Synthesis, Structural Characterization, and Reactions of Cyclic Organohydroborate Half-Zirconocene Compounds
Errun Ding; Fu-Chen Liu; Shengming Liu; Edward A. Meyers; Sheldon G. Shore; Inorganic Chemistry 41 (2002) 5329–5335; doi:10.1021/ic0202817

data_4318674
_publ_section_title
;
 Synthesis, Structural Characterization, and Reactions of Cyclic
 Organohydroborate Half-Zirconocene Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5329
_journal_page_last               5335
_journal_paper_doi               10.1021/ic0202817
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C62 H52 B2 F30 O6 Zr2'
_chemical_formula_weight         1667.10
_chemical_name_systematic
;
   ?
;
_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                61.459(10)
_cell_angle_beta                 76.237(10)
_cell_angle_gamma                69.907(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2391(10)
_cell_length_b                   12.7093(10)
_cell_length_c                   12.8877(10)
_cell_measurement_temperature    333(2)
_cell_volume                     1647.3(3)
_computing_cell_refinement       'DENZO (Otwinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nunius, 1999)'
_computing_data_reduction        'DENZO (Otwinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      333(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.1127
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6206
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.8764
_exptl_absorpt_correction_T_min  0.8400
_exptl_absorpt_correction_type   'SORTAV (blessing, 1995)'
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.625
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+1.0051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                4655
_reflns_number_total             5783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0202817_5.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1647.3(2)
_cod_database_code               4318674