Efficient X-ray scintillating lead(ii)-based MOFs derived from rigid luminescent naphthalene motifs.
Lu, Jian; Xin, Xue-Huan; Lin, Yang-Jie; Wang, Shuai-Hua; Xu, Jian-Gang; Zheng, Fa-Kun; Guo, Guo-Cong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1722–1731; doi:10.1039/c8dt04587a

data_7048616
_publ_section_title
;
 Efficient X-ray scintillating lead(ii)-based MOFs derived from rigid
 luminescent naphthalene motifs.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1722
_journal_page_last               1731
_journal_paper_doi               10.1039/c8dt04587a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C24 H14 O9 Pb2, C3 H7 N O'
_chemical_formula_sum            'C27 H21 N O10 Pb2'
_chemical_formula_weight         933.83
_chemical_name_common            '[Pb2(2,6-ndc)2H2O]n, nDMF'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-13 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                102.099(18)
_cell_angle_beta                 93.567(14)
_cell_angle_gamma                109.763(12)
_cell_formula_units_Z            2
_cell_length_a                   8.2143(7)
_cell_length_b                   11.8601(11)
_cell_length_c                   14.6928(18)
_cell_measurement_reflns_used    4489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1303.3(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19770
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         3.050
_exptl_absorpt_coefficient_mu    12.962
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5375
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4027
_reflns_number_total             5375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04587a2.cif
_cod_data_source_block           SMOF-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048615--7048618.cif.
;
_cod_database_code               7048616
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details   'Sphere (Rigaku CrystalClear)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H5-H27F_$1
 2.2 with sigma of 0.02
 O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 N1-C27A \\sim N1-C27B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C27B)
4. Others
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(H26A)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(H26)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=FVAR(1)
5.a Me refined with riding coordinates:
 C25(H25D,H25E,H25F)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16),
 C18(H18), C21(H21), C22(H22), C24(H24), C26(H26), C26(H26A)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F)
;
_shelx_res_checksum              2133
_olex2_submission_special_instructions 'No special instructions were received'