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_7712419
_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         '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           2
_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             2022-08-01
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                64.938(4)
_cell_angle_beta                 75.120(3)
_cell_angle_gamma                78.039(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1340(3)
_cell_length_b                   10.6803(4)
_cell_length_c                   12.4823(5)
_cell_measurement_reflns_used    10164
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.7840
_cell_measurement_theta_min      3.9700
_cell_volume                     943.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9887
_diffrn_measured_fraction_theta_max 0.8173
_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    -89.00  89.00   1.00    3.00    --    0.00  13.00-120.00  178
  2  \w   -176.00   2.00   1.00   12.50    --  -87.00  13.00-120.00  178
  3  \w    -89.00  89.00   1.00    3.00    --    0.00  20.00  60.00  178
  4  \w    -84.00  94.00   1.00   12.50    --    5.00  13.00-120.00  178
  5  \w   -176.00   2.00   1.00   12.50    --  -87.00  60.00 -81.62  178
  6  \w   -176.00   2.00   1.00   12.50    --  -87.00  60.00 157.39  178
  7  \w   -176.00 -10.00   1.00   12.50    --  -87.00  59.00 -17.24  166
  8  \w   -175.00   1.00   1.00   12.50    --  -87.00  60.00-148.82  176
  9  \w   -163.00-133.00   1.00   12.50    --  -87.00  10.00  30.00   30
 10  \w    -34.00  -7.00   1.00   12.50    --  -87.00  10.00  30.00   27
 11  \w   -156.00-129.00   1.00   12.50    --  -87.00  55.00  28.28   27
 12  \w   -122.00 -92.00   1.00   12.50    --  -87.00  55.00  28.28   30
 13  \w    -50.00 -23.00   1.00   12.50    --  -87.00  55.00  28.28   27
 14  \w   -106.00 -81.00   1.00   12.50    --  -87.00  50.00 120.00   25
 15  \w   -173.00-146.00   1.00   12.50    --  -87.00  60.00 123.26   27
 16  \w   -129.00-104.00   1.00   12.50    --  -87.00  60.00  46.91   25
 17  \w    -45.00 -18.00   1.00   12.50    --  -87.00  60.00 123.26   27
 18  \w   -108.00 -30.00   1.00   12.50    --  -87.00  40.00  90.00   78
 19  \w   -131.00-104.00   1.00   12.50    --  -87.00  40.00 -30.00   27
 20  \w    -56.00 -29.00   1.00   12.50    --  -87.00  20.00-150.00   27
 21  \w   -165.00-138.00   1.00   12.50    --  -87.00  60.00   6.70   27
 22  \w    -33.00  -6.00   1.00   12.50    --  -87.00  60.00   6.70   27
 23  \w   -170.00 -23.00   1.00   12.50    --  -87.00  60.00 -46.19  147
 24  \w   -150.00-123.00   1.00   12.50    --  -87.00  10.00 -90.00   27
 25  \w   -109.00 -82.00   1.00   12.50    --  -87.00  30.00 150.00   27
 26  \w   -172.00 -22.00   1.00   12.50    --  -87.00  40.00-180.00  150
 27  \w   -171.00-144.00   1.00   12.50    --  -87.00  50.00-120.00   27
 28  \w   -154.00-127.00   1.00   12.50    --  -87.00  50.00 120.00   27
 29  \w   -175.00-134.00   1.00   12.50    --  -87.00  60.00  46.91   41
 30  \w   -146.00-119.00   1.00   12.50    --  -87.00  57.00 -72.96   27
 31  \w   -175.00 -84.00   1.00   12.50    --  -87.00  60.00  91.11   91
;
_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      -0.0060030000
_diffrn_orient_matrix_UB_12      -0.1542174000
_diffrn_orient_matrix_UB_13      0.0281071000
_diffrn_orient_matrix_UB_21      0.1966354000
_diffrn_orient_matrix_UB_22      -0.0253008000
_diffrn_orient_matrix_UB_23      -0.0161176000
_diffrn_orient_matrix_UB_31      -0.0139486000
_diffrn_orient_matrix_UB_32      -0.0354654000
_diffrn_orient_matrix_UB_33      0.1349608000
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0305
_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            17027
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.013
_diffrn_reflns_theta_max         67.013
_diffrn_reflns_theta_min         3.983
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.196
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (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    1.562
_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         0.604
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0637
_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^)+6.2839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3192
_reflns_number_total             3328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04082d2.cif
_cod_data_source_block           2RS
_cod_database_code               7712419
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Zn C H F N'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.917
_diffrn_oxdiff_digest_frames
;
013b865554c1889a2fccad4240c3be6d370002598d8
;
_diffrn_oxdiff_digest_hkl
;
015d5289a4ac906959b5e46184e77cce9091af
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H8A(0.5) H8B(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 H10D(0.5) H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) C21(0.5) H21(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C13(0.5) H13(0.5)
3.a Free rotating group:
 O3(H3A,H3B)
3.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2A), N2(H2B), C8(H8A), C8(H8B), C21(H21), C13(H13)
3.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C10(H10C,H10D), C12(H12A,H12B),
 C12(H12C,H12D), C14(H14A,H14B), C22(H22A,H22B), C11(H11A,H11B)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              52181
_shelx_hkl_checksum              24480
_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 1.681
_oxdiff_exptl_absorpt_empirical_full_min 0.550