Fluorine-based Zn salan complexes
Essien, Nsikak B.; Galvácsi , Antal Tamás; Kállay, Csilla; Al-Hilaly, Youssra Kareem; Gonzalez-Mendez, Ramon; Akien, Geoffrey; Tizzard, Graham J.; Coles, Simon; Besora, Maria; Kostakis, George E.; Dalton Transactions  (2023) –; doi:10.1039/D2DT04082D

data_7712414
_publ_section_title
;
 Fluorine-based Zn salan complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04082D
_journal_year                    2023
_chemical_formula_moiety         'C22 H22 F6 N2 O4 Zn'
_chemical_formula_sum            'C22 H22 F6 N2 O4 Zn'
_chemical_formula_weight         557.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.621(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9548(5)
_cell_length_b                   7.7335(3)
_cell_length_c                   19.8034(6)
_cell_measurement_reflns_used    14107
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.8520
_cell_measurement_theta_min      3.3710
_cell_volume                     2234.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -37.00  28.00   0.50    3.00    --  -46.61  34.00 -25.00  130
  2  \w   -120.00 -34.00   0.50    3.00    --  -46.61 -34.00 176.00  172
  3  \w     34.00 120.00   0.50    3.00    --   46.61  34.00 -25.00  172
  4  \w    -27.00  41.00   0.50    3.00    --   46.61 -34.00 176.00  136
  5  \w     89.00 175.00   0.50   12.00    --  101.75  34.00 -25.00  172
  6  \w   -174.00 -90.00   0.50   12.00    -- -103.00 -34.00 176.00  168
  7  \w   -118.00 -24.00   0.50    3.00    --  -46.61 -77.00 120.00  188
  8  \w    -40.00  27.00   0.50    3.00    --  -46.61  37.00 120.00  134
  9  \w    -24.00  29.00   0.50    3.00    --  -46.61  19.00 120.00  106
 10  \w     34.00 120.00   0.50    3.00    --   46.61  37.00  30.00  172
 11  \w     24.00 118.00   0.50    3.00    --   46.61  77.00  60.00  188
 12  \w     29.00  73.00   0.50   12.00    --  101.75 -61.00-180.00   88
 13  \w     29.00  73.00   0.50   12.00    --  101.75 -61.00   0.00   88
 14  \w     29.00 112.00   0.50   12.00    --  101.75-125.00 120.00  166
 15  \w     79.00 175.00   0.50   12.00    --  101.75  77.00  60.00  192
 16  \w     29.00  73.00   0.50   12.00    --  101.75 -61.00  30.00   88
 17  \w     79.00 152.00   0.50   12.00    --  101.75  77.00  90.00  146
 18  \w     30.00  73.00   0.50   12.00    --  101.75 -61.00 -30.00   86
 19  \w     33.00  94.00   0.50   12.00    --  101.75 -77.00 -90.00  122
 20  \w     29.00  96.00   0.50   12.00    --  101.75 -94.00 -90.00  134
 21  \w     39.00  65.00   0.50   12.00    --  101.75 -61.00  90.00   52
 22  \w   -166.00-140.00   0.50   12.00    -- -103.00 -77.00 120.00   52
 23  \w   -146.00-120.00   0.50   12.00    -- -103.00 -77.00 -90.00   52
 24  \w   -108.00 -81.00   0.50   12.00    -- -103.00 -74.00 134.89   54
 25  \w   -108.00 -81.00   0.50   12.00    -- -103.00 -75.00 102.61   54
 26  \w   -110.00 -83.00   0.50   12.00    -- -103.00 -69.00  83.39   54
 27  \w   -173.00-113.00   0.50   12.00    -- -103.00 -69.00  66.46  120
 28  \w   -172.00 -85.00   0.50   12.00    -- -103.00 -66.00 124.14  174
 29  \w   -108.00 -83.00   0.50   12.00    -- -103.00 -69.00  66.46   50
 30  \w   -174.00-148.00   0.50   12.00    -- -103.00 -77.00 -90.00   52
 31  \w   -133.00 -86.00   0.50   12.00    -- -103.00 -63.00  27.83   94
 32  \w   -109.00 -83.00   0.50   12.00    -- -103.00 -69.00 123.36   52
 33  \w   -105.00 -78.00   0.50   12.00    -- -103.00 -81.00 114.46   54
 34  \w   -173.00-147.00   0.50   12.00    -- -103.00 -68.00  47.00   52
 35  \w   -105.00 -79.00   0.50   12.00    -- -103.00 -79.00  71.68   52
 36  \w   -172.00-127.00   0.50   12.00    -- -103.00 -79.00  71.68   90
 37  \w   -172.00-115.00   0.50   12.00    -- -103.00 -76.00  39.62  114
 38  \w   -106.00 -80.00   0.50   12.00    -- -103.00 -77.00  90.00   52
 39  \w   -106.00 -80.00   0.50   12.00    -- -103.00 -78.00  96.33   52
 40  \w   -110.00 -83.00   0.50   12.00    -- -103.00 -71.00 111.86   54
