Formation and structural properties of 1,1′,2,2′-tetra(tert-butylcarbamoyl)-ferrocene and -ruthenocene †
Klaß, Katrin; Fröhlich, Roland; Erker, Gerhard; Journal of the Chemical Society, Dalton Transactions  (1999) 4457–; doi:10.1039/a906553i

data_7027767
_publ_section_title
;
 Formation and structural properties of
 1,1&#x2032;,2,2&#x2032;-tetra(tert-butylcarbamoyl)-ferrocene and
 -ruthenocene&#x200A;&#x2020;
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4457
_journal_paper_doi               10.1039/a906553i
_journal_year                    1999
_chemical_formula_sum            'C54.5 H57 Cl N2 O2 P2 Ru'
_chemical_formula_weight         970.48
_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                70.27(1)
_cell_angle_beta                 73.87(1)
_cell_angle_gamma                72.15(1)
_cell_formula_units_Z            2
_cell_length_a                   11.511(1)
_cell_length_b                   13.315(1)
_cell_length_c                   18.735(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      10.91
_cell_measurement_theta_min      8.27
_cell_volume                     2523.6(4)
_computing_cell_refinement       'Express (Nonius B.V., 1994)'
_computing_data_collection       'Express (Nonius B.V., 1994)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'SCHAKAL-92 (Keller, 1992)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_measurement_method       '\w/2\q scans'
_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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.1597
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6996
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        13.3
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_correction_T_min  0.8534
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.099
_refine_diff_density_min         -2.145
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    'refined as riding atoms (see above)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                4263
_reflns_number_total             6601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906553Isup1.cif
_cod_data_source_block           erk_987
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C54.50 H57 Cl N2 O2 P2 Ru'
_cod_database_code               7027767