Five new 3D transition MOFs based on 1-(3,5-dicarboxylatobenzyl)-3,5-pyrazole dicarboxylic acid displaying the unique luminescent sensing towards Fe3+ and magnetic properties
Tong, Wen Quan; Liu, WeiNi; Ma, Lu-Lu; Wang, Yao; Wang, Jiao-Min; Wang, Yao-Yu; Hou, Lei; Dalton Transactions  (2019) –; doi:10.1039/C9DT00933G

data_7049625
_publ_section_title
;
 Five new 3D transition MOFs based on
 1-(3,5-dicarboxylatobenzyl)-3,5-pyrazole dicarboxylic acid displaying the
 unique luminescent sensing towards Fe3+ and magnetic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00933G
_journal_year                    2019
_chemical_formula_moiety         'C14 H16 Ba2 N2 O13, 2(O)'
_chemical_formula_sum            'C14 H16 Ba2 N2 O15'
_chemical_formula_weight         726.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0625(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3811(8)
_cell_length_b                   18.3474(17)
_cell_length_c                   13.1915(12)
_cell_measurement_reflns_used    6615
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.64
_cell_volume                     2192.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.966
_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  0.0271
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13409
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.427
_diffrn_reflns_theta_min         2.220
_exptl_absorpt_coefficient_mu    3.648
_exptl_absorpt_correction_T_max  0.7125
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5342
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0250P)^2^+0.7817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4733
_reflns_number_total             5342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00933g2.cif
_cod_data_source_block           2(Ba)
_cod_database_code               7049625
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2WA,H2WB} of O2W, All C(H,H) groups
 At 1.5 times of:
  {H3WA,H3WB} of O3W, {H1WA,H1WB} of O1W, {H4WC,H4WD} of O4WB, {H4WA,H4WB} of
  O4WA, {H6WA,H6WB} of O6W
2. Rigid bond restraints
 O5, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O5WA) \\sim Ueq, Uanis(O7WB) \\sim Ueq, Uanis(O7WA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5WB) \\sim Ueq, Uanis(O7WB) \\sim Ueq, Uanis(O7WA) \\sim Ueq,
Uanis(O5WA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O4WA(0.5) H4WA(0.5) H4WB(0.5) O4WB(0.5) H4WC(0.5) H4WD(0.5)
 O5(0.5) O5A(0.5) O5WA(0.5) O5WB(0.5) O7WA(0.5) O7WB(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O6W(H6WA,H6WB)
5.b Rotating group:
 O4WA(H4WA,H4WB), O4WB(H4WC,H4WD)
5.c Secondary CH2 refined with riding coordinates:
 O2W(H2WA,H2WB), C9(H9A,H9B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11)
;
_shelx_res_checksum              68611
_shelx_hkl_checksum              52789
_olex2_submission_special_instructions 'No special instructions were received'