
_cell_angle_gamma                75.542(5)
_cell_formula_units_Z            1
_cell_length_a                   13.2526(8)
_cell_length_b                   14.3785(8)
_cell_length_c                   19.9214(10)
_cell_measurement_reflns_used    9097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.2440
_cell_measurement_theta_min      3.7930
_cell_volume                     3403.5(4)
_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                 HyPix-6000HE
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -56.00  21.00   0.50    5.77    --  -48.41  37.00 -60.00  154
  2  \w    -55.00  22.00   0.50    5.77    --  -48.41  37.00-180.00  154
  3  \w    -57.00 -30.00   0.50   23.08    --  -84.25  57.00   0.00   54
  4  \w    -87.00 -41.00   0.50    5.77    --  -48.41 -19.00 -60.00   92
  5  \w    -92.00 -65.00   0.50   23.08    --  -84.25  19.00 -30.00   54
  6  \w   -119.00 -90.00   0.50    5.77    --  -48.41 -19.00 -60.00   58
  7  \w   -120.00 -42.00   0.50    5.77    --  -48.41 -19.00  30.00  156
  8  \w    -73.00 -47.00   0.50   23.08    --  -84.25  77.00  90.00   52
  9  \w    -92.00 -62.00   0.50   23.08    --  -84.25 125.00  90.00   60
 10  \w     20.00  56.00   0.50    5.77    --   48.41 -37.00 -90.00   72
 11  \w    101.00 175.00   0.50   23.08    --  105.75  19.00 -60.00  148
 12  \w    148.00 173.00   0.50   23.08    --  105.75  77.00  60.00   50
 13  \w    102.00 127.00   0.50   23.08    --  105.75  77.00  60.00   50
 14  \w     32.00 113.00   0.50   23.08    --  105.75 -19.00  60.00  162
 15  \w     43.00 111.00   0.50   23.08    --  105.75 -19.00 -60.00  136
 16  \w     73.00 100.00   0.50   23.08    --  105.75 -99.00-180.00   54
 17  \w     34.00 104.00   0.50   23.08    --  105.75 -77.00-150.00  140
 18  \w     39.00  95.00   0.50   23.08    --  105.75 -19.00-180.00  112
 19  \w     34.00 109.00   0.50   23.08    --  105.75 -99.00-150.00  150
 20  \w     34.00 118.00   0.50   23.08    --  105.75 -77.00 -30.00  168
 21  \w     36.00 108.00   0.50   23.08    --  105.75 -99.00  90.00  144
 22  \w     34.00 113.00   0.50   23.08    --  105.75 -77.00  90.00  158
 23  \w     34.00 109.00   0.50   23.08    --  105.75 -99.00 -30.00  150
 24  \w     34.00 153.00   0.50   23.08    --  105.75   0.00 -90.00  238
 25  \w    -89.00 -62.00   0.50    5.77    --  -48.41 125.00-180.00   54
 26  \w   -106.00 -72.00   0.50    5.77    --  -48.41-125.00-120.00   68
 27  \w   -118.00 -89.00   0.50    5.77    --  -48.41-125.00   0.00   58
 28  \w   -112.00 -70.00   0.50    5.77    --  -48.41-125.00  90.00   84
;
_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      0.0623744000
_diffrn_orient_matrix_UB_12      -0.0336124000
_diffrn_orient_matrix_UB_13      0.0615971000
_diffrn_orient_matrix_UB_21      0.0795433000
_diffrn_orient_matrix_UB_22      -0.0753992000
_diffrn_orient_matrix_UB_23      -0.0371164000
_diffrn_orient_matrix_UB_31      0.0692616000
_diffrn_orient_matrix_UB_32      0.0803882000
_diffrn_orient_matrix_UB_33      -0.0424692000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32919
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         5.675
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.980
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.627
_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    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         11945
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0458P)^2^+10.8910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9215
_reflns_number_total             11945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01448f2.cif
_cod_data_source_block           ucsc_4
_cod_depositor_comments
'Adding full bibliography for 7241989--7241992.cif.'
