Toward Supramolecular Assembly of 10-Vertex {closo-2,1,10-FeC2B7} Clusters: Intramolecular Imidate Formation and Polymetallic, Polycluster Species
Franken, Andreas; McGrath, Thomas D.; Stone, F. Gordon A.; Organometallics 29 (2010) 2234–; doi:10.1021/om900970x

data_4067472
_publ_section_title
;
 Toward Supramolecular Assembly of 10-Vertex {closo-2,1,10-FeC2B7}
 Clusters: Intramolecular Imidate Formation and Polymetallic, Polycluster
 Species
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2234
_journal_paper_doi               10.1021/om900970x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C17 H23 B7 Fe N O3 P, C4 H10 O'
_chemical_formula_sum            'C21 H33 B7 Fe N O4 P'
_chemical_formula_weight         525.97
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9304(3)
_cell_length_b                   8.37200(10)
_cell_length_c                   18.5982(3)
_cell_measurement_reflns_used    8425
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.68
_cell_volume                     2730.86(7)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2003)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2003)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2003)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 2001)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'Bruker SHELXTL (Bruker, 2001)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker-Nonius X8 APEX CCD area detector'
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24094
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.3427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                5113
_reflns_number_total             7119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900970x_si_001.cif
_cod_data_source_block           8a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4067472