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_4128065
_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 Ca0.04 Co0.06 F6 Mn0.46 O4 Zn0.44, 0.25(O2)'
_chemical_formula_sum            'C17 H8 Ca0.04 Co0.06 F6 Mn0.46 O4.5 Zn0.44'
_chemical_formula_weight         457.40
_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                   21.2232(6)
_cell_length_b                   21.2232(6)
_cell_length_c                   15.1771(6)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    250
_cell_measurement_theta_max      65.526
_cell_measurement_theta_min      2.404
_cell_volume                     5920.3(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0776
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33724
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        65.737
_diffrn_reflns_theta_max         65.737
_diffrn_reflns_theta_min         2.404
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.530
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1377 before and 0.0864 after correction. The Ratio of minimum to maximum transmission is 0.5924. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'bluish violet'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       needle
_exptl_crystal_F_000             2725
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 1128 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1486P)^2^+4.1297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3050
_reflns_number_total             3391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Zn0.46Mn0.34Co0.17Ca0.15(hfipbb).cif
_cod_data_source_block           1
_cod_original_cell_volume        5920.3(4)
_cod_original_formula_sum        'C17 H8 Ca0.04 Co0.06 F6 Mn0.46 O4.50 Zn0.44'
_cod_database_code               4128065
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Zn01) = Uanis(Co01)
Uanis(Mn02) = Uanis(Ca02)
3. Others
 Sof(Co01)=0.5*(1-FVAR(2))
 Sof(Zn01)=0.5*FVAR(2)
 Sof(Ca02)=0.5*(1-FVAR(3))
 Sof(Mn02)=0.5*FVAR(3)
 Fixed Sof: O1(0.25) O0AA(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00J(H00J), C00L(H00L), C00M(H00M), C00P(H00P),
 C00Q(H00Q), C00R(H00R)
;
_olex2_submission_special_instructions 'No special instructions were received'