Alkyl zinc complexes derived from formylfluorenimide ligands: synthesis, characterization and catalysis for hydroboration of aldehydes and ketones.
Wei, Biao; Qin, Zhibiao; Miao, Hui; Wang, Chaoqun; Huang, Mengna; Liu, Chenxu; Bai, Cuibing; Chen, Zheng; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3427–3436; doi:10.1039/d4dt03395g

data_7717816
_publ_section_title
;
 Alkyl zinc complexes derived from formylfluorenimide ligands: synthesis,
 characterization and catalysis for hydroboration of aldehydes and
 ketones.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3427
_journal_page_last               3436
_journal_paper_doi               10.1039/d4dt03395g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H38 N2 O Zn, 0.5[C6H14]'
_chemical_formula_sum            'C28 H38 N2 O Zn'
_chemical_formula_weight         483.97
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.7896(19)
_cell_length_b                   28.7896(19)
_cell_length_c                   19.0194(9)
_cell_measurement_reflns_used    5498
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      25.9230
_cell_measurement_theta_min      2.2870
_cell_volume                     13652.1(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.861
_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    -70.00  48.00   0.50   75.00    --  -23.24   0.00 139.00  236
  2  \w    -53.00 -28.00   0.50   75.00    --  -23.24 134.00 -31.00   50
  3  \w    -88.00 -62.00   0.50   75.00    --  -23.24 134.00 -31.00   52
  4  \w     62.00 104.00   0.50   75.00    --   24.18-178.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0119564000
_diffrn_orient_matrix_UB_12      0.0283294000
_diffrn_orient_matrix_UB_13      -0.0000594000
_diffrn_orient_matrix_UB_21      -0.0258076000
_diffrn_orient_matrix_UB_22      -0.0025422000
_diffrn_orient_matrix_UB_23      -0.0001110000
_diffrn_orient_matrix_UB_31      -0.0000966000
_diffrn_orient_matrix_UB_32      -0.0000249000
_diffrn_orient_matrix_UB_33      0.0373038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17296
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.582
_diffrn_reflns_theta_min         1.953
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             4644
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7338
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0586P)^2^+3.3013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4307
_reflns_number_total             7338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03395g2.cif
_cod_data_source_block           d31---c4
_cod_depositor_comments
'Adding full bibliography for 7717814--7717818.cif.'
_cod_original_cell_volume        13652.1(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7717816
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         CHNOZn
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.886
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Restrained distances
 C27-C26
 1.54 with sigma of 0.01
 C24'-C23 = C24-C23
 1.54 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C24': within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3. Others
 Sof(H23C)=Sof(H23D)=Sof(C24')=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
4.a Riding coordinates:
 C24(H24A,H24B,H24C), C24'(H24D,H24E,H24F)
4.b Ternary CH refined with riding coordinates:
 C15(H15), C20(H20)
4.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B), C28(H28A,
 H28B), C27(H27A,H27B), C23(H23A,H23B), C23(H23C,H23D), C26(H26A,H26B),
 C25(H25A,H25B)
4.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C11(H11), C8(H8), C2(H2), C5(H5), C4(H4), C9(H9), C3(H3), C10(H10)
4.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 423 electrons were 
found in a volume of 2853\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C6H14] per Asymmetric Unit 
which account for 450 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48257
_shelx_fab_checksum              75267
_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 4.548
_oxdiff_exptl_absorpt_empirical_full_min 0.536