Oxygenation of alkylzinc complexes with pyrrolylketiminate ligand: access to alkylperoxide versus oxo-encapsulated complexes.
Lewiński, Janusz; Suwała, Karolina; Kaczorowski, Tomasz; Gałezowski, Michał; Gryko, Daniel T; Justyniak, Iwona; Lipkowski, Janusz; Chemical communications (Cambridge, England) 34 (2008) 215–217; doi:10.1039/b813315h

data_7104116
_publ_section_title
;
 Oxygenation of alkylzinc complexes with pyrrolylketiminate ligand:
 access to alkylperoxide versus oxo-encapsulated complexes.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              215
_journal_page_last               217
_journal_paper_doi               10.1039/b813315h
_journal_volume                  34
_journal_year                    2008
_chemical_formula_sum            'C47 H62 N8 O4 Zn3'
_chemical_formula_weight         999.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.2702(10)
_cell_angle_beta                 98.1488(10)
_cell_angle_gamma                94.0181(10)
_cell_formula_units_Z            4
_cell_length_a                   14.6481(3)
_cell_length_b                   18.5359(3)
_cell_length_c                   18.7841(4)
_cell_measurement_reflns_used    27823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      0.998
_cell_volume                     5029.93(17)
_computing_cell_refinement       'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_molecular_graphics
;
DIAMOND v2.1 (Brandenburg, 1999)
Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565,
ORTEP III (Burnett, Johnson, 1996)
;
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997),

;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
226 frames, \w rotation 1.6\% per frame (50s per frame)
34 frames, \w rotation 1.6\% per frame (50s per frame)
16 frames, \w rotation 1.6\% per frame (50s per frame)
21 frames, \w rotation 1.6\% per frame (50s per frame)
35 frames, \w rotation 1.6\% per frame (50s per frame)
52 frames, \w rotation 1.6\% per frame (50s per frame)
;
_diffrn_measurement_device       '\k-geometry diffractometr'
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25362
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1130
_refine_ls_number_reflns         13525
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+22.8437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                10061
_reflns_number_total             13525
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b813315h.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               7104116