Triphenylphosphane-Modified Cobalt Catalysts for the Selective Carbonylation of Ethyl Diazoacetate
Ungvári, Neszta; Fördős, Eszter; Balogh, János; Kégl, Tamás; Párkányi, László; Ungváry, Ferenc; Organometallics 29 (2010) 3837–; doi:10.1021/om100480v

data_4066475
_publ_section_title
;
 Triphenylphosphane-Modified Cobalt Catalysts for the Selective
 Carbonylation of Ethyl Diazoacetate
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3837
_journal_paper_doi               10.1021/om100480v
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C25 H22 Co O5 P'
_chemical_formula_sum            'C25 H22 Co O5 P'
_chemical_formula_weight         492.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 113.208(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3676(3)
_cell_length_b                   18.0352(4)
_cell_length_c                   15.0701(4)
_cell_measurement_reflns_used    60870
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      3.15
_cell_volume                     2340.02(12)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    'Spek, A.L. (2003). J.Appl.Cryst. 36,7-13.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Charge Flipping (Platon)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  RAXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            80046
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 T.Higashi, Numerical Absorption Correction, NUMABS, 2002
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0418P)^2^+0.9410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                6552
_reflns_number_total             7143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100480v_si_003.cif
_cod_data_source_block           uk09
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2340.02(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4066475