New Sandwich and Half-Sandwich Titanium Hydrazido Compounds
Selby, Jonathan D.; Feliz, Marta; Schwarz, Andrew D.; Clot, Eric; Mountford, Philip; Organometallics 30 (2011) 2295–; doi:10.1021/om200068k

data_4064365
_publ_section_title
;
 New Sandwich and Half-Sandwich Titanium Hydrazido Compounds
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2295
_journal_paper_doi               10.1021/om200068k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C24 H42 Cl2 N4 Ti2'
_chemical_formula_sum            'C24 H42 Cl2 N4 Ti2'
_chemical_formula_weight         553.33
_chemical_name_systematic
;
Cp*2Ti2(u-NNMe2)2Cl2
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.8414(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0039(2)
_cell_length_b                   17.9623(5)
_cell_length_c                   15.4127(4)
_cell_measurement_reflns_used    4793
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2677.16(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9631
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         5.147
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000468
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.35 0.502 0.951 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0493
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0430
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4740
_reflns_number_total             5845
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.45
_oxford_diffrn_Wilson_scale      2.44
_oxford_refine_ls_scale          0.5151(8)
_cod_data_source_file            om200068k_si_001.cif
_cod_data_source_block           Compound_8
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4064365