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_4086249
_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         'C56 H68.00 B1 Fe1 N6 O5'
_chemical_formula_sum            'C56 H68 B Fe N6 O5'
_chemical_formula_weight         971.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             14-06-17
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 91.290(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5758(9)
_cell_length_b                   17.9460(12)
_cell_length_c                   22.3934(14)
_cell_measurement_reflns_used    6035
_cell_measurement_temperature    150
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     5052.6(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36242
_diffrn_reflns_theta_full        25.116
_diffrn_reflns_theta_max         25.116
_diffrn_reflns_theta_min         1.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.058
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.97
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8906
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.0083582
_refine_ls_shift/su_mean         0.0003256
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.12P)^2^ +15.59P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2404
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2400
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5189
_reflns_number_total             8952
_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   0.1267
_oxford_refine_ls_scale          0.06329(2)
_oxford_reflns_number_all        8909
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_14049_0m in P2(1)/c'
_cod_data_source_file            om5b00646_si_002.cif
_cod_data_source_block           14049
_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/current/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 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C56 H68.00 B1 Fe1 N6 O5'
_cod_database_code               4086249
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL O    (    2 ) 
CONT O    (    3 ,X'S,U[ISO])  UNTIL O    (   4 ) 
CONT O    (    5 ,X'S,U[ISO])  UNTIL O    (   6 ) 
CONT O    (   41 ,X'S,U[ISO]) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   44 ) 
CONT C    (   45 ,X'S,U[ISO]) UNTIL C(53) 
CONT C    (   54 ,X'S,U[ISO]) UNTIL C(55) 
CONT C    (   56 ,X'S,U[ISO]) UNTIL C(60) 
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   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) H   ( 103,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) H   ( 223,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) H   ( 494,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) H   ( 524,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,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) 
RESTRAIN 0.0, 0.01 = O(4,U[ISO])-O(41,U[ISO]) 
RESTRAIN 0.0, 0.01 = C(60,U[ISO])-O(6,U[ISO]) 
SAME 0.1, 0.01 FOR 
CONT O(3) C(45) C(46) C(47) C(48) AND 
CONT O(4) C(49) C(50) C(51) C(52) AND 
CONT O(41) C(49) C(50) C(51) C(52) AND 
CONT O(3) C(48) C(47) C(46) C(45) AND 
CONT O(4) C(52) C(51) C(50) C(49) AND 
CONT O(41) C(52) C(51) C(50) C(49) AND 
CONT O(5) C(53) C(54) C(55) C(56) AND 
CONT O(6) C(57) C(58) C(59) C(60) AND 
CONT O(5) C(56) C(55) C(54) C(53) AND 
CONT O(6) C(60) C(59) C(58) C(57) 
END                                                                             
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