_cod_database_code               7241992
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C66.6 H55.4 La3 N4.2 O23.5'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 C46A-C47A \\sim C47A-C48A
 with sigma of 0.001
 C4-C5B \\sim C4-C5A
 with sigma of 0.001
 O11-C26A \\sim O11-C26B
 with sigma of 0.001
 N3A-C28A \\sim N3B-C28B \\sim N3A-C27A \\sim N3B-C27B
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C8B \\sim C8A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C6A \\sim C6B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C7A \\sim C7B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C49A \\sim C49B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C26A \\sim C26B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
N3B \\sim N3A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C28B \\sim C28A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C64A) = Uanis(C63A)
Uanis(C6B) = Uanis(C5A)
Uanis(C5A) = Uanis(C5B)
Uanis(C8B) = Uanis(C9B)
Uanis(C8A) = Uanis(C9A)
Uanis(C6A) = Uanis(C5A)
Uanis(C27A) = Uanis(C28B)
Uanis(C27A) = Uanis(C27B)
4. Rigid body (RIGU) restrains
 C61A, C62A, C63A, C64A, C65A, C66A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C63A, C64A, C65A, C66A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C9A, C8B, C6A, C5B, C7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O19A, C49A, O18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26B, N3B, C27B, C28B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 H17B, O17, H17A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C5B)=Sof(C9A)=Sof(C8B)=Sof(H8B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(H7B)=1-
 FVAR(1)
 Sof(C9B)=Sof(C8A)=Sof(H8A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C5A)=FVAR(1)
 Sof(N3B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(N3A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=FVAR(2)
 Fixed Sof: O18A(0.5) O19A(0.5) C49A(0.5) O17(0.5) H17A(0.5) H17B(0.5)
 O21B(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H48C(0.5) N4B(0.5) C65A(0.5) H65A(0.5)
 C46B(0.5) H46B(0.5) C47B(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48B(0.5)
 H48D(0.5) H48E(0.5) H48F(0.5) N4A(0.5) C46A(0.5) H46A(0.5) C47A(0.5) H47D(0.5)
 H47E(0.5) H47F(0.5) C61A(0.5) C63A(0.5) H63A(0.5) C62A(0.5) C64A(0.5)
 C66A(0.5) H66A(0.5) C62B(0.5) C65B(0.5) H65B(0.5) C61B(0.5) C66B(0.5)
 H66B(0.5) C64B(0.5) C63B(0.5) H63B(0.5) N5(0.5) O23(0.5) C67(0.5) H67(0.5)
 C68(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5)
 O21A(0.5) O20(0.5) H20A(0.5) H20B(0.5) O19B(0.5) C49B(0.5) O18B(0.5)
6.a Rotating group:
 O17(H17A,H17B), O20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C22(H22), C24(H24), C51(H51), C54(H54), C14(H14),
 C37(H37), C33(H33), C56(H56), C59(H59), C43(H43), C32(H32), C38(H38), C40(H40),
  C52(H52), C1(H1), C57(H57), C45(H45), C31(H31), C26B(H26B), C8B(H8B),
 C23(H23), C42(H42), C6B(H6B), C7B(H7B), C16(H16), C65A(H65A), C46B(H46B),
 C46A(H46A), C63A(H63A), C66A(H66A), C65B(H65B), C66B(H66B), C63B(H63B),
 C67(H67), C8A(H8A), C6A(H6A), C7A(H7A), C26A(H26A)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C27B(H27A,H27B,H27C), C48A(H48A,H48B,H48C),
 C28B(H28A,H28B,H28C), C18(H18A,H18B,H18C), C17(H17C,H17D,H17E), C47B(H47A,H47B,
 H47C), C48B(H48D,H48E,H48F), C47A(H47D,H47E,H47F), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F)
;
_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 2.737
_oxdiff_exptl_absorpt_empirical_full_min 0.551