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_7027769
_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            'C30 H46 Fe N4 O4'
_chemical_formula_weight         582.56
_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   'geometrically, at N from Diff.-Fourier'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.05(1)
_cell_angle_beta                 99.78(1)
_cell_angle_gamma                107.58(1)
_cell_formula_units_Z            1
_cell_length_a                   6.793(1)
_cell_length_b                   10.902(1)
_cell_length_c                   11.208(1)
_cell_measurement_temperature    198(2)
_cell_volume                     776.41(16)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_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      198(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6015
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.8377
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0412P)^2^+0.3959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                3309
_reflns_number_total             3538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906553Isup1.cif
_cod_data_source_block           erk1128
_cod_original_cell_volume        776.41(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027769