Cyclic Organohydroborate Complexes of Metallocenes. VII. Synthesis, Structure, and Fluxional Behavior of Cp2ZrX{(μ-H)2BC8H14} (X =H, D, Cl)
Xuenian Chen; Shengming Liu; Christine. E. Plečnik; Fu-Chen Liu; Gideon Fraenkel; Sheldon G. Shore; Organometallics 22 (2003) 275–283; doi:10.1021/om0206249

data_4060672
_publ_section_title
;
 Cyclic Organohydroborate Complexes of Metallocenes. VII. Synthesis,
 Structure, and Fluxional Behavior of Cp2ZrX{(\m-H)2BC8H14} (X \\db H,
 D, Cl)
;
_journal_name_full               Organometallics
_journal_page_first              275
_journal_page_last               283
_journal_paper_doi               10.1021/om0206249
_journal_volume                  22
_journal_year                    2003
_chemical_formula_sum            'C18 H27 B Zr'
_chemical_formula_weight         345.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.792(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9608(10)
_cell_length_b                   10.2533(10)
_cell_length_c                   13.9041(10)
_cell_measurement_temperature    150(2)
_cell_volume                     1662.8(2)
_computing_cell_refinement       'DENZO (Oywinowsky & Minor, 1997)'
_computing_data_collection       'COLLET (Nonius, 1999)'
_computing_data_reduction        'DENZO (Oywinowsky & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius kappaCCD'
_diffrn_measurement_method       '\w at 55/-55'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10236
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.7543
_exptl_absorpt_correction_type   'SORTAV (blessing 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.4291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                2605
_reflns_number_total             2931
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4060672