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_7038354
_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         'C36 H18 Br12 F12 N6 O2 Zn2, 2(C6 H6)'
_chemical_formula_sum            'C48 H30 Br12 F12 N6 O2 Zn2'
_chemical_formula_weight         2040.44
_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                67.401(3)
_cell_angle_beta                 89.479(4)
_cell_angle_gamma                63.532(3)
_cell_formula_units_Z            1
_cell_length_a                   11.462(2)
_cell_length_b                   11.6254(19)
_cell_length_c                   14.089(2)
_cell_measurement_reflns_used    7601
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.81
_cell_measurement_theta_min      2.97
_cell_volume                     1521.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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      100.01
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13064
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         3.002
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.748
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5420
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1109 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.5420.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_description       platy
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.990
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6386
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0970P)^2^+5.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4815
_reflns_number_total             6386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00257a2.cif
_cod_data_source_block           rad156_0m_a
_cod_depositor_comments
'Adding full bibliography for 7038353--7038356.cif.'
_cod_database_code               7038354
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.089
_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(C20) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C13(H13), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'