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_7241990
_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         'C84 H64 Gd4 N4 O28'
_chemical_formula_sum            'C84 H64 Gd4 N4 O28'
_chemical_formula_weight         2206.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4366(9)
_cell_length_b                   8.7643(4)
_cell_length_c                   45.084(2)
_cell_measurement_reflns_used    5551
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.49
_cell_volume                     7680.0(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            69213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         1.807
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.500
_exptl_absorpt_correction_T_max  0.0479
_exptl_absorpt_correction_T_min  0.0215
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.4489.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.461(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         19055
_refine_ls_number_restraints     1119
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0306P)^2^+3.3319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                13636
_reflns_number_total             19055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01448f2.cif
_cod_data_source_block           gd_a
_cod_depositor_comments
'Adding full bibliography for 7241989--7241992.cif.'
_cod_original_cell_volume        7679.9(6)
_cod_database_code               7241990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.539(17)
 0.461(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O1_10-C1_10 = O1_10-C8
 1.23 with sigma of 0.001
 O1_10-C1_10 \\sim O1_10-C8
 with sigma of 0.001
 N1_10-C1_10 \\sim N37-C8
 with sigma of 0.001
 N1_10-C2_10 \\sim N1_10-C3_10 \\sim N37-C25 \\sim N37-C60
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C1_10 \\sim N1_10 \\sim C3_10 \\sim C2_10 \\sim C8 \\sim N37 \\sim C60: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C8(0.25) H8(0.25) C25(0.25) H25A(0.25) H25B(0.25) H25C(0.25)
 N37(0.25) C60(0.25) H60A(0.25) H60B(0.25) H60C(0.25) N1(0.75) C1(0.75)
 H1(0.75) C2(0.75) H2A(0.75) H2B(0.75) H2C(0.75) C3(0.75) H3A(0.75) H3B(0.75)
 H3C(0.75)
7.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C3(H3), C5(H5),
 C6(H6), C8(H8), C10(H10), C11(H11), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9),
 C11(H11), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C3(H3), C5(H5),
 C6(H6), C8(H8), C10(H10), C11(H11), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9),
 C11(H11), C1(H1), C1(H1), C1(H1), C1(H1)
7.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C60(H60A,H60B,H60C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C),
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2(H2A,H2B,
 H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              80646
_olex2_submission_special_instructions 'No special instructions were received'