Bioinspired Carboxylate‒Water Coordination Polymers with Hydrogen-Bond Clusters and Local Coordination Flexibility for Electrochemical Water Splitting
Chen, Junling; Zhang, Heng; Li, Bo; Yang, Jingzhi; Li, Xiongwen; Zhang, Tiexin; He, Cheng; Duan, Chunying; Wang, Liya; ACS Applied Energy Materials  (2020) –; doi:10.1021/acsaem.0c01552

data_4518191
_publ_section_title
;
 Bioinspired Carboxylate--Water Coordination Polymers with Hydrogen-Bond
 Clusters and Local Coordination Flexibility for Electrochemical Water
 Splitting
;
_journal_name_full               'ACS Applied Energy Materials'
_journal_paper_doi               10.1021/acsaem.0c01552
_journal_year                    2020
_chemical_formula_moiety         'C23 H9 Co2 D11 O17, 3(D2 O)'
_chemical_formula_sum            'C23 H9 Co2 D17 O20'
_chemical_formula_weight         757.40
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-20 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.327(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1793(5)
_cell_length_b                   14.7682(3)
_cell_length_c                   19.8874(4)
_cell_measurement_reflns_used    14740
_cell_measurement_temperature    106(5)
_cell_measurement_theta_max      30.4940
_cell_measurement_theta_min      1.7050
_cell_volume                     5647.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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      106(5)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.748
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00  -3.00   0.50    2.00    --   -3.77 -30.00-135.00   88
  2  \w    -10.00  37.00   0.50    2.00    --    3.38 -99.00-180.00   94
  3  \w     39.00  68.00   0.50    2.00    --   -3.77  37.00-150.00   58
  4  \w     10.00  36.00   0.50    2.00    --   -3.77  37.00-150.00   52
  5  \w    -66.00 -35.00   0.50    2.00    --    3.53 -30.00-135.00   62
  6  \w     10.00  36.00   0.50    2.00    --    3.53 -99.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.748
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19545
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.748
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.359
_diffrn_reflns_theta_min         1.739
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.023
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0411P)^2^+35.3879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5966
_reflns_number_total             6369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ae0c01552_si_005.cif
_cod_data_source_block           deuterated-Co-DL
_cod_database_code               4518191
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.742
_shelx_estimated_absorpt_t_min   0.726
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {D15A,D15B} of O15
 At 1.5 times of:
  All O(H) groups, {D17A,D17B} of O17, {D16A,D16B} of O16, {D13A,D13B} of O13,
   {D14A,D14B} of O14, {D19A,D19B} of O19, {D20A,D20B} of O20, {D21A,D21B} of
  O21, {D18A,D18B} of O18
2. Others
 Fixed Sof: O18(0.5) D18A(0.5) D18B(0.5) D20A(0.5) D20B(0.5)
3.a Riding coordinates:
 O13(D13A,D13B), O14(D14A,D14B), O15(D15A,D15B), O16(D16A,D16B), O17(D17A,
 D17B), O18(D18A,D18B), O19(D19A,D19B), O20(D20A,D20B), O21(D21A,D21B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C13(H13), C15(H15), C17(H17), C19(H19), C21(H21),
 C23(H23)
3.c Idealised tetrahedral OH refined as rotating group:
 O6(D6)
;
_shelx_res_checksum              60649
_shelx_hkl_checksum              41977
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;