#------------------------------------------------------------------------------
#$Date: 2019-11-03 10:53:11 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221194 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/80/4128063.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4128063
loop_
_publ_author_name
'Castillo-Blas, Celia'
'López-Salas, Nieves'
'Gutiérrez, María C'
'Puente-Orench, Inés'
'Gutiérrez-Puebla, Enrique'
'Ferrer, M. Luisa'
'Monge, M Ángeles'
'Gándara, Felipe'
_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 Co0.36 F6 Mn0.49 O4 Zn0.14, 0.17(O)'
_chemical_formula_sum            'C17 H8 Co0.36 F6 Mn0.49 O4.17 Zn0.14'
_chemical_formula_weight         450.40
_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             2018-05-10
_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                   21.2423(6)
_cell_length_b                   21.2423(6)
_cell_length_c                   15.1282(6)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      65.695
_cell_measurement_theta_min      2.401
_cell_volume                     5911.8(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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Data Vantec 500'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.690
_diffrn_reflns_theta_max         65.690
_diffrn_reflns_theta_min         2.402
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.128
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1474 before and 0.0973 after correction. The Ratio of minimum to maximum transmission is 0.6141. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       needle
_exptl_crystal_F_000             2683
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1172 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0394
_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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3117
_reflns_number_total             3427
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Zn0.16Mn0.47Co0.33Ca0.03hfipbb-ZnMnCoCa1441.cif
_cod_data_source_block           1test
_cod_original_cell_volume        5911.8(4)
_cod_database_code               4128063
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(Co1)=0.5*(1-FVAR(2))
 Sof(Zn1)=0.5*FVAR(2)
 Fixed Sof: O0AA(0.16667)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C16(H16), C18(H18), C22(H22), C23(H23), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+5/6'
'-y, x-y, z+2/3'
'-x, -y, z+1/2'
'-x+y, -x, z+1/3'
'y, -x+y, z+1/6'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'y, x, -z+2/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.2832(2) 0.7168(2) 0.0833 0.012(3) Uani 0.275(18) 2 d S T P A 1
Mn2 Mn 0.35019(5) 0.67510(3) -0.0833 0.0214(4) Uani 0.989(6) 2 d S T P A .
O1 O 0.25571(16) 0.62542(16) 0.0201(2) 0.0259(7) Uani 1 1 d . . . . .
O2 O 0.42413(17) 0.73286(18) 0.0214(2) 0.0308(8) Uani 1 1 d . . . . .
O3 O 0.34451(19) 0.76942(18) -0.1091(2) 0.0327(8) Uani 1 1 d . . . . .
F4 F 0.2960(2) 1.09378(19) -0.1489(3) 0.0570(10) Uani 1 1 d . . . . .
F5 F 0.2513(2) 1.1108(2) -0.2674(3) 0.0716(13) Uani 1 1 d . . . . .
F6 F 0.2616(2) 0.9531(2) -0.4056(3) 0.0618(11) Uani 1 1 d . . . . .
F7 F 0.18758(19) 1.0158(2) -0.1888(3) 0.0695(13) Uani 1 1 d . . . . .
C8 C 0.3205(3) 0.8054(2) -0.0712(3) 0.0304(11) Uani 1 1 d . . . . .
O9 O 0.2987(2) 0.7960(2) 0.0082(2) 0.0378(9) Uani 1 1 d . . . . .
F10 F 0.20531(19) 1.0122(2) -0.3891(3) 0.0712(13) Uani 1 1 d . . . . .
F11 F 0.17417(19) 0.9165(2) -0.3118(3) 0.0733(14) Uani 1 1 d . . . . .
C12 C 0.2817(3) 0.8976(3) -0.0820(4) 0.0379(12) Uani 1 1 d . . . . .
H12 H 0.2656 0.8868 -0.0239 0.045 Uiso 1 1 calc R . . . .
C13 C 0.5700(2) 1.2409(2) -0.4036(3) 0.0252(10) Uani 1 1 d . . . . .
C14 C 0.3679(3) 1.1122(3) -0.3919(4) 0.0364(12) Uani 1 1 d . . . . .
H14 H 0.3272 1.0980 -0.4274 0.044 Uiso 1 1 calc R . . . .
