Probing secondary coordination sphere influence on the oxygenation of zinc alkyls: formation of a unique zinc peroxide species
Piotr Sobota; Rafal Petrus; Karolina Zelga; Lukasz Makolski; Dominik Kubicki; Janusz Lewinski; Chem.Commun. 49 (2013) 10477–; doi:10.1039/c3cc46206d

data_7109995
_publ_section_title
;
 Probing secondary coordination sphere influence on the oxygenation of
 zinc alkyls: formation of a unique zinc peroxide species
;
_journal_name_full               Chem.Commun.
_journal_page_first              10477
_journal_paper_doi               10.1039/c3cc46206d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C96 H78 O16 Zn8, 2(C12 H10 O),  2.42(C H2 Cl2)'
_chemical_formula_sum            'C122.42 H102.84 Cl4.84 O18 Zn8'
_chemical_formula_weight         2556.32
_chemical_name_systematic
;
 ?
;
_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                91.26(2)
_cell_angle_beta                 91.15(3)
_cell_angle_gamma                94.10(3)
_cell_formula_units_Z            6
_cell_length_a                   17.903(3)
_cell_length_b                   22.986(4)
_cell_length_c                   39.788(5)
_cell_measurement_reflns_used    55866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.5500
_cell_measurement_theta_min      2.9050
_cell_volume                     16324(4)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'KUMA KM4 CCD \k-geometry diffractometer'
_diffrn_measurement_method       \w
_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  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            261959
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7821.5
_exptl_crystal_size_max          0.5440
_exptl_crystal_size_mid          0.3578
_exptl_crystal_size_min          0.1457
_refine_diff_density_max         2.653
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4255
_refine_ls_number_reflns         91751
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1858
_reflns_number_gt                45332
_reflns_number_total             91751
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cc46206d.txt
_cod_data_source_block           rp12abs
_cod_database_code               7109995