The influence of coordination modes and active sites of a 5-(triazol-1-yl) nicotinic ligand on the assembly of diverse MOFs
Yan, Yang-Tian; Zhang, Si-Si; Yang, Guo-Ping; Zhang, Wen-Yan; Zhang, Fang; Cao, Feng; Yang, Rui-Feng; Wang, Yao-Yu; Dalton Trans.  (2017) –; doi:10.1039/C7DT01523B

data_7043551
_publ_section_title
;
 The influence of coordination modes and active sites of a
 5-(triazol-1-yl) nicotinic ligand on the assembly of diverse MOFs
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01523B
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H5 Cu N4 O2.5, C H4 O, 2.5(H2 O)'
_chemical_formula_sum            'C9 H14 Cu N4 O6'
_chemical_formula_weight         337.78
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-16 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.572(6)
_cell_length_b                   16.572(6)
_cell_length_c                   10.620(4)
_cell_measurement_reflns_used    996
_cell_measurement_temperature    298
_cell_measurement_theta_max      17.531
_cell_measurement_theta_min      2.386
_cell_volume                     2525.8(16)
_computing_cell_refinement       'SAINT V8.18C (Bruker, 2016)'
_computing_data_collection       'SAINT V8.18C (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.18C (Bruker, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1601
_diffrn_reflns_av_unetI/netI     0.1710
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15692
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_min         1.419
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1276 before and 0.0759 after correction. The Ratio of minimum to maximum transmission is 0.7638. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
The structure contained large void, and the solvent and 
the positive or negative ions located in the void couldn't 
be identified because it was highly disordered had so small 
residual peak. Therefore, SQUEEZE in PLATON program was 
performed to remove the highly disordered solvent and ions. 
The numbers of masked ions and solvent molecules were 
confirmed by TG analysis. After calculation, the ions and 
solvent molecules were added in the _chemical_formula_moiety,
 _chemical_formula_sum and other relative items. 

;
_refine_ls_abs_structure_Flack   0.25(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         4130
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2373
_reflns_number_total             4130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01523b2.cif
_cod_data_source_block           5
_cod_original_cell_volume        2526(2)
_cod_database_code               7043551
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.75(3)
 0.25(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N3A-N2 \\sim N2-N3
 with sigma of 0.02
 C8A-N4 \\sim N4-C8
 with sigma of 0.02
 C8-N3 \\sim C8A-N3A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N3A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N2, N4, C7, N3, C8, N3A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N3A)=Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(N3)=Sof(C8)=Sof(H8)=FVAR(1)
7.a Riding coordinates:
 C8(H8), C8A(H8A)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C3(H3), C7(H7)
;
_shelx_res_checksum              30034
_shelx_fab_checksum              98561
_olex2_submission_special_instructions 'No special instructions were received'