Synthesis and X-ray and Neutron Structures of Zr{(μ-H)2BC8H14}4
Ding, Errun; Du, Bin; Meyers, Edward A.; Shore, Sheldon G.; Yousufuddin, Muhammed; Bau, Robert; McIntyre, Garry J.; Inorganic Chemistry 44 (2005) 2459–2464; doi:10.1021/ic048629g

data_4308993
_publ_section_title
;
 Synthesis and X-ray and Neutron Structures of Zr{(\m-H)2BC8H14}4
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2459
_journal_page_last               2464
_journal_paper_doi               10.1021/ic048629g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C32 H64 B4 Zr'
_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                92.650(10)
_cell_angle_beta                 96.550(10)
_cell_angle_gamma                91.800(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2470(10)
_cell_length_b                   11.3890(10)
_cell_length_c                   12.8980(10)
_cell_measurement_temperature    153(2)
_cell_volume                     1638.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.503
_diffrn_measured_fraction_theta_max 0.503
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.90000
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_sigmaI/netI    0.2548
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14032
_diffrn_reflns_theta_full        38.72
_diffrn_reflns_theta_max         38.72
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    0.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3
_refine_diff_density_max         1.989
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         4642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                2557
_reflns_number_total             4642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048629gsi20050116_043632.cif
_cod_data_source_block           zrbhall_acta
_cod_database_code               4308993