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_7717815
_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         'C27 H30 N2 O Zn'
_chemical_formula_sum            'C27 H30 N2 O Zn'
_chemical_formula_weight         463.90
_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                 104.812(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0642(4)
_cell_length_b                   10.5511(3)
_cell_length_c                   19.4179(7)
_cell_measurement_reflns_used    10957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9380
_cell_measurement_theta_min      2.1630
_cell_volume                     2389.58(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 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    7.00    --   24.18 -19.00 -90.00  114
  2  \w    -23.00  36.00   0.50    7.00    --  -23.24 -99.00 -30.00  118
  3  \w     31.00  66.00   0.50    7.00    --   24.18-131.00  -7.00   70
  4  \w    -13.00  35.00   0.50    7.00    --  -23.24 -99.00  90.00   96
  5  \w     36.00  62.00   0.50    7.00    --   24.18-138.00 176.00   52
  6  \w    -65.00   5.00   0.50    7.00    --   24.18 -19.00  30.00  140
  7  \w    -61.00 -14.00   0.50    7.00    --   24.18 -19.00 -30.00   94
  8  \w     10.00  66.00   0.50    7.00    --   24.18  57.00-120.00  112
  9  \w     81.00 107.00   0.50    7.00    --   24.18  57.00-120.00   52
 10  \w     82.00 107.00   0.50    7.00    --   24.18 178.00  60.00   50
 11  \w    -57.00  -1.00   0.50    7.00    --   24.18 -19.00-120.00  112
 12  \w    -72.00   5.00   0.50    7.00    --   24.18 -19.00-180.00  154
 13  \w    -86.00 -61.00   0.50    7.00    --  -23.24 138.00-120.00   50
 14  \w    -92.00 -22.00   0.50    7.00    --  -23.24 131.00  63.00  140
 15  \w    -72.00  -9.00   0.50    7.00    --   24.18 -19.00 120.00  126
;
_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      -0.0135964000
_diffrn_orient_matrix_UB_12      0.0006773000
_diffrn_orient_matrix_UB_13      0.0334518000
_diffrn_orient_matrix_UB_21      0.0592224000
_diffrn_orient_matrix_UB_22      0.0025116000
_diffrn_orient_matrix_UB_23      0.0175496000
_diffrn_orient_matrix_UB_31      -0.0020260000
_diffrn_orient_matrix_UB_32      0.0671795000
_diffrn_orient_matrix_UB_33      -0.0009889000
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0546
_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       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30900
_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         29.698
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50495
_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    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0521P)^2^+0.2119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3908
_reflns_number_total             6140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03395g2.cif
_cod_data_source_block           d33-c4
_cod_depositor_comments
'Adding full bibliography for 7717814--7717818.cif.'
_cod_database_code               7717815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONZn
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.885
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Restrained distances
 C26-C25 \\sim C25'-C26
 with sigma of 0.02
 C25-C24 \\sim C25'-C24
 with sigma of 0.02
2. Others
 Sof(H24C)=Sof(H24D)=Sof(H26C)=Sof(H26D)=Sof(C25')=Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(H26A)=Sof(H26B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C24(H24A,H24B), C24(H24C,H24D), C22(H22A,H22B), C26(H26A,
 H26B), C26(H26C,H26D), C25(H25A,H25B), C25'(H25C,H25D)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C2(H2), C5(H5), C18(H18), C11(H11), C8(H8), C3(H3), C4(H4),
 C21(H21), C10(H10), C9(H9), C19(H19), C20(H20)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              51398
_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 4.128
_oxdiff_exptl_absorpt_empirical_full_min 0.384