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_7712418
_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 ad
_chemical_formula_moiety         'C44 H44 F12 N4 O8 Zn2, 2(C H4 O), 0.75(H2 O)'
_chemical_formula_sum            'C46 H53.5 F12 N4 O10.75 Zn2'
_chemical_formula_weight         1193.16
_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             2022-10-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                81.280(3)
_cell_angle_beta                 72.282(3)
_cell_angle_gamma                85.815(4)
_cell_formula_units_Z            1
_cell_length_a                   8.7181(3)
_cell_length_b                   11.4705(6)
_cell_length_c                   13.6295(4)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.1340
_cell_measurement_theta_min      3.4340
_cell_volume                     1282.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.928
_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   -120.00 -39.00   0.50    5.00    --  -45.09 -36.00  96.00  162
  2  \w    -20.00  30.00   0.50    5.00    --  -45.09  36.00-107.00  100
  3  \w     39.00 121.00   0.50    5.00    --   45.09  36.00-107.00  164
  4  \w    -30.00  12.00   0.50    5.00    --   45.09 -36.00  96.00   84
  5  \w   -172.00 -91.00   0.50   20.00    --  -97.00 -36.00  96.00  162
  6  \w    104.00 168.00   0.50   20.00    --  109.75  36.00-107.00  128
  7  \w    -65.00  18.00   0.50    5.00    --  -45.09  77.00   0.00  166
  8  \w    -90.00 -16.00   0.50    5.00    --  -45.09 125.00 -30.00  148
  9  \w   -119.00 -37.00   0.50    5.00    --  -45.09 -45.00 -99.03  164
 10  \w    -90.00 -16.00   0.50    5.00    --  -45.09 125.00-180.00  148
 11  \w    -62.00 -33.00   0.50    5.00    --  -45.09 -58.00 174.69   58
 12  \w    -23.00  30.00   0.50    5.00    --  -45.09  38.00  30.00  106
 13  \w    -93.00 -23.00   0.50   20.00    --  -97.00  93.00 121.42  140
 14  \w   -140.00 -90.00   0.50   20.00    --  -97.00 -15.00 -30.00  100
 15  \w    -93.00 -23.00   0.50   20.00    --  -97.00  97.00 -24.81  140
 16  \w    -55.00 -23.00   0.50   20.00    --  -97.00  61.00  90.00   64
 17  \w   -170.00 -94.00   0.50   20.00    --  -97.00-125.00-180.00  152
 18  \w   -140.00 -90.00   0.50   20.00    --  -97.00 -15.00   0.00  100
 19  \w    -97.00 -23.00   0.50   20.00    --  -97.00 115.00   8.40  148
 20  \w    -55.00 -23.00   0.50   20.00    --  -97.00  61.00-120.00   64
 21  \w    -97.00 -23.00   0.50   20.00    --  -97.00 117.00-113.95  148
 22  \w    -93.00 -23.00   0.50   20.00    --  -97.00  93.00  59.16  140
 23  \w    -79.00 -23.00   0.50   20.00    --  -97.00  77.00-120.00  112
 24  \w    -79.00 -23.00   0.50   20.00    --  -97.00  77.00  60.00  112
 25  \w   -170.00-106.00   0.50   20.00    --  -97.00 -77.00-120.00  128
 26  \w    -93.00 -23.00   0.50   20.00    --  -97.00  97.00-102.29  140
 27  \w    -55.00 -23.00   0.50   20.00    --  -97.00  61.00-150.00   64
 28  \w    102.00 175.00   0.50   20.00    --  109.75  45.00 120.00  146
 29  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00  90.00  112
 30  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00   0.00  112
 31  \w    104.00 132.00   0.50   20.00    --  109.75  15.00-180.00   56
 32  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00-150.00  112
 33  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00-180.00  112
 34  \w    104.00 132.00   0.50   20.00    --  109.75  15.00-150.00   56
 35  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00 150.00  112
 36  \w     37.00  93.00   0.50   20.00    --  109.75 -95.00 -30.00  112
 37  \w    104.00 132.00   0.50   20.00    --  109.75  15.00 -30.00   56
 38  \w     37.00 100.00   0.50   20.00    --  109.75-125.00-180.00  126
 39  \w    104.00 132.00   0.50   20.00    --  109.75  15.00 150.00   56
