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_7717814
_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 H23 N O Zn'
_chemical_formula_sum            'C28 H23 N O Zn'
_chemical_formula_weight         454.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-16
_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                 102.832(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6892(7)
_cell_length_b                   21.3643(9)
_cell_length_c                   10.0608(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    300
_cell_measurement_theta_max      28.8910
_cell_measurement_theta_min      2.1650
_cell_volume                     2240.2(2)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300
_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 0.883
_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    -49.00 -11.00   0.50   10.00    --  -23.24 -19.00 -90.00   76
  2  \w    -23.00  36.00   0.50   10.00    --  -23.24 -99.00-120.00  118
  3  \w     31.00  56.00   0.50   10.00    --   24.18-125.00 -95.00   50
  4  \w     41.00  66.00   0.50   10.00    --   24.18-145.00  98.00   50
  5  \w    -67.00 -42.00   0.50   10.00    --   24.18 -19.00  30.00   50
  6  \w    -61.00   4.00   0.50   10.00    --   24.18 -19.00   0.00  130
  7  \w    -72.00   5.00   0.50   10.00    --   24.18 -19.00 -60.00  154
  8  \w    -83.00 -49.00   0.50   10.00    --  -23.24 125.00 -16.00   68
  9  \w    -69.00   5.00   0.50   10.00    --   24.18 -19.00 150.00  148
 10  \w   -106.00 -81.00   0.50   10.00    --  -23.24-145.00  98.00   50
;
_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      -0.0564067000
_diffrn_orient_matrix_UB_12      -0.0184155000
_diffrn_orient_matrix_UB_13      -0.0183600000
_diffrn_orient_matrix_UB_21      -0.0379787000
_diffrn_orient_matrix_UB_22      0.0275287000
_diffrn_orient_matrix_UB_23      -0.0060619000
_diffrn_orient_matrix_UB_31      0.0025308000
_diffrn_orient_matrix_UB_32      0.0024664000
_diffrn_orient_matrix_UB_33      -0.0696471000
_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  0.1045
_diffrn_reflns_av_unetI/netI     0.1208
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16236
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_min         1.906
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.745
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.1070
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2852
_refine_ls_wR_factor_ref         0.3244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3237
_reflns_number_total             5565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03395g2.cif
_cod_data_source_block           d25
_cod_depositor_comments
'Adding full bibliography for 7717814--7717818.cif.'
_cod_database_code               7717814
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         CHONZn
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B)
1.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C16(H16), C24(H24), C2(H2), C17(H17), C25(H25), C5(H5),
 C23(H23), C22(H22), C12(H12), C8(H8), C4(H4), C18(H18), C19(H19), C9(H9),
 C11(H11), C10(H10)
1.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
;
_shelx_res_checksum              22541
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.886
_oxdiff_exptl_absorpt_empirical_full_min 0.306