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_4128058
_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 Ca0.07 Co0.5 F6 Mn0.43 O4'
_chemical_formula_sum            'C17 H8 Ca0.07 Co0.5 F6 Mn0.43 O4'
_chemical_formula_weight         446.18
_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                   21.2499(7)
_cell_length_b                   21.2499(7)
_cell_length_c                   15.2397(6)
_cell_measurement_reflns_used    4166
_cell_measurement_temperature    250
_cell_measurement_theta_max      56.413
_cell_measurement_theta_min      2.401
_cell_volume                     5959.7(4)
_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      250
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1257
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35814
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        65.842
_diffrn_reflns_theta_max         65.842
_diffrn_reflns_theta_min         2.401
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.615
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1476 before and 0.1007 after correction. The Ratio of minimum to maximum transmission is 0.4890. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       needle
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 879 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1002P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2702
_reflns_number_total             3435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Mn0.23Co0.50Ca0.27(hfipbb).cif
_cod_data_source_block           1
_cod_original_cell_volume        5959.6(5)
_cod_original_formula_sum        'C17 H8 Ca0.07 Co0.50 F6 Mn0.43 O4'
_cod_database_code               4128058
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.620
_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)
3. Others
 Sof(Ca2)=0.5*(1-FVAR(2))
 Sof(Mn2)=0.5*FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C12(H12), C14(H14), C16(H16), C21(H21), C23(H23), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'