C15 C 0.4215(3) 1.1041(3) -0.2567(3) 0.0321(11) Uani 1 1 d . . . . .
H15 H 0.4170 1.0841 -0.2007 0.038 Uiso 1 1 calc R . . . .
C16 C 0.4351(3) 1.1648(3) -0.4214(3) 0.0324(11) Uani 1 1 d . . . . .
H16 H 0.4394 1.1858 -0.4767 0.039 Uiso 1 1 calc R . . . .
C17 C 0.3150(3) 0.8632(3) -0.1210(3) 0.0297(10) Uani 1 1 d . . . . .
C18 C 0.3324(3) 0.9326(3) -0.2525(4) 0.0342(11) Uani 1 1 d . . . . .
H18 H 0.3505 0.9451 -0.3097 0.041 Uiso 1 1 calc R . . . .
C19 C 0.2866(3) 1.0205(3) -0.2716(4) 0.0366(12) Uani 1 1 d . . . . .
C20 C 0.4967(3) 1.1870(2) -0.3695(3) 0.0282(10) Uani 1 1 d . . . . .
C21 C 0.2315(3) 0.9757(3) -0.3450(5) 0.0558(18) Uani 1 1 d . . . . .
C22 C 0.2720(3) 0.9484(3) -0.1293(4) 0.0390(12) Uani 1 1 d . . . . .
H22 H 0.2483 0.9704 -0.1031 0.047 Uiso 1 1 calc R . . . .
C23 C 0.3412(3) 0.8812(3) -0.2076(4) 0.0333(11) Uani 1 1 d . . . . .
H23 H 0.3642 0.8587 -0.2344 0.040 Uiso 1 1 calc R . . . .
C24 C 0.2550(3) 1.0601(3) -0.2184(5) 0.0512(17) Uani 1 1 d . . . . .
C25 C 0.2973(3) 0.9662(3) -0.2149(4) 0.0339(12) Uani 1 1 d . . . . .
C26 C 0.4888(3) 1.1569(3) -0.2859(3) 0.0293(10) Uani 1 1 d . . . . .
H26 H 0.5292 1.1726 -0.2495 0.035 Uiso 1 1 calc R . . . .
C27 C 0.3601(3) 1.0801(3) -0.3096(3) 0.0301(10) Uani 1 1 d . . . . .
O0AA O 0.519(2) 1.0000 0.0000 0.22(3) Uani 0.3333 2 d S T P . .
Co1 Co 0.28318(15) 0.71682(15) 0.0833 0.0280(17) Uani 0.725(18) 2 d S T P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Zn1 O1 106.9(4) . 10_665
O9 Zn1 O1 108.40(15) 10_665 .
O9 Zn1 O1 108.39(15) . 10_665
O9 Zn1 O1 114.36(14) . .
O9 Zn1 O1 114.36(14) 10_665 10_665
O9 Zn1 O9 104.7(5) . 10_665
O1 Mn2 O1 84.04(15) . 12_564
O2 Mn2 O1 164.90(12) 12_564 .
O2 Mn2 O1 88.93(11) . .
O2 Mn2 O1 88.93(11) 12_564 12_564
O2 Mn2 O1 164.90(12) . 12_564
O2 Mn2 O2 100.83(18) . 12_564
O3 Mn2 O1 79.47(12) . 12_564
O3 Mn2 O1 96.25(13) . .
O3 Mn2 O1 96.26(13) 12_564 12_564
O3 Mn2 O1 79.47(12) 12_564 .
O3 Mn2 O2 95.57(13) . 12_564
O3 Mn2 O2 95.56(13) 12_564 .
O3 Mn2 O2 88.07(13) 12_564 12_564
O3 Mn2 O2 88.07(13) . .
O3 Mn2 O3 174.3(2) . 12_564
Zn1 O1 Mn2 96.62(14) . .
C13 O1 Zn1 115.3(3) 9_454 .
C13 O1 Mn2 124.3(3) 9_454 .
C13 O1 Co1 115.3(3) 9_454 .
Co1 O1 Mn2 96.63(13) . .
C13 O2 Mn2 144.6(3) 4_675 .
