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_4086246
_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         'C54 H65 B1 Fe1 N6 O4.50'
_chemical_formula_sum            'C54 H65 B Fe N6 O4.5'
_chemical_formula_weight         936.80
_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             2015-04-13
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 91.1154(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5828(7)
_cell_length_b                   18.0547(10)
_cell_length_c                   22.4004(14)
_cell_measurement_reflns_used    6953
_cell_measurement_temperature    150
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     5087.9(5)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.060
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9056
_diffrn_reflns_theta_full        25.310
_diffrn_reflns_theta_max         25.310
_diffrn_reflns_theta_min         1.449
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.22
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9728
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9007
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.0196709
_refine_ls_shift/su_mean         0.0011084
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ +12.68P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2241
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2236
_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                5420
_reflns_number_total             9056
_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   0.1117
_oxford_refine_ls_scale          0.06819(2)
_oxford_reflns_number_all        9011
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'mo_15037_0ma in P2(1)/c'
_cod_data_source_file            om5b00646_si_002.cif
_cod_data_source_block           15037
_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_cell_volume        5087.9(3)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C54 H65 B1 Fe1 N6 O4.50'
_cod_database_code               4086246