C‒N Coupling of Isocyanide Ligands Promoted by Acetylide Addition to Diiron Aminocarbyne Complexes
Marchetti, Fabio; Zacchini, Stefano; Zanotti, Valerio; Organometallics 34 (2015) 3658–; doi:10.1021/acs.organomet.5b00515

data_4086059
_publ_section_title
;
 C--N Coupling of Isocyanide Ligands Promoted by Acetylide Addition to
 Diiron Aminocarbyne Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3658
_journal_paper_doi               10.1021/acs.organomet.5b00515
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C48 H47 Fe2 N3 O'
_chemical_formula_weight         793.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.291(3)
_cell_length_b                   17.124(3)
_cell_length_c                   18.910(4)
_cell_measurement_reflns_used    939
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.6925
_cell_measurement_theta_min      2.406
_cell_volume                     3953.5(15)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0834
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24578
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.8420
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0760 (selected reflections only, before parameter refinement)
 R(int) =  0.0539 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         6996
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0784P)^2^+1.2839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                4512
_reflns_number_total             6996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00515_si_002.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4086059--4086060.cif.
;
_cod_original_cell_volume        3953.7(14)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4086059