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_7109994
_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         'C52 H46 O4 Zn3'
_chemical_formula_sum            'C52 H46 O4 Zn3'
_chemical_formula_weight         931.00
_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                78.61(2)
_cell_angle_beta                 77.69(2)
_cell_angle_gamma                83.52(3)
_cell_formula_units_Z            2
_cell_length_a                   10.018(2)
_cell_length_b                   14.641(4)
_cell_length_c                   15.057(5)
_cell_measurement_reflns_used    11073
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.7954
_cell_measurement_theta_min      2.8021
_cell_volume                     2109.4(10)
_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 0.891
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25290
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                7540
_reflns_number_total             10950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46206d.txt
_cod_data_source_block           rp17
_cod_database_code               7109994