Low-Valent Iron Carbonyl Complexes with a Tripodal Carbene Ligand
Hickey, Anne K.; Chen, Chun-Hsing; Pink, Maren; Smith, Jeremy M.; Organometallics 34 (2015) 4560–; doi:10.1021/acs.organomet.5b00646

data_4086248
_publ_section_title
;
 Low-Valent Iron Carbonyl Complexes with a Tripodal Carbene Ligand
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4560
_journal_paper_doi               10.1021/acs.organomet.5b00646
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C44 H44 B Fe N6 O2, C18 H36 K N2 O6, 3 (C4 H8 O)'
_chemical_formula_sum            'C74 H104 B Fe K N8 O11'
_chemical_formula_weight         1387.41
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.9708(18)
_cell_angle_beta                 77.5592(18)
_cell_angle_gamma                70.3780(17)
_cell_formula_units_Z            2
_cell_length_a                   15.9892(5)
_cell_length_b                   16.2233(6)
_cell_length_c                   16.4966(5)
_cell_measurement_reflns_used    8657
_cell_measurement_temperature    186(2)
_cell_measurement_theta_max      22.12
_cell_measurement_theta_min      2.57
_cell_volume                     3716.7(2)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXTL (Bruker, 2012)'
_computing_structure_solution    'SHELXTL (Bruker, 2013)'
_diffrn_ambient_temperature      186(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
'0.50 degree frames measured for 40 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50541
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.9444
_exptl_absorpt_correction_T_min  0.9268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2014'
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         13074
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0786P)^2^+1.4225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                8003
_reflns_number_total             13074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00646_si_002.cif
_cod_data_source_block           15045
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4086248