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_7042949
_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
'0.5(C168 H72 Cd4 Na2 O48),5(C2H8N),4(C3H7NO),2(H2O)'
_chemical_formula_sum            'C106 H110 Cd2 N9 Na O38'
_chemical_formula_weight         2365.85
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 99.105(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.546(2)
_cell_length_b                   21.3217(10)
_cell_length_c                   35.974(2)
_cell_measurement_reflns_used    5020
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.2468
_cell_measurement_theta_min      3.2842
_cell_volume                     13288.7(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5058
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   -3.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7938 -125.0000  150.0000 97

  2 omega   11.00   93.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7938   57.0000  -30.0000 82

  3 omega -153.00  -98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000 -125.0000   60.0000 55

  4 omega   65.00  169.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       90.6218   30.0000  150.0000 104

  5 omega   60.00  158.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       90.6218   77.0000 -150.0000 98

  6 omega   20.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       90.6218  -30.0000  -30.0000 49

  7 omega   41.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       90.6218 -126.0000 -166.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20358
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        62.993
_diffrn_reflns_theta_max         62.993
_diffrn_reflns_theta_min         3.287
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.994
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3996
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         10562
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.1299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1627P)^2^+245.5013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3633
_refine_ls_wR_factor_ref         0.3795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8286
_reflns_number_total             10562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01242j2.cif
_cod_data_source_block           2
_cod_original_cell_volume        13288.6(19)
_cod_database_code               7042949
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C5 \\sim C11 \\sim C10 \\sim C12: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C23, C37, C36, O9, O10, C35, C38, C34, C39, C33, C40, C32, C27, C41, C31, C28,
  C26, C42, C29, C25, C2AA, C24, C22, O1AA, O0AA, O8, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C1, C2, O1, O2, C3, C21, C4, C20, C5, C19, C6, C18, C7, C10, C12, C17,
 C8, C13, C15, C9, C14, C16, O3, O4, O5, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17), C21(H21),
 C20(H20), C35(H35), C32(H32), C31(H31), C28(H28), C25(H25), C24(H24), C42(H42),
  C38(H38), C39(H39)
;
_shelx_res_checksum              11505
_shelx_fab_checksum              68379
_olex2_submission_special_instructions 'No special instructions were received'