Reductive Coupling of CO Templated by Iron Bound to the Tris(pyrrolide)ethane Scaffold
Sazama, Graham T.; Betley, Theodore A.; Organometallics 30 (2011) 4315–; doi:10.1021/om2003859

data_4063572
_publ_section_title
;
 Reductive Coupling of CO Templated by Iron Bound to the
 Tris(pyrrolide)ethane Scaffold
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4315
_journal_paper_doi               10.1021/om2003859
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C69 H86 Fe Li N6 O'
_chemical_formula_weight         1078.23
_chemical_name_common            '[(tpe)Fe(NCtBu)3][Li(THF)]'
_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                88.352(4)
_cell_angle_beta                 84.975(4)
_cell_angle_gamma                72.407(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7409(7)
_cell_length_b                   12.5697(8)
_cell_length_c                   23.8076(15)
_cell_measurement_reflns_used    7342
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.30
_cell_volume                     3052.1(3)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72882
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.9381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.068
_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     732
_refine_ls_number_reflns         15598
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                11040
_reflns_number_total             15598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2003859_si_002.cif
_cod_data_source_block           gts016
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063572