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_7717817
_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         'C52 H54 N4 O2 Zn2'
_chemical_formula_sum            'C52 H54 N4 O2 Zn2'
_chemical_formula_weight         897.73
_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   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                101.392(7)
_cell_angle_beta                 92.843(5)
_cell_angle_gamma                116.235(6)
_cell_formula_units_Z            1
_cell_length_a                   8.5422(4)
_cell_length_b                   9.1132(6)
_cell_length_c                   16.3399(12)
_cell_measurement_reflns_used    3294
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      28.8700
_cell_measurement_theta_min      2.5620
_cell_volume                     1104.86(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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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    -51.00   5.00   0.50   19.31    --   24.18 -19.00-120.00  112
  2  \w    -22.00  34.00   0.50   19.31    --  -23.24 -99.00 -90.00  112
  3  \w     20.00  70.00   0.50   19.31    --   24.18-131.00 -50.00  100
  4  \w     20.00 104.00   0.50   19.31    --   24.18-137.00 133.00  168
  5  \w    -18.00  36.00   0.50   19.31    --  -23.24 -99.00  90.00  108
  6  \w    -58.00   4.00   0.50   19.31    --   24.18 -19.00 120.00  124
  7  \w    -48.00 -22.00   0.50   19.31    --  -23.24 131.00  20.00   52
  8  \w    -67.00 -42.00   0.50   19.31    --  -23.24 137.00-163.00   50
  9  \w    -52.00  21.00   0.50   19.31    --   24.18 -37.00-180.00  146
 10  \w    -72.00  -1.00   0.50   19.31    --   24.18 -19.00-150.00  142
 11  \w   -111.00   5.00   0.50   19.31    --  -23.24 -19.00 -90.00  232
;
_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      0.0166695000
_diffrn_orient_matrix_UB_12      0.0424367000
_diffrn_orient_matrix_UB_13      0.0432727000
_diffrn_orient_matrix_UB_21      0.0149829000
_diffrn_orient_matrix_UB_22      0.0755684000
_diffrn_orient_matrix_UB_23      -0.0116449000
_diffrn_orient_matrix_UB_31      -0.0909935000
_diffrn_orient_matrix_UB_32      -0.0223199000
_diffrn_orient_matrix_UB_33      -0.0011779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1515
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3824
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.570
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53286
_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    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0849
_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^)+(0.1458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2817
_reflns_number_total             3824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03395g2.cif
_cod_data_source_block           l10-c4_tw
_cod_depositor_comments
'Adding full bibliography for 7717814--7717818.cif.'
_cod_original_cell_volume        1104.86(13)
_cod_database_code               7717817
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         CHNOZn
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80039
 0.19961
2.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C26(H26A,H26B), C24(H24A,H24B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C19(H19), C10(H10), C4(H4), C3(H3), C13(H13), C16(H16),
 C18(H18), C12(H12), C17(H17), C2(H2), C11(H11)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              17600
_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 5.052
_oxdiff_exptl_absorpt_empirical_full_min 0.234