Cyanide Ligand Assembly by Carbon Atom Transfer to an Iron Nitride.
Martinez, Jorge L.; Lin, Hsiu-Jung; Lee, Wei-Tsung; Pink, Maren; Chen, Chun-Hsing; Gao, Xinfeng; Dickie, Diane A.; Smith, Jeremy M.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08704

data_4126488
_publ_section_title
;
 Cyanide Ligand Assembly by Carbon Atom Transfer to an Iron Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08704
_journal_year                    2017
_chemical_formula_moiety         'C43.50 H61.50 B1 Cl1 Fe1 N6'
_chemical_formula_sum            'C43.5 H61.5 B Cl Fe N6'
_chemical_formula_weight         770.62
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-10-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                82.9470(10)
_cell_angle_beta                 81.975(2)
_cell_angle_gamma                64.9910(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4756(3)
_cell_length_b                   12.1783(3)
_cell_length_c                   17.3054(5)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2164.78(10)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44162
_diffrn_reflns_theta_full        28.817
_diffrn_reflns_theta_max         28.817
_diffrn_reflns_theta_min         1.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             825
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.536
_exptl_crystal_size_min          0.324
_refine_diff_density_max         1.73
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         11236
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.0419843
_refine_ls_shift/su_mean         0.0016558
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.72P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1175
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1175
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9792
_reflns_number_total             11275
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      56.68
_oxford_refine_ls_r_factor_ref   0.0499
_oxford_refine_ls_scale          0.18358(8)
_oxford_reflns_number_all        11237
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'mo_13102_0m in P-1'
_cod_data_source_file            ja7b08704_si_002.cif
_cod_data_source_block           13102
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C43.50 H61.50 B1 Cl1 Fe1 N6'
_cod_database_code               4126488
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL C    (   33 ) 
CONT C    (   34 ,X'S,U[ISO])  UNTIL C    (   38 ) 
CONT C    (   39 ,X'S,U[ISO]) 
CONT C    (   40 ,X'S,U[ISO])  UNTIL C    (   441 ) 
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   (   4,X'S) H   (  41,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) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,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) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,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) 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   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,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   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   ( 391,X'S) H   (3911,X'S) 
RIDE C   ( 401,X'S) H   (4011,X'S) 
RIDE C   ( 411,X'S) H   (4111,X'S) 
RIDE C   ( 421,X'S) H   (4211,X'S) 
RIDE C   ( 431,X'S) H   (4311,X'S) 
RIDE C   ( 441,X'S) H   (4411,X'S) H   (4412,X'S) H   (4413,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 C(38) C(39) C(40) C(41) C(42) C(43) C(44) AND 
CONT C(38) C(43) C(42) C(41) C(40) C(39) C(44) AND 
CONT C(381) C(391) C(401) C(411) C(421) C(431) C(441) AND 
CONT C(381) C(431) C(421) C(411) C(401) C(391) C(441) 
ANGLE 120.000000 , 1.000000 = C(35) TO C(34) TO C(36) 
DISTANCE 1.400000 , 0.010000 = C(34) TO C(36) 
END                                                                             
;