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_4323189
_publ_section_title
;
 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]
;
_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            'C66 H94 Cl3 N O4 Zr2'
_chemical_formula_weight         1254.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.615(2)
_cell_length_b                   13.623(2)
_cell_length_c                   36.042(5)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    183
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      9.5
_cell_volume                     6685.0(17)
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7934
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.949
_refine_ls_goodness_of_fit_obs   0.978
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      0.978
_refine_ls_R_factor_all          0.1313
_refine_ls_R_factor_obs          0.0679
_refine_ls_shift/esd_max         0.050
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+14.3135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1997
_refine_ls_wR_factor_obs         0.1542
_reflns_number_observed          4662
_reflns_number_total             7655
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980645o_2.cif
_cod_data_source_block           xr69
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+14.3135P] 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^)+(0.0917P)^2^+14.3135P] where P=(Fo^2^+2Fc^2^)/3'.

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

2020-09-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         627.11
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'C33 H47 Cl1.50 N0.50 O2 Zr'
_cod_database_code               4323189