Fe(iv) alkylidenes via protonation of Fe(ii) vinyl chelates and a comparative Mössbauer spectroscopic study
Lindley, Brian M.; Swidan, Ala'aeddeen; Lobkovsky, Emil B.; Wolczanski, Peter T.; Adelhardt, Mario; Sutter, Jörg; Meyer, Karsten; Chem. Sci. 6 (2015) 4730–; doi:10.1039/C5SC01268F

data_1520227
_publ_section_title
;
 Fe(iv) alkylidenes via protonation of Fe(ii) vinyl chelates and a
 comparative M\"ossbauer spectroscopic study
;
_journal_issue                   8
_journal_name_full               'Chem. Sci.'
_journal_page_first              4730
_journal_paper_doi               10.1039/C5SC01268F
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C26 H43 Fe N P3'
_chemical_formula_sum            'C58 H55 B F24 Fe N P3'
_chemical_formula_weight         1381.60
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-03 deposited with the CCDC.
2015-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.5300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4232(6)
_cell_length_b                   13.0618(4)
_cell_length_c                   25.9802(8)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.61
_cell_volume                     6165.6(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35706
_diffrn_reflns_theta_full        23.57
_diffrn_reflns_theta_max         23.57
_diffrn_reflns_theta_min         1.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.8288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         9178
_refine_ls_number_restraints     518
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.607
_refine_ls_shift/su_mean         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+6.1783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                6479
_reflns_number_total             9178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc01268f2.cif
_cod_data_source_block           bl8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1520227--1520230.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1520227