Water-mediated proton conduction in Ni(ii) and Co(ii) benzenetriphosphonates
Feng, Lu; Pan, Zhi-Quan; Zhou, Hong; Zhou, Min; Hou, Hao-Bo; Dalton Transactions  (2019) –; doi:10.1039/C9DT02960E

data_7701114
_publ_section_title
;
 Water-mediated proton conduction in Ni(ii) and Co(ii)
 benzenetriphosphonates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02960E
_journal_year                    2019
_chemical_formula_moiety         'C20 H26 N4 Ni O4, 2(C9 H13 O9 P3), 9(H2 O)'
_chemical_formula_sum            'C38 H70 N4 Ni O31 P6'
_chemical_formula_weight         1323.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-12 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.057(2)
_cell_angle_beta                 98.106(2)
_cell_angle_gamma                101.379(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5385(5)
_cell_length_b                   12.3978(6)
_cell_length_c                   22.3593(12)
_cell_measurement_reflns_used    6866
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.81
_cell_volume                     2783.2(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29664
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.425
_diffrn_reflns_theta_min         2.812
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0370P)^2^+1.3505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6960
_reflns_number_total             10129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02960e2.cif
_cod_data_source_block           1
_cod_database_code               7701114
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              30203