Synthesis of Alkynyl Amino Acids and Peptides and Their Palladium-Catalyzed Coupling to Ferrocene
Oliver Brosch; Thomas Weyhermüller; Nils Metzler-Nolte; Inorganic Chemistry 38 (1999) 5308–5313; doi:10.1021/ic990256+

data_4327668
_publ_section_title
;
 Synthesis of Alkynyl Amino Acids and Peptides and Their
 Palladium-Catalyzed Coupling to Ferrocene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5308
_journal_page_last               5313
_journal_paper_doi               10.1021/ic990256+
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C21 H30 N2 O3'
_chemical_formula_weight         358.47
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   12.147(3)
_cell_length_b                   20.320(4)
_cell_length_c                   26.646(5)
_cell_measurement_reflns_used    6525
_cell_measurement_temperature    293(2)
_cell_volume                     6577(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens ShelXTL'
_computing_publication_material  'Siemens ShelXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg/frame'
_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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.1291
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22426
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick 1994'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       'Transparent Block '
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          1.12
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   'not reliable '
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.933
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_obs          0.0598
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1391
_refine_ls_wR_factor_obs         0.1281
_reflns_number_observed          5960
_reflns_number_total             8576
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9902562B.cif
_cod_data_source_block           2a
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4327668