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_4086650
_publ_section_title
;
 A Bidentate Carbene Ligand Stabilizes a Low-Coordinate Iron(0) Carbonyl
 Complex
;
_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         'C76 H104 B2 Fe2 K2 N8 O9'
_chemical_formula_sum            'C76 H104 B2 Fe2 K2 N8 O9'
_chemical_formula_weight         1485.22
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-09-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 111.215(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.2814(8)
_cell_length_b                   10.6535(4)
_cell_length_c                   20.1649(8)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3861.4(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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.024
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12691
_diffrn_reflns_theta_full        25.107
_diffrn_reflns_theta_max         25.107
_diffrn_reflns_theta_min         2.167
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9778
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6661
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0247211
_refine_ls_shift/su_mean         0.0012585
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 7.51P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1429
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1429
_reflns_limit_h_max              20
_reflns_limit_h_min              -23
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5051
_reflns_number_total             6689
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.48
_oxford_diffrn_Wilson_scale      50.52
_oxford_refine_ls_r_factor_ref   0.0681
_oxford_refine_ls_scale          0.11317(5)
_oxford_reflns_number_all        6661
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_14083_0m in P2(1)/n'
_cod_data_source_file            om6b00599_si_002.cif
_cod_data_source_block           14083
_cod_depositor_comments
;
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 1 21/n 1 '
_cod_database_code               4086650
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL O    (    3 ) 
CONT O    (    4 ,X'S,U[ISO])  UNTIL O    (    41 ) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   32 ) 
CONT C    (   33 ,X'S,U[ISO])  UNTIL C    (   361 ) 
CONT B    (    1 ,X'S,U'S) 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
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   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,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) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   ( 331,X'S) H   (3311,X'S) H   (3312,X'S) 
RIDE C   ( 341,X'S) H   (3411,X'S) H   (3412,X'S) 
RIDE C   ( 351,X'S) H   (3511,X'S) H   (3512,X'S) 
RIDE C   ( 361,X'S) H   (3611,X'S) H   (3612,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
SAME 0.01, 0.1 FOR 
CONT O(3) C(29) C(30) C(31) C(32) AND 
CONT O(3) C(32) C(31) C(30) C(29) AND 
CONT O(4) C(33) C(34) C(35) C(36) AND 
CONT O(4) C(36) C(35) C(34) C(33) AND 
CONT O(41) C(331) C(341) C(351) C(361) AND 
CONT O(41) C(361) C(351) C(341) C(331) AND 
CONT O(5) C(37) C(38) C(39) C(40) AND 
CONT O(5) C(40) C(39) C(38) C(37) 
RESTRAIN 0.0, 0.005 = O(4,U[ISO])-O(41,U[ISO]) 
RESTRAIN 0.0, 0.005 = C(33,U[ISO])-C(331,U[ISO]) 
RESTRAIN 0.0, 0.005 = C(34,U[ISO])-C(341,U[ISO]) 
RESTRAIN 0.0, 0.005 = C(36,U[ISO])-C(361,U[ISO]) 
END                                                                             
;