 41  \w   -121.00 -88.00   0.50   12.00    -- -103.00 -61.00 150.00   66
 42  \w   -116.00 -80.00   0.50   12.00    -- -103.00 -77.00 150.00   72
 43  \w   -170.00-130.00   0.50   12.00    -- -103.00 -61.00 150.00   80
 44  \w   -115.00 -86.00   0.50   12.00    -- -103.00 -61.00  30.00   58
 45  \w    -68.00 -31.00   0.50   12.00    -- -103.00  61.00   0.00   74
 46  \w   -154.00 -83.00   0.50   12.00    -- -103.00 -69.00  75.04  142
 47  \w   -173.00-147.00   0.50   12.00    -- -103.00 -81.00  69.12   52
 48  \w   -104.00 -78.00   0.50   12.00    -- -103.00 -81.00  69.12   52
 49  \w   -173.00 -87.00   0.50   12.00    -- -103.00 -60.00 106.67  172
 50  \w   -114.00 -86.00   0.50   12.00    -- -103.00 -61.00  60.00   56
 51  \w   -104.00 -78.00   0.50   12.00    -- -103.00 -82.00 150.13   52
 52  \w   -110.00 -82.00   0.50   12.00    -- -103.00 -72.00  94.12   56
 53  \w   -130.00 -84.00   0.50   12.00    -- -103.00 -68.00  47.00   92
 54  \w   -106.00 -80.00   0.50   12.00    -- -103.00 -77.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
;
Rigaku 007HF diffractometer equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0060348000
_diffrn_orient_matrix_UB_12      -0.0211024000
_diffrn_orient_matrix_UB_13      -0.0762041000
_diffrn_orient_matrix_UB_21      0.0950636000
_diffrn_orient_matrix_UB_22      -0.0844442000
_diffrn_orient_matrix_UB_23      0.0231881000
_diffrn_orient_matrix_UB_31      -0.0456082000
_diffrn_orient_matrix_UB_32      -0.1791756000
_diffrn_orient_matrix_UB_33      -0.0019620000
_diffrn_radiation_collimation    'Arc)Sec VHF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.523
_diffrn_reflns_theta_min         3.373
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0734P)^2^+5.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3787
_reflns_number_total             4532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04082d2.cif
_cod_data_source_block           1RS
_cod_database_code               7712414
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H16 F6 N2 O4 Zn'
_chemical_oxdiff_usercomment     NBE729
_olex2_refinement_description
;
1. Restrained distances
 N008-C00X \\sim N008-C2
 with sigma of 0.02
 C00O-C00X \\sim C00O-C2
 with sigma of 0.04
 N00B-C00T \\sim N00B-C1
 with sigma of 0.02
 C00O-C00T \\sim C00O-C1
 with sigma of 0.02
 N008-C00T \\sim N008-C1
 with sigma of 0.04
 C00O-C00Y \\sim C00O-C3
 with sigma of 0.02
 C00S-C00T \\sim C00S-C1
 with sigma of 0.04
 C00S-C00X \\sim C00S-C2
 with sigma of 0.02
 C00S-C00Z \\sim C00S-C00{
 with sigma of 0.02
 C00T-C00X \\sim C1-C2
 with sigma of 0.02
 N00B-C00X \\sim N00B-C2
 with sigma of 0.04
 C00O-C00Z \\sim C00O-C00{
 with sigma of 0.04
 C00S-C00Y \\sim C00S-C3
 with sigma of 0.04
 C00Y-C00Z \\sim C3-C00{
 with sigma of 0.02
2. Rigid body (RIGU) restrains
 C00O, C00S, C00T, C00Y, C00Z, C1, C2, C3, C00{, C00X, N00B, N008
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H00A)=Sof(H00J)=Sof(H00L)=Sof(H00Q)=Sof(H00S)=Sof(C1)=Sof(H1)=Sof(C2)=
 Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C00{)=Sof(H00Z)=Sof(HA)=1-FVAR(1)
 Sof(H00B)=Sof(H00G)=Sof(H00I)=Sof(H00N)=Sof(H00O)=Sof(C00T)=Sof(H00T)=
 Sof(C00X)=Sof(H00X)=Sof(C00Y)=Sof(H00V)=Sof(H00W)=Sof(C00Z)=Sof(H00Y)=Sof(H)=
 FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N008(H008), N00B(H00B), N00B(H00A), C00T(H00T), C00X(H00X), C1(H1), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C00L(H00C,H00D), C00N(H00E,H00F), C00O(H00G,H00I), C00O(H00J,H00L), C00S(H00N,
 H00O), C00S(H00Q,H00S), C00Y(H00V,H00W), C00Z(H00Y,H), C3(H3A,H3B), C00{(H00Z,
 HA)
4.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00M(H00M), C00P(H00P), C00R(H00R), C00U(H00U)
;
_shelx_res_checksum              70297
_shelx_hkl_checksum              64147
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id NBE728
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.223
_oxdiff_exptl_absorpt_empirical_full_min 0.580