C8 O3 Mn2 137.1(3) . .
O3 C8 O9 124.6(4) . .
O3 C8 C17 119.6(5) . .
O9 C8 C17 115.8(4) . .
C8 O9 Zn1 126.1(4) . .
C8 O9 Co1 126.1(3) . .
C17 C12 C22 120.3(5) . .
O1 C13 C20 117.1(4) 9_564 .
O2 C13 O1 123.3(4) 4_674 9_564
O2 C13 C20 119.5(4) 4_674 .
C16 C14 C27 120.6(5) . .
C26 C15 C27 120.9(5) . .
C14 C16 C20 120.7(5) . .
C12 C17 C8 119.4(5) . .
C12 C17 C23 119.7(5) . .
C23 C17 C8 120.9(4) . .
C23 C18 C25 121.8(5) . .
C21 C19 C27 112.3(5) . .
C24 C19 C21 108.0(5) . .
C24 C19 C25 112.7(5) . .
C24 C19 C27 106.5(4) . .
C25 C19 C21 106.8(4) . .
C25 C19 C27 110.6(4) . .
C16 C20 C13 120.6(4) . .
C26 C20 C13 120.6(4) . .
C26 C20 C16 118.8(5) . .
F6 C21 F10 106.2(6) . .
F6 C21 C19 111.3(5) . .
F10 C21 C19 114.1(6) . .
F11 C21 F6 107.1(6) . .
F11 C21 F10 106.5(5) . .
F11 C21 C19 111.2(5) . .
C25 C22 C12 120.3(5) . .
C18 C23 C17 119.1(5) . .
F4 C24 F5 107.0(5) . .
F4 C24 F7 107.3(6) . .
F4 C24 C19 111.3(5) . .
F5 C24 C19 111.5(5) . .
F7 C24 F5 106.1(5) . .
F7 C24 C19 113.3(5) . .
C18 C25 C19 118.4(5) . .
C22 C25 C18 118.7(5) . .
C22 C25 C19 122.9(5) . .
C15 C26 C20 120.4(5) . .
C14 C27 C15 118.5(4) . .
C14 C27 C19 123.9(4) . .
C15 C27 C19 117.6(4) . .
O1 Co1 O1 106.8(3) . 10_665
O9 Co1 O1 114.37(14) 10_665 10_665
O9 Co1 O1 108.39(15) . 10_665
O9 Co1 O1 108.40(15) 10_665 .
O9 Co1 O1 114.36(14) . .
O9 Co1 O9 104.7(3) . 10_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.972(6) 10_665
Zn1 O1 1.972(6) .
Zn1 O9 1.918(6) 10_665
Zn1 O9 1.918(6) .
Mn2 O1 2.339(3) .
Mn2 O1 2.339(3) 12_564
Mn2 O2 2.135(3) .
Mn2 O2 2.135(3) 12_564
Mn2 O3 2.103(3) 12_564
Mn2 O3 2.103(3) .
O1 C13 1.299(6) 9_454
O1 Co1 1.973(4) .
O2 C13 1.243(6) 4_675
O3 C8 1.250(6) .
F4 C24 1.323(8) .
F5 C24 1.342(7) .
F6 C21 1.336(9) .
F7 C24 1.338(7) .
C8 O9 1.267(6) .
C8 C17 1.494(6) .
O9 Co1 1.917(5) .
F10 C21 1.337(7) .
F11 C21 1.336(7) .
C12 C17 1.379(8) .
C12 C22 1.393(8) .
C13 O1 1.299(6) 9_564
C13 O2 1.243(6) 4_674
C13 C20 1.490(6) .
C14 C16 1.375(7) .
C14 C27 1.390(7) .
C15 C26 1.376(7) .
C15 C27 1.392(7) .
C16 C20 1.392(7) .
C17 C23 1.399(7) .
C18 C23 1.376(7) .
C18 C25 1.385(8) .
C19 C21 1.547(9) .
C19 C24 1.540(8) .
C19 C25 1.544(7) .
C19 C27 1.548(7) .
C20 C26 1.389(7) .
C22 C25 1.381(8) .
Co1 O1 1.973(4) 10_665
Co1 O9 1.917(5) 10_665
