Bis-hydroxylaminato group 4 half-sandwich complexes—syntheses, structures and polymerisation activity studies
Willner, Alexander; Niemeyer, Jochen; Mitzel, Norbert W.; Dalton Transactions  (2009) 4473–4480; doi:10.1039/b821786f

data_7001397
_publ_section_title
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 Bis-hydroxylaminato group 4 half-sandwich complexes---syntheses,
 structures and polymerisation activity studies
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4473
_journal_page_last               4480
_journal_paper_doi               10.1039/b821786f
_journal_year                    2009
_chemical_formula_sum            'C14 H26 N2 O2 Ti'
_chemical_formula_weight         302.27
_chemical_name_common            '[Cp*TiMe(ONMe)2CH2]'
_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                78.397(18)
_cell_angle_beta                 86.828(18)
_cell_angle_gamma                65.249(16)
_cell_formula_units_Z            2
_cell_length_a                   8.1352(13)
_cell_length_b                   8.6112(14)
_cell_length_c                   12.593(2)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      4.56
_cell_volume                     784.4(2)
_computing_cell_refinement       'STOE IPDS-1 software package'
_computing_data_collection       'STOE IPDS-1 software package'
_computing_data_reduction        'STOE IPDS-1 software package'
_computing_molecular_graphics
;
ORTEP3, L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       '\phi 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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12203
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         4.56
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.9474
_exptl_absorpt_correction_T_min  0.7719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction was done with the program abscor from the STOE
IPDS-1 sotware package. abscor works similar to the well known difabs
but uses Fo^2^ values instead of Fo.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0625P)^2^+0.2927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                2745
_reflns_number_total             3118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821786f.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        784.3(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001397