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_7712416
_publ_section_title
;
 Fluorine-based Zn salan complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04082D
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C40 H44 F4 N4 O4 Zn2, 2(H2 O)'
_chemical_formula_sum            'C40 H48 F4 N4 O6 Zn2'
_chemical_formula_weight         887.56
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                64.9809(19)
_cell_angle_beta                 75.1697(17)
_cell_angle_gamma                78.0265(16)
_cell_formula_units_Z            1
_cell_length_a                   8.12372(16)
_cell_length_b                   10.6734(2)
_cell_length_c                   12.4777(3)
_cell_measurement_reflns_used    26915
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.9120
_cell_measurement_theta_min      4.7490
_cell_volume                     941.64(4)
_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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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   -111.00  67.00   1.00    1.00    --  -22.00  46.00  56.47  178
  2  \w   -111.00  67.00   1.00    1.00    --  -22.00  46.00  56.47  178
  3  \w   -123.00  55.00   1.00    1.00    --  -34.00  51.00-156.55  178
  4  \w   -131.00  47.00   1.00    1.00    --  -42.00  44.00 -85.10  178
  5  \w   -135.00  43.00   1.00    2.08    --  -46.00  58.00  24.75  178
  6  \w   -139.00  39.00   1.00    2.08    --  -50.00  55.00 171.11  178
  7  \w   -139.00  39.00   1.00    2.08    --  -50.00  55.00-123.39  178
  8  \w   -143.00  35.00   1.00    2.08    --  -54.00  60.00 -20.58  178
  9  \w   -147.00  31.00   1.00    2.08    --  -58.00  58.00  46.27  178
 10  \w   -159.00  19.00   1.00    2.08    --  -70.00  52.00 -44.20  178
 11  \w   -159.00  19.00   1.00    2.08    --  -70.00  55.00-119.82  178
 12  \w   -176.00   2.00   1.00    2.08    --  -87.00  59.00 162.49  178
 13  \w   -176.00   2.00   1.00    2.08    --  -87.00  59.00-145.31  178
 14  \w   -164.00   2.00   1.00    2.08    --  -87.00  60.00 149.58  166
 15  \w   -175.00-149.00   1.00    2.08    --  -87.00  10.00 -30.00   26
 16  \w    -30.00  -3.00   1.00    2.08    --  -87.00  60.00  42.05   27
 17  \w    -51.00   2.00   1.00    2.08    --  -87.00  60.00  30.21   53
 18  \w    -83.00  -1.00   1.00    2.08    --  -87.00  57.00 -55.78   82
 19  \w    -23.00   2.00   1.00    2.08    --  -87.00  60.00  53.77   25
 20  \w   -132.00-105.00   1.00    2.08    --  -87.00  10.00-180.00   27
 21  \w   -121.00   0.00   1.00    2.08    --  -87.00  60.00 -66.96  121
 22  \w   -108.00 -55.00   1.00    2.08    --  -87.00  58.00 101.32   53
 23  \w    -33.00   2.00   1.00    2.08    --  -87.00  58.00 101.32   35
 24  \w   -131.00 -70.00   1.00    2.08    --  -87.00  60.00  30.21   61
 25  \w    -54.00   2.00   1.00    2.08    --  -87.00  53.00-172.71   56
 26  \w   -176.00-150.00   1.00    2.08    --  -87.00  60.00  30.21   26
 27  \w    -25.00   1.00   1.00    2.08    --  -87.00  57.00 177.66   26
 28  \w    -67.00 -42.00   1.00    2.08    --  -87.00  59.00 135.61   25
 29  \w    -27.00   2.00   1.00    2.08    --  -87.00  60.00 -40.31   29
 30  \w    -53.00 -26.00   1.00    2.08    --  -87.00  57.00 177.66   27
 31  \w   -119.00 -75.00   1.00    2.08    --  -87.00  60.00 -40.31   44
 32  \w   -163.00-136.00   1.00    2.08    --  -87.00  60.00 -40.31   27
 33  \w   -175.00   1.00   1.00    2.08    --  -87.00  60.00  64.05  176
 34  \w    -24.00   2.00   1.00    2.08    --  -87.00  59.00 135.61   26
 35  \w   -111.00 -81.00   1.00    2.08    --  -87.00  53.00-172.71   30
 36  \w    -23.00   2.00   1.00    2.08    --  -87.00  59.00-121.40   25
 37  \w   -109.00 -75.00   1.00    2.08    --  -87.00  56.00   7.17   34
 38  \w    -55.00   2.00   1.00    2.08    --  -87.00  56.00   7.17   57
 39  \w    -77.00 -37.00   1.00    2.08    --  -87.00  60.00  42.05   40
 40  \w   -113.00 -84.00   1.00    2.08    --  -87.00  59.00-121.40   29
 41  \w   -176.00-150.00   1.00    2.08    --  -87.00  59.00-121.40   26
 42  \w    -87.00  -1.00   1.00    2.08    --  -87.00  10.00 -30.00   86
 43  \w    -65.00 -40.00   1.00    2.08    --  -87.00  60.00  53.77   25
 44  \w   -126.00   2.00   1.00    2.08    --  -87.00  58.00 117.10  128
 45  \w   -171.00   2.00   1.00    2.08    --  -87.00  58.00 -94.32  173
 46  \w   -117.00 -79.00   1.00    2.08    --  -87.00  59.00 -22.26   38
 47  \w    -56.00   2.00   1.00    2.08    --  -87.00  59.00 -22.26   58
 48  \w    -69.00   1.00   1.00    2.08    --  -87.00  59.00  85.62   70
 49  \w    -84.00  -4.00   1.00    2.08    --  -87.00  10.00-180.00   80
 50  \w   -167.00-138.00   1.00    2.08    --  -87.00  50.00-120.00   29
 51  \w   -113.00 -87.00   1.00    2.08    --  -87.00  50.00-120.00   26
 52  \w    -43.00   1.00   1.00    2.08    --  -87.00  50.00-120.00   44
 53  \w    -77.00 -50.00   1.00    2.08    --  -87.00  58.00  -3.80   27
 54  \w    -26.00   1.00   1.00    2.08    --  -87.00  58.00  -3.80   27
 55  \w   -145.00-118.00   1.00    2.08    --  -87.00  59.00  85.62   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0497353000
_diffrn_orient_matrix_UB_12      0.1422988000
_diffrn_orient_matrix_UB_13      -0.0960380000
_diffrn_orient_matrix_UB_21      0.1745960000
_diffrn_orient_matrix_UB_22      -0.0313435000
_diffrn_orient_matrix_UB_23      0.0386639000
_diffrn_orient_matrix_UB_31      0.0776289000
_diffrn_orient_matrix_UB_32      -0.0668528000
_diffrn_orient_matrix_UB_33      -0.0924084000
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31783
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.124
_diffrn_reflns_theta_max         67.124
_diffrn_reflns_theta_min         4.765
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53783
_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    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0538
_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^)+(0.1114P)^2^+0.6634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                6236
_reflns_number_total             6456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04082d2.cif
_cod_data_source_block           2SS
_cod_database_code               7712416
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Zn C H O N F'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.917
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
2.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C8(H8), C13(H13), C28(H28), C33(H33)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C34(H34A,H34B)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4A), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
 C25(H25), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              90463
_shelx_hkl_checksum              82398
_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 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.566