The First Nitro-Substituted Heteroscorpionate Ligand
Maura Pellei; Franco Benetollo; Giancarlo Gioia Lobbia; Simone Alidori; Carlo Santini; Inorganic Chemistry 44 (2005) 846–848; doi:10.1021/ic048562x

data_4308546
_publ_contact_author             ' Carlo Santini'
_publ_section_title
;
The First Nitro-Substituted Heteroscorpionate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              846
_journal_page_last               848
_journal_paper_doi               10.1021/ic048562x
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[H~2~B(3-NO~2~Tz)~2~]K]'
_chemical_formula_sum            'C4 H4 B K N8 O4'
_chemical_formula_weight         278.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 106.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.931(2)
_cell_length_b                   10.952(3)
_cell_length_c                   10.448(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1088.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Philips PW1100'
_diffrn_measurement_method       \Q/2\Q
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2524
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.512
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0414P)^2^+0.7171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                2379
_reflns_number_total             2415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048562xsi20041018_025714.cif
_cod_data_source_block           camK
_cod_database_code               4308546