#------------------------------------------------------------------------------
#$Date: 2019-11-03 10:47:28 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221189 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/80/4128058.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_4128058
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 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       'φ and ω 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 λ/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/[σ²(Fo²)+(0.1002P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_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.
;
_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'
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
Co1 Co 0.71691(4) 0.28309(4) 0.0833 0.0379(4) Uani 1 2 d S T P A .
Mn2 Mn 0.6507(4) 0.3253(2) -0.0833 0.0353(12) Uani 0.87(3) 2 d S T P A 1
O1 O 0.5756(3) 0.2669(3) 0.0219(4) 0.0501(14) Uani 1 1 d . . . . .
O2 O 0.7450(3) 0.3741(3) 0.0204(3) 0.0433(12) Uani 1 1 d . . . . .
F3 F 0.2954(4) 0.0940(4) 0.3488(5) 0.087(2) Uani 1 1 d . . . . .
O4 O 0.6559(3) 0.2302(3) -0.1084(4) 0.0522(14) Uani 1 1 d . . . . .
O5 O 0.7017(4) 0.2043(3) 0.0090(4) 0.0582(16) Uani 1 1 d . . . . .
F6 F 0.2513(4) 0.1105(3) 0.2321(6) 0.099(3) Uani 1 1 d . . . . .
C7 C 0.3681(5) 0.1108(5) 0.1079(6) 0.054(2) Uani 1 1 d . . . . .
H7 H 0.3274 0.0958 0.0715 0.065 Uiso 1 1 calc R . . . .
C8 C 0.7189(5) 0.1021(5) -0.0818(7) 0.055(2) Uani 1 1 d . . . . .
H8 H 0.7360 0.1132 -0.0238 0.066 Uiso 1 1 calc R . . . .
F9 F 0.1877(3) 0.0158(4) 0.3099(6) 0.098(3) Uani 1 1 d . . . . .
F10 F 0.1745(4) -0.0839(4) 0.1886(6) 0.105(3) Uani 1 1 d . . . . .
F11 F 0.2622(4) -0.0485(4) 0.0958(5) 0.090(2) Uani 1 1 d . . . . .
C12 C 0.4211(4) 0.1034(4) 0.2427(6) 0.0491(19) Uani 1 1 d . . . . .
H12 H 0.4165 0.0833 0.2989 0.059 Uiso 1 1 calc R . . . .
C13 C 0.6803(4) 0.1935(4) -0.0698(6) 0.052(2) Uani 1 1 d . . . . .
C14 C 0.4356(4) 0.1639(5) 0.0801(6) 0.052(2) Uani 1 1 d . . . . .
H14 H 0.4401 0.1855 0.0249 0.062 Uiso 1 1 calc R . . . .
C15 C 0.4964(4) 0.1861(4) 0.1308(6) 0.0439(18) Uani 1 1 d . . . . .
C16 C 0.6671(5) 0.0678(4) -0.2516(7) 0.053(2) Uani 1 1 d . . . . .
H16 H 0.6485 0.0555 -0.3089 0.064 Uiso 1 1 calc R . . . .
C17 C 0.2864(5) 0.0192(5) 0.2281(6) 0.056(2) Uani 1 1 d . . . . .
C18 C 0.5695(4) 0.2399(4) 0.0964(5) 0.0410(17) Uani 1 1 d . . . . .
C19 C 0.6850(5) 0.1362(4) -0.1193(6) 0.0464(19) Uani 1 1 d . . . . .
F20 F 0.2050(3) 0.0112(4) 0.1123(5) 0.099(3) Uani 1 1 d . . . . .
C21 C 0.7282(5) 0.0510(5) -0.1299(7) 0.058(2) Uani 1 1 d . . . . .
H21 H 0.7520 0.0283 -0.1041 0.070 Uiso 1 1 calc R . . . .
C22 C 0.2326(6) -0.0251(6) 0.1544(10) 0.085(4) Uani 1 1 d . . . . .
