Fluorinated triazapentadienyl ligand supported ethyl zinc(ii) complexes: reaction with dioxygen and catalytic applications in the Tishchenko reaction.
Kulkarni, Naveen V.; Das, Animesh; Ridlen, Shawn G.; Maxfield, Erin; Adiraju, Venkata A. K.; Yousufuddin, Muhammed; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4896–4906; doi:10.1039/c6dt00257a

data_7038355
_publ_section_title
;
 Fluorinated triazapentadienyl ligand supported ethyl zinc(ii) complexes:
 reaction with dioxygen and catalytic applications in the Tishchenko
 reaction.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4896
_journal_page_last               4906
_journal_paper_doi               10.1039/c6dt00257a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C22 H11 Cl4 F14 N3 O Zn, C6 H6'
_chemical_formula_sum            'C28 H17 Cl4 F14 N3 O Zn'
_chemical_formula_weight         884.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-09 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.972(2)
_cell_angle_beta                 79.294(2)
_cell_angle_gamma                87.809(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3583(10)
_cell_length_b                   12.0545(11)
_cell_length_c                   12.6061(11)
_cell_measurement_reflns_used    7498
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      31.88
_cell_measurement_theta_min      3.14
_cell_volume                     1694.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      101.58
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16822
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.139
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0734 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.7407.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       platy
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.361
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.415
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0898P)^2^+2.5736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5168
_reflns_number_total             6634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00257a2.cif
_cod_data_source_block           rad205_0m_a
_cod_depositor_comments
'Adding full bibliography for 7038353--7038356.cif.'
_cod_database_code               7038355
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
3. Rigid body (RIGU) restrains
 C34, C33, C32, C31, C30, C29, C25, C24, C23, C28, C27, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5)
 H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C34(0.5)
 H34(0.5) C33(0.5) H33(0.5) C32(0.5) H32(0.5) C31(0.5) H31(0.5) C30(0.5)
 H30(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C33(H33), C32(H32),
  C31(H31), C30(H30)
5.c Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C28), C29(C34,C33,C32,C31,C30)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'