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_7717818
_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         'C29 H28 N2 O Zn'
_chemical_formula_sum            'C29 H28 N2 O Zn'
_chemical_formula_weight         485.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 101.383(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0635(4)
_cell_length_b                   10.6401(4)
_cell_length_c                   19.2513(8)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2010
_cell_measurement_theta_min      2.1350
_cell_volume                     2422.43(16)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.905
_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    -52.00   5.00   0.50   16.00    --   24.18 -19.00 -30.00  114
  2  \w    -59.00  -1.00   0.50   16.00    --   24.18 -19.00 -90.00  116
  3  \w    -20.00   5.00   0.50   16.00    --   24.18 -19.00-180.00   50
  4  \w    -14.00  12.00   0.50   16.00    --   24.18 -37.00-180.00   52
  5  \w     37.00 104.00   0.50   16.00    --   24.18-136.00 -32.00  134
  6  \w     48.00  74.00   0.50   16.00    --   24.18-132.00 144.00   52
  7  \w    -64.00  21.00   0.50   16.00    --   24.18 -37.00 -30.00  170
  8  \w    -72.00 -27.00   0.50   16.00    --   24.18 -19.00-120.00   90
  9  \w   -113.00  21.00   0.50   16.00    --  -23.24 -37.00  60.00  268
 10  \w   -101.00 -25.00   0.50   16.00    --  -23.24 132.00-145.00  152
 11  \w    -66.00 -41.00   0.50   16.00    --  -23.24 136.00  31.00   50
 12  \w     43.00  81.00   0.50   16.00    --   24.18 178.00 120.00   76
 13  \w     47.00  92.00   0.50   16.00    --   24.18 178.00 -90.00   90
 14  \w     55.00  80.00   0.50   16.00    --   24.18 178.00-120.00   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      -0.0112337000
_diffrn_orient_matrix_UB_12      0.0008609000
_diffrn_orient_matrix_UB_13      -0.0375619000
_diffrn_orient_matrix_UB_21      0.0587538000
_diffrn_orient_matrix_UB_22      0.0054489000
_diffrn_orient_matrix_UB_23      0.0004432000
_diffrn_orient_matrix_UB_31      0.0046716000
_diffrn_orient_matrix_UB_32      -0.0664438000
_diffrn_orient_matrix_UB_33      -0.0004446000
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31471
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.651
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49347
_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    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0637P)^2^+1.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3990
_reflns_number_total             6199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03395g2.cif
_cod_data_source_block           l12-c4
_cod_depositor_comments
'Adding full bibliography for 7717814--7717818.cif.'
_cod_database_code               7717818
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNZn
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.868
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C26(H26A,H26B), C28(H28A,H28B), C24(H24A,H24B), C27(H27A,H27B)
1.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C11(H11), C5(H5), C2(H2), C18(H18), C17(H17), C8(H8),
 C23(H23), C10(H10), C3(H3), C9(H9), C21(H21), C4(H4), C22(H22)
1.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              63892
_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 2.106
_oxdiff_exptl_absorpt_empirical_full_min 0.464