Structural diversity, gas sorption properties, luminescent sensing of three Cd(II) complexes based on 3, 5-Di(2′, 5-dicarboxylphenyl)pyridine
Zhao, Li; Zhang, Jie; Wang, Jiang; Niu, Xiao-Yan; Wang, Xiao-Qing; Fan, Li-Ming; Hu, Tuo-Ping; Journal of Solid State Chemistry 268 (2018) 1–8; doi:10.1016/j.jssc.2018.08.028

data_1560710
_publ_section_title
;
 Structural diversity, gas sorption properties, luminescent sensing of
 three Cd(II) complexes based on 3, 5-Di(2&#x2032;,
 5-dicarboxylphenyl)pyridine
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1
_journal_page_last               8
_journal_paper_doi               10.1016/j.jssc.2018.08.028
_journal_volume                  268
_journal_year                    2018
_chemical_formula_moiety         'C33 H19 Cd2 N3 O9'
_chemical_formula_sum            'C33 H19 Cd2 N3 O9'
_chemical_formula_weight         826.33
_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'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 124.9730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0616(8)
_cell_length_b                   28.9143(10)
_cell_length_c                   14.1125(5)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.049
_cell_measurement_theta_min      2.256
_cell_volume                     8045.4(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0929
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46969
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_min         2.255
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.7402
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0747 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.9010. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.429
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7390
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0487P)^2^+145.8413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5564
_reflns_number_total             7390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc5.cif
_cod_data_source_block           mo_0819_1_0m_sq
_cod_database_code               1560710
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C29A-C28A
 1.4 with sigma of 0.02
 C24A-C25A = C25A-C26A
 1.4 with sigma of 0.02
 C27A-C28A = C28A-C29A
 1.4 with sigma of 0.02
 C27A-C26A
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(N3A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C24A)
\\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(N2A)
\\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C33A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cd1, N2, N2A, N3, N3A, C22, C22A, C23, C23A, C24, C24A, C25, C25A, C26, C26A,
 C27, C27A, C28, C28A, C29, C29A, C30, C30A, C31, C31A, C32, C32A, C33, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N2A)=Sof(N3A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=1-FVAR(1)
 Sof(N2)=Sof(N3)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=FVAR(1)
6.a Riding coordinates:
 O9(H9A,H9B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C24(H24), C24A(H24A), C25(H25), C25A(H25A), C26(H26), C26A(H26A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C31(H31), C31A(H31A), C32(H32),
 C32A(H32A), C33(H33), C33A(H33A)
;
_shelx_res_checksum              48979
_shelx_hkl_checksum              87856
_shelx_fab_checksum              9518