C23 C 0.6588(5) 0.1194(5) -0.2057(6) 0.053(2) Uani 1 1 d . . . . .
H23 H 0.6359 0.1428 -0.2319 0.063 Uiso 1 1 calc R . . . .
C24 C 0.3604(5) 0.0791(4) 0.1909(6) 0.051(2) Uani 1 1 d . . . . .
C25 C 0.7025(4) 0.0337(4) -0.2151(6) 0.050(2) Uani 1 1 d . . . . .
C26 C 0.4887(4) 0.1567(4) 0.2139(6) 0.0469(19) Uani 1 1 d . . . . .
H26 H 0.5294 0.1729 0.2508 0.056 Uiso 1 1 calc R . . . .
C28 C 0.2546(6) 0.0580(6) 0.2799(9) 0.074(3) Uani 1 1 d . . . . .
Ca2 Ca 0.639(4) 0.3194(19) -0.0833 0.0353(12) Uani 0.13(3) 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'
Ca Ca 0.3641 1.2855 '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'
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
O2 Co1 O2 107.8(3) . 10_665
O2 Co1 Ca2 85.1(10) . 5_665
O2 Co1 Ca2 85.1(10) 10_665 .
O2 Co1 Ca2 48.8(9) . .
O2 Co1 Ca2 48.8(9) 10_665 5_665
O5 Co1 O2 114.1(3) 10_665 10_665
O5 Co1 O2 108.3(3) . 10_665
O5 Co1 O2 114.1(3) . .
O5 Co1 O2 108.3(3) 10_665 .
O5 Co1 O5 104.4(4) . 10_665
O5 Co1 Ca2 155.5(11) . 5_665
O5 Co1 Ca2 82.3(2) 10_665 5_665
O5 Co1 Ca2 155.5(11) 10_665 .
O5 Co1 Ca2 82.3(2) . .
Ca2 Co1 Ca2 101.5(7) . 5_665
O1 Mn2 O1 100.6(4) . 12_554
O1 Mn2 O2 88.6(2) . .
O1 Mn2 O2 165.6(2) . 12_554
O1 Mn2 O2 88.6(2) 12_554 12_554
O1 Mn2 O2 165.6(2) 12_554 .
O2 Mn2 O2 84.7(3) . 12_554
O4 Mn2 O1 87.8(2) 12_554 12_554
O4 Mn2 O1 95.6(3) . 12_554
O4 Mn2 O1 95.6(3) 12_554 .
O4 Mn2 O1 87.8(2) . .
O4 Mn2 O2 95.8(3) 12_554 12_554
O4 Mn2 O2 95.8(3) . .
O4 Mn2 O2 80.3(2) . 12_554
O4 Mn2 O2 80.3(2) 12_554 .
O4 Mn2 O4 174.8(5) 12_554 .
C18 O1 Mn2 144.6(6) . .
C18 O1 Ca2 149.1(16) . .
Co1 O2 Mn2 97.0(2) . .
Co1 O2 Ca2 95.3(6) . .
C18 O2 Co1 115.5(5) 10_665 .
C18 O2 Mn2 123.8(5) 10_665 .
C18 O2 Ca2 122.5(6) 10_665 .
C13 O4 Mn2 137.2(6) . .
C13 O4 Ca2 139.7(9) . .
C13 O5 Co1 127.5(6) . .
C14 C7 C24 119.7(8) . .
C19 C8 C21 120.2(9) . .
C24 C12 C26 121.4(8) . .
O4 C13 C19 119.0(8) . .
O4 C13 Ca2 25.4(5) . .
O5 C13 O4 123.2(8) . .
O5 C13 C19 117.9(8) . .
O5 C13 Ca2 97.7(6) . .
C19 C13 Ca2 144.4(7) . .
C15 C14 C7 121.7(8) . .
C14 C15 C18 120.5(8) . .
