A two-dimensional Ni(II) coordination polymer based on 3,5-bis(1’,2’,4’-triazol-1’-yl) pyridine ligand for water electro-oxidation
Wang, Chunling; Song, Chuanqqi; Shen, Wen-Hui; Qi, Yuan-Yuan; Xue, Ying; Shi, Yao-Cheng; Yu, Huaguang; Feng, Ligang; Catalysis Science & Technology  (2019) –; doi:10.1039/C9CY00191C

data_1550750
_publ_section_title
;
 A two-dimensional Ni(II) coordination polymer based on
 3,5-bis(1&#x2019;,2&#x2019;,4&#x2019;-triazol-1&#x2019;-yl) pyridine
 ligand for water electro-oxidation
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C9CY00191C
_journal_year                    2019
_chemical_formula_moiety         '0.5(C72 H80 N28 Ni6 O44)'
_chemical_formula_sum            'C36 H40 N14 Ni3 O22'
_chemical_formula_weight         1196.95
_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   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc209bc1
_audit_creation_date             2018-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-16 deposited with the CCDC.    2019-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.669(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1497(19)
_cell_length_b                   7.1876(7)
_cell_length_c                   34.937(4)
_cell_measurement_reflns_used    7959
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.20
_cell_measurement_theta_min      2.34
_cell_volume                     5043.1(9)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            26375
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0745 before and 0.0502 after correction. The Ratio of minimum to maximum transmission is 0.9027. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5783
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+12.7128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3994
_reflns_number_total             5783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy00191c2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        5043.0(9)
_cod_database_code               1550750
_shelx_shelxl_version_number     2014/7
_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
 O8B-C17 \\sim O8-C17 \\sim O9B-C17 \\sim O9-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(O9B) = Uanis(O8) = Uanis(O8B)
4. Others
 Sof(O9)=Sof(O8)=1-FVAR(1)
 Sof(O9B)=Sof(O8B)=FVAR(1)
5.a Rotating group:
 O3(H3A,H3B), O5(H5A,H5B), O4(H4A,H4B), O2(H2A,H2B), O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C7(H7), C15(H15), C8(H8), C5(H5), C4(H4), C2(H2), C1(H1), C13(H13),
 C9(H9)
;
_shelx_res_checksum              7648
_shelx_fab_checksum              71751
_olex2_submission_special_instructions 'No special instructions were received'