#------------------------------------------------------------------------------
#$Date: 2024-04-16 00:47:36 +0200 (Tue 16 de Apr de 2024) $
#$Revision: 291203 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/84/7248407.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_7248407
loop_
_publ_author_name
'Igoa, Fernando'
'López Cabrera, Agustín'
'Gonzalez-Platas, Javier'
'Suescun, Leopoldo'
'Kremer, Carlos'
'Torres, Julia'
_publ_section_title
;
 Extended isomerism in heteronuclear metal-organic frameworks: synthetic
 strategies and crystal structures of lanthanide-cobalt-oxydiacetate
 systems
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00168K
_journal_year                    2024
_chemical_formula_moiety         'C24 H30 Co3 Ho2 O36, 4.5(O)'
_chemical_formula_sum            'C24 H30 Co3 Ho2 O40.5'
_chemical_formula_weight         1473.13
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-28 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.5351(9)
_cell_length_b                   14.5351(9)
_cell_length_c                   15.8928(10)
_cell_measurement_reflns_used    3167
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.5880
_cell_measurement_theta_min      2.5620
_cell_volume                     2907.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     41.00  66.00   1.00   30.00    --   -0.39  57.00 120.00   25
  2  ω     -2.00  23.00   1.00   30.00    --   -0.39  57.00 120.00   25
  3  ω     57.00 106.00   1.00  120.00    --   30.13 178.00-120.00   49
  4  ω     -7.00  34.00   1.00  120.00    --  -30.91  57.00  90.00   41
  5  ω   -102.00  -6.00   1.00  120.00    --  -30.91 -57.00 -60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0151997000
_diffrn_orient_matrix_UB_12      0.0518810000
_diffrn_orient_matrix_UB_13      0.0141913000
_diffrn_orient_matrix_UB_21      -0.0055976000
_diffrn_orient_matrix_UB_22      -0.0174900000
_diffrn_orient_matrix_UB_23      0.0423834000
_diffrn_orient_matrix_UB_31      0.0539504000
_diffrn_orient_matrix_UB_32      0.0128434000
_diffrn_orient_matrix_UB_33      0.0003794000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7362
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         2.803
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.621
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             1426
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0292
_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)+(0.0461P)²+6.2785P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                935
_reflns_number_total             1250
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00168k2.cif
_cod_data_source_block           hex_hocooda
_cod_original_cell_volume        2907.8(4)
_cod_original_formula_sum        'C24 H30 Co3 Ho2 O40.50'
_cod_database_code               7248407
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Ho2 Co3 C24 H36 O40'
_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.
;
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1W(0.5) O2W(0.125) O3W(0.25)
3.a Rotating group:
 O1W(H1W)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.786
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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
Ho Ho 0.333333 0.666667 0.750000 0.02262(15) Uani 1 6 d S T P . .
Co Co 0.500000 0.500000 0.500000 0.0236(2) Uani 1 4 d S T P . .
O3 O 0.23604(16) 0.4721(3) 0.750000 0.0334(9) Uani 1 2 d S T P . .
O1 O 0.3861(2) 0.5830(2) 0.64669(19) 0.0349(6) Uani 1 1 d . . . . .
O1W O 0.5066(3) 0.6520(3) 0.500000 0.0340(9) Uani 1 2 d S T P . .
H1W H 0.465559 0.660809 0.542883 0.051 Uiso 0.5 1 d R U P . .
O2 O 0.3838(3) 0.4402(3) 0.5908(2) 0.0552(10) Uani 1 1 d . . . . .
C1 C 0.3510(3) 0.4842(3) 0.6404(3) 0.0371(9) Uani 1 1 d . . . . .
C2 C 0.2607(5) 0.4119(4) 0.6960(4) 0.070(2) Uani 1 1 d . . . . .
H2A H 0.199233 0.365883 0.662016 0.084 Uiso 1 1 calc R U . . .
H2B H 0.280093 0.367713 0.728593 0.084 Uiso 1 1 calc R U . . .
O2W O 0.231(4) 0.220(4) 0.500000 0.144(15) Uiso 0.25 2 d S . P . .
O3W O 0.015(3) 0.160(3) 0.690(2) 0.193(14) Uiso 0.25 1 d . . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 -2 0 0.0241
-1 3 5 0.0524
2 -7 0 0.0075
-1 1 0 0.0305
1 -1 0 0.0132
1 0 0 0.0327
-2 7 0 0.0393
0 1 -5 0.0450
0 -1 5 0.0450
-5 2 0 0.0241
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
_geom_angle_publ_flag
O3 Ho O3 120.000(1) 3_565 . ?
O3 Ho O3 120.000(1) 3_565 2_665 ?
O3 Ho O3 120.000(1) 2_665 . ?
O1 Ho O3 136.02(8) 12_566 . ?
O1 Ho O3 73.83(7) . 2_665 ?
O1 Ho O3 63.82(6) . . ?
O1 Ho O3 63.82(6) 11_556 . ?
O1 Ho O3 63.82(7) 10_666 2_665 ?
O1 Ho O3 63.82(6) 2_665 2_665 ?
O1 Ho O3 73.83(7) 3_565 . ?
O1 Ho O3 73.83(7) 2_665 3_565 ?
O1 Ho O3 63.82(6) 3_565 3_565 ?