C14 C15 C26 118.7(8) . .
C26 C15 C18 120.8(7) . .
C23 C16 C25 121.7(9) . .
C22 C17 C24 111.8(8) . .
C25 C17 C22 107.6(8) 4_655 .
C25 C17 C24 110.1(7) 4_655 .
C28 C17 C22 108.4(10) . .
C28 C17 C24 106.7(7) . .
C28 C17 C25 112.3(8) . 4_655
O1 C18 O2 122.7(7) . 10_665
O1 C18 C15 120.1(7) . .
O1 C18 Ca2 19.2(12) . .
O2 C18 C15 117.2(7) 10_665 .
O2 C18 Ca2 104.2(12) 10_665 .
C15 C18 Ca2 137.9(12) . .
C8 C19 C13 119.3(8) . .
C8 C19 C23 120.2(8) . .
C23 C19 C13 120.4(8) . .
C25 C21 C8 120.3(9) . .
F10 C22 C17 109.9(10) . .
F11 C22 F10 107.5(11) . .
F11 C22 C17 112.1(9) . .
F11 C22 F20 108.5(11) . .
F20 C22 F10 104.9(9) . .
F20 C22 C17 113.5(10) . .
C16 C23 C19 118.9(8) . .
C7 C24 C17 123.4(8) . .
C12 C24 C7 118.3(8) . .
C12 C24 C17 118.3(8) . .
C16 C25 C17 118.6(8) . 4_654
C21 C25 C16 118.7(8) . .
C21 C25 C17 122.6(9) . 4_654
C12 C26 C15 120.0(8) . .
F3 C28 F6 103.8(10) . .
F3 C28 C17 112.4(9) . .
F6 C28 C17 112.6(10) . .
F9 C28 F3 106.6(10) . .
F9 C28 F6 105.1(8) . .
F9 C28 C17 115.4(10) . .
Co1 Ca2 Co1 129(2) . 3_654
O1 Ca2 Co1 162.8(14) 12_554 .
O1 Ca2 Co1 62.6(5) . .
O1 Ca2 Co1 162.8(14) . 3_654
O1 Ca2 Co1 62.6(5) 12_554 3_654
O1 Ca2 O1 110(3) . 12_554
O1 Ca2 O2 87.2(6) . .
O1 Ca2 O2 160(2) 12_554 .
O1 Ca2 O2 87.2(6) 12_554 12_554
O1 Ca2 O2 160(2) . 12_554
O1 Ca2 O4 90.7(8) . .
O1 Ca2 O4 99.0(10) . 12_554
O1 Ca2 O4 90.7(8) 12_554 12_554
O1 Ca2 O4 99.0(9) 12_554 .
O1 Ca2 C13 113.5(7) 12_554 .
O1 Ca2 C13 82.7(3) . .
O1 Ca2 C13 113.5(7) . 12_554
O1 Ca2 C13 82.7(3) 12_554 12_554
O1 Ca2 C18 121(3) . 12_554
O1 Ca2 C18 11.7(5) . .
O1 Ca2 C18 121(3) 12_554 .
O1 Ca2 C18 11.7(5) 12_554 12_554
O2 Ca2 Co1 97.9(19) . 3_654
O2 Ca2 Co1 36.0(4) 12_554 3_654
O2 Ca2 Co1 97.9(19) 12_554 .
O2 Ca2 Co1 36.0(4) . .
O2 Ca2 O2 78(2) . 12_554
O2 Ca2 C13 77.8(11) . .
O2 Ca2 C13 81.0(11) 12_554 .
O2 Ca2 C13 77.8(11) 12_554 12_554
O2 Ca2 C13 81.0(11) . 12_554
O2 Ca2 C18 148.5(18) . 12_554
O2 Ca2 C18 148.5(18) 12_554 .
O2 Ca2 C18 76.9(3) 12_554 12_554
O2 Ca2 C18 76.9(3) . .
