Reactions of N-heterocyclic ligands with substitutionally labile organometallic complexes, [(eta5-C5R5)Fe(CO)2E]BF4
Mthiruaine, Cyprian M.; Friedrich, Holger B.; Changamu, Evans O.; Bala, Muhammad D.; Inorganica Chimica Acta 390 (2012) 83–94; doi:10.1016/j.ica.2012.04.003

data_1508225
_publ_section_title
;
 Reactions of N-heterocyclic ligands with substitutionally labile
 organometallic complexes, [(eta5-C5R5)Fe(CO)2E]BF4
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              83
_journal_page_last               94
_journal_paper_doi               10.1016/j.ica.2012.04.003
_journal_volume                  390
_journal_year                    2012
_chemical_formula_moiety         'C16 H21 Fe N2 O2, B F4'
_chemical_formula_sum            'C16 H21 B F4 Fe N2 O2'
_chemical_formula_weight         416.01
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0840(4)
_cell_length_b                   13.9877(4)
_cell_length_c                   7.6984(2)
_cell_measurement_reflns_used    7644
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.79
_cell_volume                     1839.65(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20793
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.9913
_exptl_absorpt_correction_T_min  0.7006
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Face indexed absorption corrections carried out with XPREP
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4441
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                3823
_reflns_number_total             4441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-83-94-2.cif
_cod_data_source_block           New_Global_Publ_Block-II
_cod_database_code               1508225