Mono(pentamethylcyclopentadienyl)titanium and -zirconium Complexes Supported by Chiral Diolate Ligands. X-ray Crystal Structures of [(η-C5Me5)TiCl(μ-η1,η1-2-CF3-dpbd)]2 and [HNEt3][(η-C5Me5)2Zr2Cl2(μ-Cl)(μ-η1,η2-3,5-Me2-dpbd)2]
David L. Clark; Damon R. Click; Steven K. Grumbine; Brian L. Scott; John G. Watkin; Inorganic Chemistry 37 (1998) 6237–6243; doi:10.1021/ic980645o

data_4323188
_publ_section_title
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 Mono(pentamethylcyclopentadienyl)titanium and -zirconium Complexes
 Supported by Chiral Diolate Ligands. X-ray Crystal Structures of
 [(\h-C5Me5)TiCl(\m-\h1,\h1-2-CF3-dpbd)]2 and
 [HNEt3][(\h-C5Me5)2Zr2Cl2(\m-Cl)(\m-\h1,\h2-3,5-Me2-dpbd)2]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6237
_journal_page_last               6243
_journal_paper_doi               10.1021/ic980645o
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C70 H74 Cl2 F12 O4 Ti2'
_chemical_formula_weight         1373.99
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.208(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.399(1)
_cell_length_b                   22.229(2)
_cell_length_c                   13.275(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      12
_cell_volume                     3411.0(5)
_computing_cell_refinement       'XSCANS 2.10b (Siemens)'
_computing_data_collection       'XSCANS 2.10b (Siemens)'
_computing_data_reduction        'XSCANS 2.10b (Siemens)'
_computing_molecular_graphics    'SHELXTL PC 4.2/360 (Siemens)'
_computing_publication_material  'SHELXTL PC 4.2/360 (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183
_diffrn_measurement_device       'Siemens P4/PC'
_diffrn_measurement_method       '\w scans'
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9572
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         8433
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_obs          0.0671
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.3753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1877
_refine_ls_wR_factor_obs         0.1607
_reflns_number_observed          5744
_reflns_number_total             8433
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980645o_1.cif
_cod_data_source_block           xr63
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.3753P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.3753P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323188