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_7712417
_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             2022-06-29
_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                64.867(6)
_cell_angle_beta                 75.150(6)
_cell_angle_gamma                78.068(5)
_cell_formula_units_Z            1
_cell_length_a                   8.1202(5)
_cell_length_b                   10.6670(5)
_cell_length_c                   12.4761(8)
_cell_measurement_reflns_used    25493
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      66.8650
_cell_measurement_theta_min      5.6320
_cell_volume                     939.73(11)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     14.00  89.00   1.00    1.00    --    0.00  30.00 -90.00   75
  2  \w    -77.00  -5.00   1.00    1.00    --    0.00  30.00 -90.00   72
  3  \w   -175.00-137.00   1.00    1.00    --  -87.00  12.00-150.17   38
  4  \w   -160.00-133.00   1.00    1.00    --  -87.00  60.00  -9.76   27
  5  \w   -111.00 -76.00   1.00    1.00    --  -87.00  60.00  -9.76   35
  6  \w    -46.00 -19.00   1.00    1.00    --  -87.00  60.00  -9.76   27
  7  \w   -159.00 -88.00   1.00    1.00    --  -87.00  60.00 109.71   71
  8  \w   -141.00 -75.00   1.00    1.00    --  -87.00  50.00  30.00   66
  9  \w   -153.00-103.00   1.00    1.00    --  -87.00  40.00  90.00   50
 10  \w    -75.00 -30.00   1.00    1.00    --  -87.00  40.00  90.00   45
 11  \w   -176.00-121.00   1.00    1.00    --  -87.00  60.00  71.73   55
 12  \w    -58.00   1.00   1.00    1.00    --  -87.00  60.00  71.73   59
 13  \w   -175.00-137.00   1.00    1.00    --  -87.00  60.00 -34.01   38
 14  \w   -122.00 -46.00   1.00    1.00    --  -87.00  60.00 -34.01   76
 15  \w   -174.00 -67.00   1.00    1.00    --  -87.00  30.00-120.00  107
 16  \w   -113.00  -1.00   1.00    1.00    --  -87.00  12.00-150.17  112
 17  \w    -46.00 -19.00   1.00    1.00    --  -87.00  60.00-106.92   27
 18  \w   -173.00-119.00   1.00    1.00    --  -87.00  60.00-161.23   54
 19  \w   -161.00 -76.00   1.00    1.00    --  -87.00  60.00-106.92   85
 20  \w   -164.00-138.00   1.00    1.00    --  -87.00  27.00-153.00   26
 21  \w    -71.00 -45.00   1.00    1.00    --  -87.00  10.00 -60.00   26
 22  \w   -162.00-136.00   1.00    1.00    --  -87.00  40.00 -30.00   26
 23  \w   -163.00-137.00   1.00    1.00    --  -87.00  10.00 -60.00   26
 24  \w    -84.00 -59.00   1.00    1.00    --    5.00  50.00  60.00   25
 25  \w   -111.00 -85.00   1.00    1.00    --  -87.00  40.00 -60.00   26
 26  \w   -117.00 -91.00   1.00    1.00    --  -87.00  58.00 149.86   26
 27  \w    -39.00   0.00   1.00    1.00    --  -87.00  30.00 150.00   39
 28  \w   -156.00-130.00   1.00    1.00    --  -87.00  40.00-180.00   26
 29  \w   -171.00-145.00   1.00    1.00    --  -87.00  58.00 149.86   26
 30  \w   -102.00 -76.00   1.00    1.00    --  -87.00  30.00 150.00   26
 31  \w    -40.00 -14.00   1.00    1.00    --  -87.00  58.00 149.86   26
 32  \w    -81.00 -55.00   1.00    1.00    --  -87.00  50.00 -90.00   26
 33  \w    -29.00  -3.00   1.00    1.00    --  -87.00  50.00 -90.00   26
 34  \w    -59.00 -33.00   1.00    1.00    --  -87.00  42.00 120.95   26
 35  \w   -143.00-117.00   1.00    1.00    --  -87.00  50.00   0.00   26
 36  \w   -158.00-117.00   1.00    1.00    --  -87.00  42.00 120.95   41
 37  \w    -89.00  89.00   1.00    1.00    --    0.00  10.00 120.00  178
 38  \w    -89.00  89.00   1.00    1.00    --    0.00  20.00-120.00  178
 39  \w    -89.00  89.00   1.00    1.00    --    0.00  50.00-180.00  178
 40  \w   -176.00 -22.00   1.00    1.00    --  -87.00  58.00 140.53  154
 41  \w   -176.00   2.00   1.00    1.00    --  -87.00   0.00  30.00  178
 42  \w     13.00  59.00   1.00    1.00    --  -30.00  53.00-119.47   46
 43  \w   -110.00 -84.00   1.00    1.00    --  -30.00  53.00-119.47   26
 44  \w      3.00  43.00   1.00    1.00    --  -46.00  56.00 179.68   40
 45  \w     10.00  35.00   1.00    1.00    --  -54.00  60.00  33.46   25
 46  \w   -110.00 -84.00   1.00    1.00    --  -58.00  58.00  58.43   26
 47  \w      0.00  29.00   1.00    1.00    --  -58.00  49.00 -29.09   29
 48  \w      6.00  31.00   1.00    1.00    --  -58.00  58.00  58.43   25
 49  \w     -3.00  23.00   1.00    1.00    --  -66.00  45.00 126.07   26
 50  \w    -11.00  15.00   1.00    1.00    --  -74.00  60.00-164.07   26
 51  \w    -10.00  15.00   1.00    1.00    --  -74.00  60.00 102.72   25
 52  \w    -12.00  14.00   1.00    1.00    --  -74.00  53.00 -73.55   26
