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_4331478
_publ_section_title
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 Synthesis and X-ray and Neutron Structures of Zr{(\m-H)2BC8H14}4
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_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'
_chemical_formula_weight         583.33
_space_group_IT_number           2
_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_duplicate_entry             4308993
_cod_data_source_file            ic048629gsup2.cif
_cod_data_source_block           zrbhall_acta
_cod_depositor_comments
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  The atom site type symbol for all hydrogen atoms was set as "Y" (ytrium??)
  in the atom list. This provoked an absurd formula and strange molecular
  connectivity. The file has been modified and all H atoms type has been set
  as "H" and the formula corrected accordingly.

  miguel
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_cod_database_code               4331478