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_1560709
_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
'C44 H29 Cd4 N2 O20.5, 0.5(C4 H9 N O), 1.5(H2 O)'
_chemical_formula_sum            'C46 H36.5 Cd4 N2.5 O22.5'
_chemical_formula_weight         1433.92
_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                 113.399(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.459(4)
_cell_length_b                   24.215(3)
_cell_length_c                   18.917(3)
_cell_measurement_reflns_used    5108
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.657
_cell_measurement_theta_min      2.305
_cell_volume                     11544(3)
_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)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.629
_diffrn_reflns_theta_min         2.051
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0627 before and 0.0533 after correction. The Ratio of minimum to maximum transmission is 0.9211. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         13355
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1491
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7895
_reflns_number_total             13355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           z_sq
_cod_original_formula_sum        'C46 H36.50 Cd4 N2.50 O22.50'
_cod_database_code               1560709
_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 O(H,H) groups
2. Restrained distances
 C50-C47 = C49-C48
 1.5 with sigma of 0.02
 C47-O11 = O11-C48
 1.4 with sigma of 0.02
 C50-O23 = O23-C49
 1.4 with sigma of 0.02
 C47-O23 = O23-C48
 2.4 with sigma of 0.02
 O24-O26_$1
 2.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cd3A) \\sim Ueq, Uanis(Cd3) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O11, C50, O23, C49, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, N3, C45, C46, C43, O21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cd3, Cd3A, O24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cd3A)=1-FVAR(1)
 Sof(Cd3)=FVAR(1)
 Fixed Sof: O11(0.5) O21(0.5) C43(0.5) N3(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 H44C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 H46C(0.5) O22(0.5) H22A(0.5) H22B(0.5) C50(0.5) H50A(0.5) H50B(0.5) O23(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5) H48A(0.5)
 H48B(0.5) O24(0.5) H24A(0.5) H24B(0.5) O25(0.5) H25A(0.5) H25B(0.5) O26(0.5)
 H26A(0.5) H26B(0.5)
6.a Riding coordinates:
 O20(H20A,H20B), O22(H22A,H22B), O24(H24A,H24B), O25(H25A,H25B), O26(H26A,H26B)
6.b Rotating group:
 O15(H15A,H15B)
6.c Secondary CH2 refined with riding coordinates:
 O4(H4A,H4B), C50(H50A,H50B), C49(H49A,H49B), C47(H47A,H47B), C48(H48A,H48B)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C8(H8), C15(H15), C16(H16), C20(H20), C21(H21),
 C23(H23), C26(H26), C27(H27), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38),
  C40(H40), C41(H41)
6.e Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              51492
_shelx_hkl_checksum              74712
_shelx_fab_checksum              75574