A Bidentate Carbene Ligand Stabilizes a Low-Coordinate Iron(0) Carbonyl Complex
Hickey, Anne K.; Lee, Wei-Tsung; Chen, Chun-Hsing; Pink, Maren; Smith, Jeremy M.; Organometallics 35 (2016) 3069–; doi:10.1021/acs.organomet.6b00599

data_4086649
_publ_section_title
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 A Bidentate Carbene Ligand Stabilizes a Low-Coordinate Iron(0) Carbonyl
 Complex
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_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3069
_journal_paper_doi               10.1021/acs.organomet.6b00599
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C35 H38 B1 Fe1 N4 O3'
_chemical_formula_sum            'C35 H38 B Fe N4 O3'
_chemical_formula_weight         629.37
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-08-18
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 110.301(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7519(7)
_cell_length_b                   18.4759(17)
_cell_length_c                   11.7496(11)
_cell_measurement_reflns_used    2436
_cell_measurement_temperature    150
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     1781.9(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12358
_diffrn_reflns_theta_full        23.953
_diffrn_reflns_theta_max         24.694
_diffrn_reflns_theta_min         1.848
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.03
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9703
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3072
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.0042983
_refine_ls_shift/su_mean         0.0005354
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.17P)^2^ + 7.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3081
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3081
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2014
_reflns_number_total             3089
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1338
_oxford_refine_ls_scale          0.1850(4)
_oxford_reflns_number_all        3072
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_14058_0m in P2(1)/m'
_cod_data_source_file            om6b00599_si_002.cif
_cod_data_source_block           14058
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086647--4086651.cif.
;
_cod_original_sg_symbol_H-M      'P 21/m '
_cod_original_formula_sum        'C35 H38 B1 Fe1 N4 O3'
_cod_database_code               4086649
_iucr_refine_instruction_details_constraints
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BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL C    (   19 ) 
CONT C    (   20 ,X'S,U[ISO])  UNTIL C    (   24 ) 
CONT B    (   13 ,X'S,U'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
U(IJ)'S  0.0, 0.007000 = C(4) TO C(5) 
U(IJ)'S  0.0, 0.007000 = C(6) TO C(7) 
DISTANCE 1.400000 , 0.010000 = C(21) TO C(20) 
DISTANCE 1.400000 , 0.010000 = C(21) TO C(22) 
DISTANCE 1.400000 , 0.020000 = C(24,-1,1,1,1,2) TO C(24) 
RESTRAIN 0.0, 0.001=C(24,U[ISO])-C(23,U[ISO]) 
END                                                                             
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