Activation of group 15 based cage compounds by [CpBIGFe(CO)2] radicals
Heinl, Sebastian; Scheer, Manfred; Chemical Science 5 (2014) 3221–; doi:10.1039/c4sc01213e

data_1516277
_publ_section_title
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 Activation of group 15 based cage compounds by [CpBIGFe(CO)2] radicals
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3221
_journal_paper_doi               10.1039/c4sc01213e
_journal_volume                  5
_journal_year                    2014
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C114 H130 Fe2 O4 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C116 H134 Cl4 Fe2 O4 P4'
_chemical_formula_weight         1969.61
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.041(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5044(2)
_cell_length_b                   23.0305(2)
_cell_length_c                   28.6494(3)
_cell_measurement_reflns_used    38957
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      76.0550
_cell_measurement_theta_min      3.1775
_cell_volume                     10564.4(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123.(1)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            60294
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        76.24
_diffrn_reflns_theta_max         76.24
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47343
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Bars
_exptl_crystal_F_000             4168
_exptl_crystal_size_max          0.4717
_exptl_crystal_size_mid          0.2226
_exptl_crystal_size_min          0.0923
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10951
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+11.5859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                10412
_reflns_number_total             10951
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c4sc01213e2.cif
_cod_data_source_block           1
_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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 1516277--1516281.cif.
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_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1516277