3D Ni and Co redox-active metal-organic frameworks based on ferrocenyl diphosphinate and 4,4'-bipyridine ligands as efficient electrocatalysts for the hydrogen evolution reaction.
Khrizanforova, Vera; Shekurov, Ruslan; Miluykov, Vasily; Khrizanforov, Mikhail; Bon, Volodymyr; Kaskel, Stefan; Gubaidullin, Aidar; Sinyashin, Oleg; Budnikova, Yulia; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2794–2802; doi:10.1039/c9dt04834k

data_7703381
_publ_section_title
;
 3D Ni and Co redox-active metal-organic frameworks based on ferrocenyl
 diphosphinate and 4,4'-bipyridine ligands as efficient electrocatalysts
 for the hydrogen evolution reaction.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2794
_journal_page_last               2802
_journal_paper_doi               10.1039/c9dt04834k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C21 H22 Fe N2 Ni O5 P2'
_chemical_formula_weight         558.90
_chemical_name_systematic        NibpyfcdHp
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2019-12-08 deposited with the CCDC.	2020-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.710(2)
_cell_length_b                   17.590(4)
_cell_length_c                   11.290(2)
_cell_measurement_reflns_used    274
_cell_measurement_temperature    263(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.7
_cell_volume                     2126.9(7)
_computing_cell_refinement       'XDSAPP 2.0'
_computing_data_collection       MarCCD
_computing_data_reduction        'XDSAPP 2.0'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      263(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       '\D\f scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88556
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16045
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        32.096
_diffrn_reflns_theta_max         35.094
_diffrn_reflns_theta_min         2.886
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2354
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.361
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0581P)^2^+3.6743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2036
_reflns_number_total             2354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04834k2.cif
_cod_data_source_block           rs488_a
_cod_depositor_comments          'Adding full bibliography for 7703381.cif.'
_cod_database_code               7703381
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              81587