 40  \w    104.00 132.00   0.50   20.00    --  109.75  15.00-120.00   56
 41  \w     37.00  71.00   0.50   20.00    --  109.75 -77.00 120.00   68
 42  \w   -120.00 -39.00   0.50    5.00    --  -45.09 -38.00 -60.00  162
 43  \w   -118.00 -36.00   0.50    5.00    --  -45.09 -48.00-143.32  164
 44  \w    -62.00 -34.00   0.50    5.00    --  -45.09 -57.00  49.79   56
 45  \w   -120.00 -39.00   0.50    5.00    --  -45.09 -38.00   0.00  162
 46  \w     36.00 118.00   0.50    5.00    --   45.09  49.00 159.34  164
 47  \w     35.00 118.00   0.50    5.00    --   45.09  53.00  23.84  166
 48  \w     35.00 118.00   0.50    5.00    --   45.09  53.00  67.75  166
 49  \w     35.00  93.00   0.50    5.00    --   45.09  53.00 -31.63  116
 50  \w     36.00 118.00   0.50    5.00    --   45.09  52.00-177.10  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF diffractometer with HF Varimax confocal mirrors, an 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      0.1825787000
_diffrn_orient_matrix_UB_12      0.0031693000
_diffrn_orient_matrix_UB_13      -0.0553469000
_diffrn_orient_matrix_UB_21      0.0066883000
_diffrn_orient_matrix_UB_22      -0.1353607000
_diffrn_orient_matrix_UB_23      0.0056501000
_diffrn_orient_matrix_UB_31      -0.0325711000
_diffrn_orient_matrix_UB_32      0.0120428000
_diffrn_orient_matrix_UB_33      -0.1060706000
_diffrn_radiation_collimation    'HF 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  0.0651
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23112
_diffrn_reflns_point_group_measured_fraction_full 0.805
_diffrn_reflns_point_group_measured_fraction_max 0.734
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.187
_diffrn_reflns_theta_min         3.436
_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    2.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (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    1.545
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         7985
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.581
_reflns_Friedel_fraction_full    0.617
_reflns_Friedel_fraction_max     0.539
_reflns_number_gt                6460
_reflns_number_total             7985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04082d2.cif
_cod_data_source_block           1RR
_cod_original_formula_sum        'C46 H53.50 F12 N4 O10.75 Zn2'
_cod_database_code               7712418
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H22 F6 N2 O2 Zn'
_chemical_oxdiff_usercomment     NBE728
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H71B-O61A_$1
 1.9 with sigma of 0.0002
 H71A-O51
 2 with sigma of 0.0002
 O61A-C61A \\sim O61B-C61B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O61B) \\sim Ueq, Uanis(C61B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O61B, C61B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O71(0.75) H71A(0.75) H71B(0.75) O61A(0.75) H61A(0.75) C61A(0.75)
 H61B(0.75) H61C(0.75) H61D(0.75) O61B(0.25) H61E(0.25) C61B(0.25) H61F(0.25)
 H61G(0.25) H61H(0.25)
6.a Free rotating group:
 O71(H71A,H71B)
6.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C9(H9), C14(H14), C31(H31), C36(H36)
6.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C15(H15A,H15B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C37(H37A,H37B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C5(H5), C17(H17), C19(H19), C20(H20), C24(H24), C25(H25),
 C27(H27), C39(H39), C41(H41), C42(H42)
6.e Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C61A(H61B,H61C,H61D), C61B(H61F,H61G,H61H)
6.f Idealised tetrahedral OH refined as rotating group:
 O51(H51), O61A(H61A), O61B(H61E)
;
_shelx_res_checksum              64889
_shelx_hkl_checksum              77060
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 1.927
_oxdiff_exptl_absorpt_empirical_full_min 0.593