Reactions of Oxygen with Metallaheterocyclic Alkyl Amide Complexes. Selective Insertion of Oxygen into Metal−Carbon Bonds
Yu, Xianghua; Chen, Xue-Tai; Xue, Zi-Ling; Organometallics 28 (2009) 6642–; doi:10.1021/om900773w

data_4070385
_publ_section_title
;
 Reactions of Oxygen with Metallaheterocyclic Alkyl Amide Complexes.
 Selective Insertion of Oxygen into Metal&#x2212;Carbon Bonds
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6642
_journal_paper_doi               10.1021/om900773w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C28 H81 N6 O2 Si8 Zr2'
_chemical_formula_weight         235.54
_chemical_name_systematic
; 
Zirconium Amdie Cylic O complex
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.113(10)
_cell_length_b                   17.835(12)
_cell_length_c                   18.047(12)
_cell_measurement_temperature    173(2)
_cell_volume                     4864(6)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1091
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50387
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.8911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+31.1031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                3746
_reflns_number_total             6067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900773w_si_003.cif
_cod_data_source_block           orthcycli
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2021-11-22
Formula fixed to be consistent with given Z
                 miguel
;
_cod_original_formula_sum            'C112 H328 N24 O8 Si32 Zr24'
_cod_original_cell_volume        4865(6)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4070385