O4 Ca2 Co1 66.7(7) . .
O4 Ca2 Co1 105.5(12) . 3_654
O4 Ca2 Co1 66.7(7) 12_554 3_654
O4 Ca2 Co1 105.5(12) 12_554 .
O4 Ca2 O2 76.1(14) 12_554 .
O4 Ca2 O2 76.1(14) . 12_554
O4 Ca2 O2 90.6(17) . .
O4 Ca2 O2 90.6(17) 12_554 12_554
O4 Ca2 O4 163(4) 12_554 .
O4 Ca2 C13 14.9(4) . .
O4 Ca2 C13 154(3) . 12_554
O4 Ca2 C13 14.9(4) 12_554 12_554
O4 Ca2 C13 154(3) 12_554 .
O4 Ca2 C18 101.4(7) . 12_554
O4 Ca2 C18 101.4(7) 12_554 .
O4 Ca2 C18 85.5(6) 12_554 12_554
O4 Ca2 C18 85.5(6) . .
C13 Ca2 Co1 114.4(13) . 3_654
C13 Ca2 Co1 51.8(4) . .
C13 Ca2 Co1 51.8(4) 12_554 3_654
C13 Ca2 Co1 114.4(13) 12_554 .
C13 Ca2 C13 153(2) . 12_554
C18 Ca2 Co1 50.90(16) . .
C18 Ca2 Co1 168.0(3) . 3_654
C18 Ca2 Co1 168.0(4) 12_554 .
C18 Ca2 Co1 50.90(16) 12_554 3_654
C18 Ca2 C13 75.4(3) . .
C18 Ca2 C13 116.3(4) 12_554 .
C18 Ca2 C13 116.3(4) . 12_554
C18 Ca2 C13 75.4(3) 12_554 12_554
C18 Ca2 C18 133(2) . 12_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 1.964(5) 10_665
Co1 O2 1.964(5) .
Co1 O5 1.912(6) 10_665
Co1 O5 1.912(5) .
Co1 Ca2 3.33(3) .
Co1 Ca2 3.33(3) 5_665
Mn2 O1 2.162(7) 12_554
Mn2 O1 2.162(7) .
Mn2 O2 2.348(8) 12_554
Mn2 O2 2.348(8) .
Mn2 O4 2.113(6) .
Mn2 O4 2.113(6) 12_554
O1 C18 1.250(10) .
O1 Ca2 2.03(4) .
O2 C18 1.316(9) 10_665
O2 Ca2 2.51(5) .
F3 C28 1.332(15) .
O4 C13 1.276(11) .
O4 Ca2 2.134(12) .
O5 C13 1.264(11) .
F6 C28 1.363(11) .
C7 C14 1.374(12) .
C7 C24 1.403(12) .
C8 C19 1.375(13) .
C8 C21 1.405(12) .
F9 C28 1.327(12) .
F10 C22 1.347(12) .
F11 C22 1.323(17) .
C12 C24 1.375(12) .
C12 C26 1.382(11) .
C13 C19 1.478(11) .
C13 Ca2 3.215(19) .
C14 C15 1.372(11) .
C15 C18 1.489(11) .
C15 C26 1.385(12) .
C16 C23 1.385(12) .
C16 C25 1.395(13) .
C17 C22 1.542(15) .
C17 C24 1.553(11) .
C17 C25 1.529(11) 4_655
C17 C28 1.521(15) .
C18 O2 1.316(9) 10_665
C18 Ca2 3.17(3) .
C19 C23 1.404(13) .
F20 C22 1.343(13) .
C21 C25 1.385(13) .
C25 C17 1.529(11) 4_654
Ca2 Co1 3.33(3) 3_654
Ca2 O1 2.03(4) 12_554
Ca2 O2 2.51(5) 12_554
Ca2 O4 2.134(11) 12_554
Ca2 C13 3.215(19) 12_554
Ca2 C18 3.17(3) 12_554