O1 Ho O3 73.83(7) 12_566 2_665 ?
O1 Ho O3 136.02(7) 2_665 . ?
O1 Ho O3 136.02(8) 3_565 2_665 ?
O1 Ho O3 73.83(7) 11_556 3_565 ?
O1 Ho O3 136.02(7) . 3_565 ?
O1 Ho O3 63.82(6) 12_566 3_565 ?
O1 Ho O3 73.83(7) 10_666 . ?
O1 Ho O3 136.02(7) 10_666 3_565 ?
O1 Ho O3 136.02(7) 11_556 2_665 ?
O1 Ho O1 77.88(11) 12_566 10_666 ?
O1 Ho O1 127.65(13) 12_566 3_565 ?
O1 Ho O1 127.65(13) 11_556 . ?
O1 Ho O1 87.95(15) 10_666 . ?
O1 Ho O1 87.95(15) 3_565 11_556 ?
O1 Ho O1 87.95(15) 12_566 2_665 ?
O1 Ho O1 127.65(13) 2_665 10_666 ?
O1 Ho O1 147.66(14) 3_565 10_666 ?
O1 Ho O1 147.66(14) 12_566 . ?
O1 Ho O1 77.88(11) 12_566 11_556 ?
O1 Ho O1 77.88(11) 3_565 2_665 ?
O1 Ho O1 77.88(11) 11_556 10_666 ?
O1 Ho O1 147.66(14) 11_556 2_665 ?
O1 Ho O1 77.88(11) 2_665 . ?
O1 Ho O1 77.88(11) 3_565 . ?
O1W Co O1W 180.0 . 13_666 ?
O2 Co O1W 92.28(12) 13_666 13_666 ?
O2 Co O1W 87.72(12) 16_556 13_666 ?
O2 Co O1W 92.28(12) 4_665 13_666 ?
O2 Co O1W 87.72(12) . 13_666 ?
O2 Co O1W 87.72(12) 4_665 . ?
O2 Co O1W 92.28(12) 16_556 . ?
O2 Co O1W 87.72(12) 13_666 . ?
O2 Co O1W 92.28(12) . . ?
O2 Co O2 89.2(2) 4_665 13_666 ?
O2 Co O2 90.8(2) 4_665 . ?
O2 Co O2 89.2(2) 16_556 . ?
O2 Co O2 90.8(2) 16_556 13_666 ?
O2 Co O2 180.0 13_666 . ?
O2 Co O2 180.0 16_556 4_665 ?
C2 O3 Ho 122.9(2) . . ?
C2 O3 Ho 122.9(2) 11_556 . ?
C2 O3 C2 114.2(5) . 11_556 ?
C1 O1 Ho 125.6(3) . . ?
Co O1W H1W 115.2 . . ?
C1 O2 Co 132.0(3) . . ?
O1 C1 C2 117.8(4) . . ?
O2 C1 O1 126.2(4) . . ?
O2 C1 C2 116.0(4) . . ?
O3 C2 C1 109.5(4) . . ?
O3 C2 H2A 109.8 . . ?
O3 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho O3 2.449(4) 2_665 ?
Ho O3 2.449(4) . ?
Ho O3 2.449(4) 3_565 ?
Ho O1 2.387(3) . ?
Ho O1 2.387(3) 12_566 ?
Ho O1 2.387(3) 11_556 ?
Ho O1 2.387(3) 3_565 ?
Ho O1 2.387(3) 2_665 ?
Ho O1 2.387(3) 10_666 ?
Co O1W 2.162(4) 13_666 ?
Co O1W 2.162(4) . ?
Co O2 2.055(3) 13_666 ?
Co O2 2.055(3) . ?
Co O2 2.055(3) 4_665 ?
Co O2 2.055(3) 16_556 ?
O3 C2 1.394(5) . ?
O3 C2 1.394(5) 11_556 ?
O1 C1 1.265(5) . ?
O1W H1W 0.9560 . ?
O2 C1 1.250(5) . ?
C1 C2 1.493(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho O3 C2 C1 -1.0(7) . . . . ?
Ho O1 C1 O2 -174.1(4) . . . . ?
Ho O1 C1 C2 6.9(6) . . . . ?
Co O2 C1 O1 -1.2(8) . . . . ?
Co O2 C1 C2 177.8(4) . . . . ?
O1 C1 C2 O3 -3.5(7) . . . . ?
O2 C1 C2 O3 177.4(5) . . . . ?
C2 O3 C2 C1 179.0(6) 11_556 . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5.0159 -1.9622 -0.0867 -0.0268 0.0026 0.2454
-0.9208 2.9770 4.9964 0.2114 0.1649 -0.0095
1.9650 -7.0244 0.0102 -0.3344 0.1123 0.0158
-0.9992 0.9963 0.0130 0.0367 -0.0113 -0.0411
0.9992 -0.9963 -0.0130 -0.0367 0.0113 0.0411
1.0058 0.0101 -0.0202 0.0155 -0.0067 0.0544
-1.9650 7.0244 -0.0102 0.3344 -0.1123 -0.0158
-0.0584 1.0384 -5.0051 -0.0180 -0.2300 0.0083
0.0584 -1.0384 5.0051 0.0180 0.2300 -0.0083
-5.0159 1.9622 0.0867 0.0268 -0.0026 -0.2454
