Structure and magnetic properties of an amine-templated one-dimensional cobalt-fluoro-sulfate containing Co4F4 Cubane & hydrogen evolution reaction (HER) performance of its derived carbon-wrapped CoSe2 nanorods
Behera, Jogendra Nath; Sahoo, Malaya Kumar; Dalton Transactions  (2023) –; doi:10.1039/D3DT01789C

data_7713474
_publ_section_title
;
 Structure and magnetic properties of an amine-templated one-dimensional
 cobalt-fluoro-sulfate containing Co4F4 Cubane &amp; hydrogen evolution
 reaction (HER) performance of its derived carbon-wrapped CoSe2 nanorods
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01789C
_journal_year                    2023
_chemical_formula_moiety         'C12 H16 Co4 F4 N8 O12 S3, 2(C2 H8 N)'
_chemical_formula_sum            'C16 H32 Co4 F4 N10 O12 S3'
_chemical_formula_weight         964.41
_chemical_name_systematic        'CobaltFluorocubane 1D MOF'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.375(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8453(8)
_cell_length_b                   8.0828(3)
_cell_length_c                   11.4284(5)
_cell_measurement_reflns_used    15689
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.5900
_cell_measurement_theta_min      3.6480
_cell_volume                     1686.30(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00   7.00   0.50   15.72    --    3.67 -35.00 -44.00  140
  2  \w      1.00  71.00   0.50   15.72    --    3.67  35.00 112.00  140
  3  \w     -7.00  63.00   0.50   15.72    --   -3.98  35.00 112.00  140
  4  \w    -71.00  -1.00   0.50   15.72    --   -3.98 -35.00 -44.00  140
  5  \w    -66.00   9.00   0.50   15.72    --    3.67 -19.00-150.00  150
  6  \w    -19.00  68.00   0.50   15.72    --    3.67  77.00 -90.00  174
  7  \w    -20.00  40.00   0.50   15.72    --    3.67 -99.00-180.00  120
  8  \w     -9.00  18.00   0.50   15.72    --   -3.98 -99.00-150.00   54
  9  \w    -20.00  26.00   0.50   15.72    --   -3.98 -99.00  90.00   92
 10  \w     27.00  53.00   0.50   15.72    --   -3.98  19.00-180.00   52
 11  \w     -6.00  61.00   0.50   15.72    --   -3.98  38.00-150.00  134
 12  \w    -19.00  30.00   0.50   15.72    --   -3.98 -99.00 120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0328086000
_diffrn_orient_matrix_UB_12      0.0328303000
_diffrn_orient_matrix_UB_13      -0.0103932000
_diffrn_orient_matrix_UB_21      0.0118743000
_diffrn_orient_matrix_UB_22      0.0221317000
_diffrn_orient_matrix_UB_23      0.0618507000
_diffrn_orient_matrix_UB_31      0.0170911000
_diffrn_orient_matrix_UB_32      -0.0783092000
_diffrn_orient_matrix_UB_33      0.0131109000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17206
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.713
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_preparation       'solvothermal,Magnetic properties'
_exptl_crystal_recrystallization_method NA
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0711P)^2^+31.2156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3455
_reflns_number_total             3548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01789c2.cif
_cod_data_source_block           cubane
_cod_database_code               7713474
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C32 H56 Co10 F24 N12 O8 S12 '
_diffrn_oxdiff_ac3_digest_frames
;
019b5856969ae961831a891b104466ae5b000262d93
;
_diffrn_oxdiff_ac3_digest_hkl
;
01ce2236316288af4933002790b6a73339f838
;
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C3(H3), C5(H5), C4(H4), C6(H6), N4(H4A)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.831