 53  \w    -11.00  15.00   1.00    1.00    --  -74.00  58.00  26.08   26
 54  \w    -15.00  11.00   1.00    1.00    --  -78.00  57.00 -77.01   26
 55  \w    -16.00  10.00   1.00    1.00    --  -78.00  55.00 136.76   26
 56  \w    -20.00   6.00   1.00    1.00    --  -82.00  54.00-132.78   26
 57  \w    -24.00   2.00   1.00    1.00    --  -87.00  50.00-120.00   26
 58  \w   -134.00-108.00   1.00    1.00    --  -87.00  50.00-120.00   26
 59  \w    -56.00 -10.00   1.00    1.00    --  -87.00  30.00 -90.00   46
 60  \w    -43.00   2.00   1.00    1.00    --  -87.00  54.00 -95.65   45
 61  \w   -172.00-146.00   1.00    1.00    --  -87.00  50.00   0.00   26
 62  \w    -42.00   0.00   1.00    1.00    --  -87.00  50.00 -30.00   42
 63  \w    -27.00   1.00   1.00    1.00    --  -87.00  50.00-180.00   28
 64  \w    -96.00 -70.00   1.00    1.00    --  -87.00  26.00 106.66   26
 65  \w   -158.00-115.00   1.00    1.00    --  -87.00  26.00 106.66   43
 66  \w    -38.00  -5.00   1.00    1.00    --  -87.00  50.00   0.00   33
 67  \w    -28.00   1.00   1.00    1.00    --  -87.00  50.00 120.00   29
 68  \w    -35.00   2.00   1.00    1.00    --  -87.00  53.00 -53.72   37
 69  \w   -119.00 -94.00   1.00    1.00    --  -87.00  53.00 -53.72   25
 70  \w   -109.00 -83.00   1.00    1.00    --  -87.00  50.00  90.00   26
 71  \w   -147.00-103.00   1.00    1.00    --  -87.00  20.00 -30.00   44
 72  \w    -41.00   2.00   1.00    1.00    --  -87.00  60.00  25.99   43
 73  \w    -27.00  -1.00   1.00    1.00    --  -87.00  50.00 150.00   26
 74  \w    -74.00 -48.00   1.00    1.00    --  -87.00  50.00 150.00   26
 75  \w   -138.00-112.00   1.00    1.00    --  -87.00  60.00  25.99   26
 76  \w    -37.00   0.00   1.00    1.00    --  -87.00  50.00-150.00   37
 77  \w    -28.00  -2.00   1.00    1.00    --  -87.00  50.00  90.00   26
 78  \w    -42.00 -10.00   1.00    1.00    --  -87.00  20.00 -30.00   32
 79  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00   0.00  178
 80  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00 -30.00  178
 81  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00-180.00  178
 82  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00-150.00  178
 83  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00-120.00  178
 84  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00 -90.00  178
 85  \w    -89.00  89.00   1.00    1.00    --    0.00   0.00 -60.00  178
 86  \w   -107.00  71.00   1.00    1.00    --  -18.00  55.00 179.70  178
 87  \w   -119.00  59.00   1.00    1.00    --  -30.00  53.00-119.47  178
 88  \w   -131.00  47.00   1.00    1.00    --  -42.00  54.00 171.20  178
 89  \w     21.00  47.00   1.00    1.00    --  -42.00  57.00-142.70   26
 90  \w     -3.00  23.00   1.00    1.00    --  -66.00  56.00  95.62   26
;
_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      -0.1220360000
_diffrn_orient_matrix_UB_12      0.0437942000
_diffrn_orient_matrix_UB_13      0.0982055000
_diffrn_orient_matrix_UB_21      0.1287029000
_diffrn_orient_matrix_UB_22      -0.0765402000
_diffrn_orient_matrix_UB_23      0.0853615000
_diffrn_orient_matrix_UB_31      0.0868047000
_diffrn_orient_matrix_UB_32      0.1340184000
_diffrn_orient_matrix_UB_33      -0.0486109000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_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            31560
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.060
_diffrn_reflns_theta_max         67.060
_diffrn_reflns_theta_min         5.672
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62914
_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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 2832 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         6398
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0736P)^2^+0.1307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                6201
_reflns_number_total             6398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04082d2.cif
_cod_data_source_block           2RR
_cod_database_code               7712417
_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 98.84
_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:
 C3(H3A), C4(H4A), C5(H5), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
 C25(H25), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              48355
_shelx_hkl_checksum              79404
_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 2.387
_oxdiff_exptl_absorpt_empirical_full_min 0.559