Synthesis and characterization of an iron complex bearing a hemilabile NNN-pincer for catalytic hydrosilylation of organic carbonyl compounds.
Lin, Hsiu-Jung; Lutz, Sean; O'Kane, Catherine; Zeller, Matthias; Chen, Chun-Hsing; Al Assil, Talal; Lee, Wei-Tsung; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3243–3247; doi:10.1039/c7dt04928e

data_7045406
_publ_section_title
;
 Synthesis and characterization of an iron complex bearing a hemilabile
 NNN-pincer for catalytic hydrosilylation of organic carbonyl compounds.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3243
_journal_page_last               3247
_journal_paper_doi               10.1039/c7dt04928e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C45.35 H71.92 Fe1 N6 Si2'
_chemical_formula_sum            'C45.35 H71.92 Fe N6 Si2'
_chemical_formula_weight         813.21
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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             2016-01-08
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-01-06 deposited with the CCDC.
2018-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                85.8334(18)
_cell_angle_beta                 77.5244(16)
_cell_angle_gamma                72.8578(15)
_cell_formula_units_Z            4
_cell_length_a                   13.6609(3)
_cell_length_b                   16.2506(5)
_cell_length_c                   22.6277(6)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     4686.6(2)
_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      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_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  0.048
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27191
_diffrn_reflns_theta_full        27.650
_diffrn_reflns_theta_max         30.054
_diffrn_reflns_theta_min         0.922
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760.002
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.054
_refine_diff_density_max         2.44
_refine_diff_density_min         -1.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1418
_refine_ls_number_reflns         27096
_refine_ls_number_restraints     645
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.0369802
_refine_ls_shift/su_mean         0.0008302
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.12P)^2^ +10.03P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2633
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2620
_reflns_limit_h_max              19
_reflns_limit_h_min              -18
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                15292
_reflns_number_total             27191
_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   0.1423
_oxford_refine_ls_scale          0.048306(8)
_oxford_reflns_number_all        27135
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'lee_1_0m in P-1'
_cod_data_source_file            c7dt04928e2.cif
_cod_data_source_block           LEE_1
_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/RSC/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 

 Adding full bibliography for 7045406--7045408.cif.
;
_cod_original_cell_volume        4686.59(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45.35 H71.92 Fe1 N6 Si2'
_cod_database_code               7045406