Synthesis and the structure of 8-tetrahydrofuronium and 8-tetrahydropyronium derivatives of iron bis(dicarbollide)(-I) and their cleavage reactions.
Lobanova, Irina; Kosenko, Irina; Laskova, Julia; Ananyev, Ivan; Druzina, Anna; Godovikov, Ivan; Bregadze, Vladimir I.; Qi, Shicheng; Leśnikowski, Zbigniew J; Semioshkin, Andrey; Dalton transactions (Cambridge, England : 2003) 44 (2015) 1571–1584; doi:10.1039/c4dt03015j

data_7033153
_publ_section_title
;
 Synthesis and the structure of 8-tetrahydrofuronium and
 8-tetrahydropyronium derivatives of iron bis(dicarbollide)(-I) and their
 cleavage reactions.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1571
_journal_page_last               1584
_journal_paper_doi               10.1039/c4dt03015j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C68 H106 B36 Fe2 O2 P4, (C H2 Cl2), 0.5 (C H2 Cl2)'
_chemical_formula_sum            'C35.5 H56 B18 Cl3 Fe O P2'
_chemical_formula_weight         917.52
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.620(2)
_cell_angle_beta                 81.392(2)
_cell_angle_gamma                69.815(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2119(4)
_cell_length_b                   13.9471(5)
_cell_length_c                   15.1730(5)
_cell_measurement_reflns_used    756
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      65
_cell_measurement_theta_min      3
_cell_volume                     2311.68(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_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, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25676
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    5.084
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         7547
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+0.9248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                6335
_reflns_number_total             7547
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4dt03015j2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7033150--7033153.cif.
;
_cod_original_formula_sum        'C35.50 H56 B18 Cl3 Fe O P2'
_cod_database_code               7033153