Encoding Metal-Cation Arrangements in Metal-Organic Frameworks for Programming the Composition of Electrocatalytically Active Multimetal Oxides.
Castillo-Blas, Celia; López-Salas, Nieves; Gutiérrez, María C; Puente-Orench, Inés; Gutiérrez-Puebla, Enrique; Ferrer, M. Luisa; Monge, M Ángeles; Gándara, Felipe; Journal of the American Chemical Society 141 (2019) 1766–1774; doi:10.1021/jacs.8b12860

data_4128062
_publ_section_title
;
 Encoding Metal-Cation Arrangements in Metal-Organic Frameworks for
 Programming the Composition of Electrocatalytically Active Multimetal
 Oxides.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1766
_journal_page_last               1774
_journal_paper_doi               10.1021/jacs.8b12860
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C17 H8 Ca0.21 Co0.12 F6 Mn0.29 O4 Zn0.38'
_chemical_formula_sum            'C17 H8 Ca0.21 Co0.12 F6 Mn0.29 O4 Zn0.38'
_chemical_formula_weight         446.47
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   21.2824(18)
_cell_length_b                   21.2824(18)
_cell_length_c                   15.3210(14)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      65.538
_cell_measurement_theta_min      2.397
_cell_volume                     6009.8(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      296.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Vantec 500'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30147
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        65.539
_diffrn_reflns_theta_max         65.539
_diffrn_reflns_theta_min         3.752
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.248
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1697 before and 0.1026 after correction. The Ratio of minimum to maximum transmission is 0.6184. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       needle
_exptl_crystal_F_000             2665
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.913
_refine_diff_density_min         -2.002
_refine_diff_density_rms         0.338
_refine_ls_abs_structure_details
;
 Flack x determined using 1208 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.044(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.655
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.655
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.1315
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3335
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                3156
_reflns_number_total             3351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Zn0.37Mn0.28Co0.13Ca0.22(hfipbb).cif
_cod_data_source_block           1
_cod_original_cell_volume        6009.8(12)
_cod_database_code               4128062
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Mn2) = Uanis(Ca2)
Uanis(Zn1) = Uanis(Co1)
3. Others
 Sof(Ca2)=0.5*(1-FVAR(2))
 Sof(Mn2)=0.5*FVAR(2)
 Sof(Co1)=0.5*(1-FVAR(3))
 Sof(Zn1)=0.5*FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C27(H27)
;
_olex2_submission_special_instructions 'No special instructions were received'