Two bilayer metal−organic frameworks with rare trinuclear heterometal clusters and tunable photoluminescence
Gong, Yun-Nan; Wei, Xue-Wen; He, Lv-Heng; Wen, Ya-Qiong; Ren, Ya-Wen; Xie, Yong-Rong; Zhong, Di-Chang; Dalton Trans.  (2017) –; doi:10.1039/C7DT01242J

data_7042948
_publ_section_title
;
 Two bilayer metal&#x2212;organic frameworks with rare trinuclear
 heterometal clusters and tunable photoluminescence
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01242J
_journal_year                    2017
_chemical_formula_moiety         'C42 H18 Cl2 K O12 Pb2, 3(C2 H8 N)'
_chemical_formula_sum            'C48 H42 Cl2 K N3 O12 Pb2'
_chemical_formula_weight         1377.22
_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   geom
_audit_creation_date             2017-04-25
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.03.14 svn.r3397 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.383(2)
_cell_angle_beta                 108.957(2)
_cell_angle_gamma                91.213(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9175(5)
_cell_length_b                   10.0625(4)
_cell_length_c                   13.4072(7)
_cell_measurement_reflns_used    4414
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.85
_cell_volume                     1197.20(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10094
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         2.190
_exptl_absorpt_coefficient_mu    7.286
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1113 before and 0.0311 after correction. The Ratio of minimum to maximum transmission is 0.6207. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.170
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5386
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0311P)^2^+3.4908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4666
_reflns_number_total             5386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01242j2.cif
_cod_data_source_block           1
_cod_database_code               7042948
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N24-C3 \\sim N24-C1A
 with sigma of 0.0001
 C22-C23 \\sim C3-C1A
 with sigma of 0.001
3. Rigid body (RIGU) restrains
 N24, C3, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) N24(0.5) H24A(0.5) H24B(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N24(H24A,H24B), N2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C15(H15), C16(H16), C18(H18)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              74649
_olex2_submission_special_instructions 'No special instructions were received'