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_4518190
_publ_section_title
;
 Bioinspired Carboxylate--Water Coordination Polymers with Hydrogen-Bond
 Clusters and Local Coordination Flexibility for Electrochemical Water
 Splitting
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_journal_name_full               'ACS Applied Energy Materials'
_journal_paper_doi               10.1021/acsaem.0c01552
_journal_year                    2020
_chemical_formula_moiety         'C23 H20 Co2 O17, 1.5(H2 O)'
_chemical_formula_sum            'C23 H23 Co2 O18.5'
_chemical_formula_weight         713.27
_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             2020-09-18
_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                 127.180(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.130(2)
_cell_length_b                   14.8945(12)
_cell_length_c                   19.8961(16)
_cell_measurement_reflns_used    5898
_cell_measurement_temperature    339.98(10)
_cell_measurement_theta_max      29.7980
_cell_measurement_theta_min      1.7510
_cell_volume                     5697.3(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      339.98(10)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.1218
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17700
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.730
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.423
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         4912
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0910
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1939P)^2^+11.2506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2644
_refine_ls_wR_factor_ref         0.2789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3742
_reflns_number_total             4912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ae0c01552_si_004.cif
_cod_data_source_block           Co-HL-67degree
_cod_original_cell_volume        5697.2(10)
_cod_original_formula_sum        'C23 H23 Co2 O18.50'
_cod_database_code               4518190
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.691
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H15A,H15B} of O15
 At 1.5 times of:
  All O(H) groups, {H19A,H19B} of O19, {H20A,H20B} of O20, {H13A,H13B} of O13,
   {H16A,H16B} of O16, {H17A,H17B} of O17, {H14A,H14B} of O14, {H18A,H18B} of
  O18
2. Restrained distances
 O16-H16A = O16-H16B
 0.85 with sigma of 0.02
 O18-H18A = O18-H18B
 0.85 with sigma of 0.02
 O17-H17A = O17-H17B
 0.85 with sigma of 0.02
 O14-H14A = O14-H14B
 0.85 with sigma of 0.02
 O13-H13A = O13-H13B
 0.85 with sigma of 0.02
 O20-H20A = O20-H20B
 0.85 with sigma of 0.02
 H18A-H18B
 1.34 with sigma of 0.04
 H16A-H16B
 1.34 with sigma of 0.04
 H17A-H17B
 1.34 with sigma of 0.04
 H20A-H20B
 1.34 with sigma of 0.04
 H14A-H14B
 1.34 with sigma of 0.04
 H13A-H13B
 1.34 with sigma of 0.04
 Co2-H16A \\sim Co2-H16B
 with sigma of 0.02
 Co1-H14A \\sim Co1-H14B
 with sigma of 0.02
 Co2-H17A \\sim Co2-H17B
 with sigma of 0.02
 Co1-H13A \\sim Co1-H13B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O19) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: H18A(0.5) H18B(0.5) O19(0.5) H19A(0.5) H19B(0.5) O20(0.5)
 H20A(0.5) H20B(0.5)
5.a Riding coordinates:
 O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
5.b Secondary CH2 refined with riding coordinates:
 O15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C7(H7), C9(H9), C11(H11), C13(H13), C17(H17), C19(H19), C21(H21),
 C23(H23)
5.d Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_shelx_res_checksum              38305
_shelx_hkl_checksum              68416
_olex2_submission_special_instructions 'No special instructions were received'