Synthesis and structural characterization of Group 4 metallocene complexes that contain remote carboxamide functionalities at their Cp-side chains
Doris Huerlander; Roland Frohlich; Gerhard Erker; Journal of the Chemical Society, Dalton Transactions  (2002) 1513–1520; doi:10.1039/B106026K

data_7702296
_publ_section_title
;
 Synthesis and structural characterization of Group 4 metallocene
 complexes that contain remote carboxamide functionalities at their
 Cp-side chains
;
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1513
_journal_page_last               1520
_journal_paper_doi               10.1039/B106026K
_journal_year                    2002
_chemical_formula_sum            'C26 H40 Fe N2 O2'
_chemical_formula_weight         468.45
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                99.19(1)
_cell_angle_beta                 94.36(1)
_cell_angle_gamma                93.36(1)
_cell_formula_units_Z            1
_cell_length_a                   6.001(1)
_cell_length_b                   8.113(1)
_cell_length_c                   12.399(1)
_cell_measurement_temperature    198(2)
_cell_volume                     592.65(13)
_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 (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Shedlrick, 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_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4789
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.8791
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0185P)^2^+0.2638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                2611
_reflns_number_total             2720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106026k.cif
_cod_data_source_block           erk1178
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702296