The complex metal-rich boride Ti1+xRh2−x+yIr3−yB3 (x=0.68, y=1.06) with a new structure type containing B4 zigzag fragments: Synthesis, crystal chemistry and theoretical calculations
Goerens, Christian; Fokwa, Boniface P.T.; Journal of Solid State Chemistry 192 (2012) 113–119; doi:10.1016/j.jssc.2012.04.005

data_1562953
_publ_section_title
;
 The complex metal-rich boride Ti1+xRh2&#x2212;x+yIr3&#x2212;yB3 (x=0.68,
 y=1.06) with a new structure type containing B4 zigzag fragments:
 Synthesis, crystal chemistry and theoretical calculations
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              113
_journal_page_last               119
_journal_paper_doi               10.1016/j.jssc.2012.04.005
_journal_volume                  192
_journal_year                    2012
_chemical_formula_sum            'B3 Ir1.94 Rh2.38 Ti1.68'
_chemical_formula_weight         731.28
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      55
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_atom_sites_solution_hydrogens   refall
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6200(10)
_cell_length_b                   14.9947(17)
_cell_length_c                   3.2337(4)
_cell_measurement_temperature    293(2)
_cell_volume                     417.97(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 3.1e (K. Brandenburg, 2007)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'integretion method'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6511
_diffrn_reflns_theta_full        36.02
_diffrn_reflns_theta_max         36.02
_diffrn_reflns_theta_min         4.71
_exptl_absorpt_coefficient_mu    73.695
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.052
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'by multipole expansion (Blessing, 1995)'
_exptl_crystal_colour            silver
_exptl_crystal_density_diffrn    11.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1235
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.060
_refine_diff_density_min         -4.892
_refine_diff_density_rms         0.805
_refine_ls_extinction_coef       0.0020(2)
_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   1.158
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0324P)^2^+17.9266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                981
_reflns_number_total             1112
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            JSSC-2012-192-113.cif
_cod_data_source_block           boni82
_cod_database_code               1562953