Testing mixed metal bimetallic, and monometallic, cryptates for electrocatalytic hydrogen evolution.
Singh, Varinder; Robb, Matthew G.; Brooker, Sally; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3165–3173; doi:10.1039/d4dt03161j

data_7717801
_publ_section_title
;
 Testing mixed metal bimetallic, and monometallic, cryptates for
 electrocatalytic hydrogen evolution.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3165
_journal_page_last               3173
_journal_paper_doi               10.1039/d4dt03161j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H36 N14 Zn, 2(B F4)'
_chemical_formula_sum            'C30 H36 B2 F8 N14 Zn'
_chemical_formula_weight         831.72
_chemical_name_common            'monometallic Zn(II) cryptate'
_chemical_name_systematic        '[Zn(II)Li](BF4)2'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2025-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.359(2)
_cell_angle_beta                 87.624(2)
_cell_angle_gamma                76.780(2)
_cell_formula_units_Z            4
_cell_length_a                   9.5340(2)
_cell_length_b                   13.1923(4)
_cell_length_c                   28.9592(6)
_cell_measurement_reflns_used    24179
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.6680
_cell_measurement_theta_min      3.8310
_cell_volume                     3533.21(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.815
_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   -130.00 -39.00   1.00    1.00    --  -42.04-178.00-180.00   91
  2  \w    -70.00  31.00   1.00    1.00    --  -42.04  57.00-180.00  101
  3  \w   -114.00 -14.00   1.00    1.00    --  -42.04 -57.00  30.00  100
  4  \w    -21.00  75.00   1.00    1.00    --   42.04 -77.00 -90.00   96
  5  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00  30.00   84
  6  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00 -30.00   84
  7  \w     28.00 133.00   1.00    1.00    --  104.32 -30.00 -60.00  105
  8  \w    103.00 178.00   1.00    1.00    --  104.32  77.00-120.00   75
  9  \w     32.00 133.00   1.00    1.00    --  104.32 -61.00  90.00  101
 10  \w     23.00 157.00   1.00    1.00    --  104.32 -15.00  90.00  134
 11  \w     22.00 106.00   1.00    1.00    --  104.32 -95.00 120.00   84
 12  \w     31.00 112.00   1.00    1.00    --  104.32-125.00 -90.00   81
 13  \w     31.00 130.00   1.00    1.00    --  104.32 -45.00  30.00   99
 14  \w     28.00 133.00   1.00    1.00    --  104.32 -30.00-150.00  105
 15  \w    103.00 178.00   1.00    1.00    --  104.32  77.00  90.00   75
 16  \w    103.00 178.00   1.00    1.00    --  104.32  77.00   0.00   75
 17  \w     29.00 110.00   1.00    1.00    --  104.32-114.00 -65.46   81
 18  \w   -116.00 -18.00   1.00    1.00    --  -42.04 -38.00-150.00   98
 19  \w      8.00  34.00   1.00    1.00    --   42.04  83.00  -1.92   26
 20  \w      9.00  42.00   1.00    1.00    --   42.04  79.00-139.39   33
 21  \w      8.00  42.00   1.00    1.00    --   42.04  82.00 -75.13   34
 22  \w      9.00  42.00   1.00    1.00    --   42.04  80.00 170.61   33
 23  \w     76.00 178.00   1.00    1.00    --  104.32  30.00 -30.00  102
 24  \w     52.00 178.00   1.00    1.00    --  104.32  15.00-150.00  126
 25  \w     75.00 136.00   1.00    1.00    --  104.32  61.00  30.00   61
 26  \w     75.00 177.00   1.00    1.00    --  104.32  61.00-120.00  102
 27  \w     75.00 177.00   1.00    1.00    --  104.32  61.00  90.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0283704000
_diffrn_orient_matrix_UB_12      0.1070315000
_diffrn_orient_matrix_UB_13      -0.0175951000
_diffrn_orient_matrix_UB_21      -0.1536028000
_diffrn_orient_matrix_UB_22      0.0331654000
_diffrn_orient_matrix_UB_23      -0.0189920000
_diffrn_orient_matrix_UB_31      -0.0562805000
_diffrn_orient_matrix_UB_32      0.0437246000
_diffrn_orient_matrix_UB_33      0.0466900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            52456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.922
_diffrn_reflns_theta_min         3.451
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_preparation       'tested as hydrogen electrocatalyst'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: from MeCN by vapour diffusion of diethylether'
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         13811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0060P)^2^+21.8004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12910
_reflns_number_total             13811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03161j2.cif
_cod_data_source_block           vxsznli
_cod_depositor_comments
'Adding full bibliography for 7717799--7717801.cif.'
_cod_database_code               7717801
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C30H36N14ZnB2F8
_chemical_oxdiff_usercomment     M777
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9905(5)
 0.0095(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C01M(H01A,H01B), C01N(H01C,H01E), C026(H02Z,H), C028(H02A,H02B), C029(H02,HA),
  C02A(H1,HB), C02B(H02C,H02D), C02C(H02E,H02F), C02D(H2,HC), C02E(H3,HD),
 C02F(H02G,H02H), C02G(H02I,H02J), C02H(H4,HE), C02L(H02L,H02M), C02N(H7,HF),
 C02O(H02O,H02P), C02P(H8,HG), C02Q(H02Q,H02R), C02S(H10,HH), C02T(H02S,H02T),
 C02U(H02U,H02V), C02V(H02W,H02X), C02W(H02Y,HI), C02X(H11,HJ)
3.b Aromatic/amide H refined with riding coordinates:
 C01D(H01D), C01J(H01J), C01K(H01K), C01L(H01L), C01O(H01O), C01P(H01P),
 C01S(H01S), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Z(H01Z),
 C020(H020), C021(H021), C022(H022), C023(H023), C024(H024), C027(H027),
 C02I(H5), C02J(H02K), C02K(H6), C02M(H02N), C02R(H9), C02Y(H12)
;
_shelx_res_checksum              64863
_shelx_hkl_checksum              54246
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.775